Processing of Ceramics - User contributions [en]

Field assisted sintering technology/spark plasma sintering

2021-08-05T07:07:33Z

M.bram: /* Alternative operation modes of FAST/SPS devices */

== General principle of FAST/SPS ==
Field Assisted Sintering Technology/Spark Plasma Sintering (FAST/SPS) is a low-voltage, current-activated and pressure-supported sintering process that is based on Joule heating (= resistance heating) of the conductive tools ('''Figure 1''') and is characterized by high heating rates and short cycle times. If electrically conductive powders are applied, the powder itself is also heated directly via the Joule effect. The FAST/SPS process is established in the industry and particularly promising when powders are to be sintered, which have a low sintering activity or an unfavorable particle morphology and particle size distribution for conventional pressing and sintering. Furthermore, the method is well suited for the production of composite materials, especially when phases will be combined, which have very different physical properties. Some typical application examples of FAST/SPS technology are presented in Chapter 7. Due to the great flexibility, the short cycle times and the comparatively simple and cost-effective production of tools, research and development is another important field of application for FAST/SPS technology and is widespread there.

[[File:Wiki Keramik FAST SPS Abb 01.jpg|thumb|center]]
'''Figure 1:''' ''Heated graphite tool in a FAST / SPS device.''

In principle, a FAST/SPS device is a mechanical press, which at the same time also forms a high-energy current circuit. The FAST/SPS process is carried out in a conductive tool consisting of two punches and a die. Two additional cones establish the contact with the device's electrodes. The pressing force is also applied via these electrodes by means of a hydraulic pressure cylinder. '''Figure 2''' shows a schematic sketch of such a device. FAST/SPS processes are usually carried out in a vacuum or protective gas to protect the tool and the powder inside the tool from oxidation. Accordingly, the pressing device is located in a water-cooled chamber, in which a moderate vacuum (0.5 - 20 mbar) or a defined protective gas atmosphere (e.g. Ar or N2) can be set. The heating of the tool via the Joule effect requires the use of conductive materials for the punch and the die. The standard material for punch and die is graphite, alternatives to this are introduced in Chapter 4.

[[File:Wiki Keramik FAST SPS Abb 02 englisch.jpg|thumb|center]]
'''Figure 2:''' ''Schematic sketch of a FAST/SPS device.''

The tool is heated by a continuous or pulsed direct current with moderate voltages <10 V and high currents in the range from 1 to several 10 kA (depending on the size of the device). Non-conductive powders can also be sintered in good quality via FAST/SPS. Here, the direct contact between the tool and the powder leads to rapid heat transfer and relatively even heating over the entire cross-section of the sample. The heating takes place primarily via thermal conduction. In order to reduce the heat loss through thermal radiation, the die can optionally be thermally insulated, e.g. with a graphite felt. In the standard configuration, heating rates of up to approx. 300 K/min can be achieved in a FAST/SPS device. The high heating rates are one of the main reasons for the fast cycle times, as grain boundary and volume diffusion necessary for mass transport during sintering are activated directly. Due to the thermal mass of the tools, extremely high cooling rates cannot be achieved. Typical cooling rates are around 100 - 150 K/min. It should be noted here that the use of thermal insulation materials further reduces the cooling rates. In addition to the rapid heating, the sintering kinetics are also supported by the applied load. Depending on the type of system and sample size, compaction pressure in the range of 50 - 100 MPa can be achieved with the standard material graphite. Special grades of graphite allow maximum pressures of up to 200 MPa. When using graphite tools, temperatures of up to approx. 2,200 °C can be achieved in FAST/SPS devices. Alternative tools made of highly heat-resistant metals or electrically conductive ceramics enable pressures of up to 400 MPa, but the maximum permissible sintering temperatures are usually significantly lower in these cases. In order to improve the electrical contact between the punches, the die and the sample, a flexible, ideally electrically conductive foil is usually positioned between the punches and the sample. Graphite has also proven to be the standard material for this foil. FAST/SPS systems are usually controlled by programming the temperature-time curve. The measurement of the temperature as a major process parameter is carried out by axially or radially arranged pyrometers or by thermocouples. A direct measurement of the sample temperature is usually not possible. In order to measure the temperature as close as possible to the sample, holes are often drilled in the tools, at the bottom of which the temperature is measured. Furthermore, especially with increasing size of sintered parts and complexity of shape, it is recommended to predict the temperature distribution in the parts using suitable FEM modeling.

== Advantages and limitations of FAST/SPS ==
i.) '''Advantages:''' An essential feature of the FAST/SPS process is the rapid heating of the sample, which is based on the direct heating of the tool and the good heat transfer between the die and the powder. The superimposition of an uniaxial pressure during sintering further accelerates the sintering kinetics, so that the sintering temperature can often be significantly reduced compared to conventional sintering processes. Accordingly, the FAST/SPS process is a promising technology for

* '''Powder with low sintering activity:''' FAST/SPS enables the compaction of powders that have a low sintering activity (e.g. borides, carbides, nitrides and their mixtures).
* '''Powders with unfavorable powder properties:''' Powders can be sintered whose particle size distribution and morphology are unsuitable for conventional pressing and sintering.
* '''Nanoscale powders:''' The rapid processing in the case of FAST/SPS makes it possible to preserve the structure of nanoscale powders in the component.
* '''Materials with limited stability:''' FAST/SPS enables the sintering of materials that tend to decompose at high temperatures and long dwell times and to form undesirable secondary phases.
* '''Materials containing phases out of thermodynamic equilibrium:''' Phases out of thermodynamic equilibrium can be maintained in the sintered part (e.g. amorphous phases). Based on this, properties can be achieved that are not feasible with other sintering methods.
* '''Composite materials:''' FAST/SPS has great potential for sintering of composite materials that combine phases, which have large differences in their physical properties (e.g. very different melting points).
* '''Energy-efficient processing:''' In general, the FAST/SPS process is classified as an energy-efficient process due to the reduced sintering temperature and the short cycle times, but the degree of automation and the number of components per sintering cycle must also be taken carefully into account for an objective comparison with other sintering technologies.

ii.) '''Limitations:''' Despite the obvious advantages of FAST/SPS technology, there are also a number of process-related limitations.
* '''Risk of density and stress gradients in the component:''' If powders with a low thermal conductivity and high electrical resistance are sintered by FAST/SPS, there might arise an inhomogeneous temperature distribution in the component, which becomes more pronounced with increasing sample size. If exceeding a critical value, density and/or stress gradients in the sintered part result. There are also limitations with respect to the maximum height/diameter ratio. Similar to conventional pressing, wall friction can cause density gradients in the sintered part.
* '''Chemical and electrochemical interaction with the tool materials:''' The direct contact of the powder with the tools is advantageous with respect to heat transfer, but in the worst case it also leads to a chemical interaction with the tools or the inserted foils. When using graphite tools or foils, possible contamination of the component with carbon must be taken carefully into account. Therefore, adhering residues of the graphite foil and the reaction zone on the component surface must be removed mechanically, e.g. by grinding. In addition, it must be noted that the electrical field applied to the powder can trigger electrochemical reactions at the interfaces. A well-known effect is electrochemical blackening of oxide ceramics caused by the release of oxygen at low oxygen partial pressures. Furthermore, oxide ceramics that contain transition metals at the A or B position are sensitive to chemical expansion, which in the worst case leads to severe cracking in the component.
* '''Change of conductivity of semi-conductive and mixed-conductive materials:''' When sintering semi-conductive and mixed-conductive materials via FAST/SPS, it should be noted that the conductivity of the powder changes with increasing temperature and density during the FAST/SPS cycle. If the heating at the beginning of the sintering cycle is primarily based on heat conduction, this state might change suddenly if a current flow through the sample becomes possible when the temperature exceeds a specific value. The result is a complex sintering process that becomes difficult to control and which can impair reproducibility. This effect is used for specific kinds of field-assisted sintering, e.g. for flash sintering. For more details, see Chapter 8.
* '''Net-shaping:''' The FAST/SPS process reaches its limits when complex shapes are to be realized. In addition to the challenges of suitable tool design, increasing geometrical complexity might cause inhomogeneous temperature distribution and, in the case of conductive powders, inhomogeneous current flow over the entire sample cross-section. There are a number of approaches to manufacture complex shapes e.g. by using split tools or by sintering near net-shaped green parts in a powder bed directly via FAST/SPS. However, the possibilities for automating these technologies must be evaluated critical.
* '''Automation of the FAST/SPS process:''' At current state of development, cycle times in FAST/SPS systems cannot compete with conventional pressing and sintering, since a complete FAST/SPS cycle takes several minutes despite high heating rates and short dwell times. If insert foils are used to improve the electrical and thermal contact during tool assembly, this slows down the cycle time further. In order to operate FAST/SPS devices with higher productivity, partially automated, multiple tools (capacity up to several hundred components) are in use, which can optionally be filled with a robot system outside the device and then installed in the device via a manipulator. Another concept are FAST/SPS devices with a system of separate chambers in which the individual processing steps of tool assembly, powder filling, compression and cooling are carried out in a separate and sequential manner.

== How to conduct a standard FAST/SPS cycle ==
In this section, the processing steps for sintering a ceramic powder via FAST/SPS are explained in detail. For conducting FAST/SPS cycles, the following three devices are available at the institute IEK-1 ('''Figure 3''').

'''-> Figure 3''' 
'''Figure 3:''' ''FAST/SPS devices at the institute IEK-1 '''a.)''' Laboratory device HP-D 5 '''b.)''' Hybrid sintering system H-HP-D25 SD/FL/MoSi '''c.)''' Sintering press DSP515 on industrial scale.''

The '''HP-D 5 laboratory device''' is characterized by the following operating parameters:
* Type: HP-D 5
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 50 kN
* Maximum heating power: 37 kW
* Maximum sample diameter: 30 mm
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operating mode: FAST / SPS with pulsed direct current

The '''hybrid sintering device H-HP-D25 SD/FL/MoSi''' enables a number of different operating modes in addition to the conventional FAST/SPS mode through the optional application of additional heaters or operation with an external voltage source.
* Type: H-HP-D25 SD/FL/MoSi
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 250 kN
* Maximum sample diameter: 100 mm (FAST/SPS mode), 20 mm (Flash sintering mode)
* Maximum heating power (FAST / SPS): 60 kW
* Maximum heating power (Induction): 80 kW
* Maximum heating power (MoSi2): 10 kW
* Maximum heating power (Hybrid heating): 100 kW
* External voltage source: AC/DC, 1000 V, max. 25 A
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operation modes: i.) FAST / SPS with pulsed direct current ii.) Hybrid FAST/SPS with induction coil or MoSi2 furnace as additional heater iii.) Hot press with MoSi2 heater iv.) Flash SPS with defined heating power v.) Flash sintering with an external voltage source and MoSi2 heater.

The '''DSP515 sintering press''' is a device, which can be used for industrial production and enables the scaling up of promising results from experiments on lab-scale.
* Type: DSP515
* Manufacturer: Dr. Fritsch Sondermaschinen GmbH, Fellbach, Germany
* Maxiumum pressing force: 555 kN
* Electrode size: 180 x 180 mm2
* Maximum sample size: approx. 160 x 160 mm2
* Maximum heating power: 170 kW
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2
* Operating modes: i.) FAST/SPS with constant direct current ii.) Flash SPS with defined heating power.
* Debinding unit: The system is also equipped with a cooling trap for debinding of tape-cast parts.

Below, the steps of a standard FAST/SPS cycle using a graphite tool with a sample diameter of 20 mm are described. An additional graphite foil (thickness approx. 0.35 mm) is inserted into the graphite tool. The thickness of the foil must be taken into account when designing the tool. The inserted foil has two main functions. On the one hand, it improves the electrical and thermal contact between the punch and the die as well as between the powder, the face of the punch and the die. On the other hand, it avoids chemical interactions between powder and tool, so that the tool life is increased. The FAST/SPS cycle shown here was carried out in the HP-D 5 laboratory device.

i.) '''Sample preparation:''' '''Figure 4''' shows the parts of a lab-scale graphite tool (inner diameter 20 mm) as well as the graphite insert foils (thickness 0.35 mm), which are sized with respect to the tool dimensions. In a first step, the graphite foils are positioned on the inner wall of the die and on the faces of the punches. It is important that the foils has a tight contact to the tool components and that there are no kinks or gaps after positioning. For health protection, the graphite tool should be filled in a laboratory hood. Filling can be carried out on a balance. This increases the accuracy of the powder quantity weighed in.

'''-> Figure 4''' 
'''Figure 4:''' ''Preparation of the graphite tool and the insert foil for the FAST/SPS cycle. For accurate sample preparation, the powder should be directly balanced in the tool. Furthermore, it is recommended to handle the powder in a hood.''

After filling in the tool, the powder is covered with an additional graphite foil and pre-pressed in a manual laboratory press with 50 MPa (16 KN for diameter 20 mm tool) ('''Figure 5'''). In order to avoid sticking of powder particles on the face the upper punch, the upper punch is removed again and powder residues are manually removed. Afterwards, the upper punch is placed again in the tool.

'''-> Figure 5''' 
'''Figure 5:''' '''''a.)''' Filling the mold and positioning the graphite foil '''b.)''' Pre-pressing of the FAST/SPS sample in a manual hand press '''c.)''' Removal of the upper punch after the pressing process and removal of adhering powder particles.''

ii.) '''Mounting of the tool and programming the FAST/SPS device:''' At the laboratory system HP-D 5, the programming of the FAST/SPS parameters can be done via a process controller type Stange SE607 ('''Figure 6'''). The main operating parameters temperature, pressing force, pulse length of the current and moving speed of the lower electrode is programmed in individual program segments. During the FAST/SPS cycle, all process data are shown on the controller display as a numerical values and as a time-resolved graph. In parallel, all data are saved via a data logger integrated in the system. By default, the data are transferred to an external PC for data management and further evaluation. Individual parameter sets of the users are also stored on the PC and can be easily transferred to the controller if required.

'''-> Figure 6''' 
'''Figure 6:''' ''Display of the controller of the HP-D 5 device giving a compact overview of all process-relevant data.''

'''Figure 7''' shows the graphite tool mounted into the HP-D 5 devices as well as the CuBe electrodes. Optionally, the graphite tool can be thermally isolated with a jacket made of a graphite felt (not shown here). A graphite cord can be used to fix the graphite felt on the tool.

'''-> Figure 7''' 
'''Figure 7:''' ''View on the processing chamber of the HP-D 5 device with mounted graphite tool. When installing the tool and the two cones, it should be noted that graphite is a brittle and shock-sensitive material and therefore breaks very easily. For this reason, sudden contact of all graphite parts with the other system components (stamp, chamber walls) must be avoided.''

After the graphite tool has been inserted and fixed by lifting the lower punch, the container door is closed and the FAST/SPS cycle can be started.

iii.) '''Choice and regulation of the sintering atmosphere:''' A FAST/SPS cycle is usually carried out in vacuum or under protective gas atmosphere. Accordingly, the process chamber is evacuated by a vacuum pump at the beginning of the cycle. In the laboratory device HP-D 5, a vacuum of approx. 0.5 mbar is achieved; in larger systems, this value can also be higher (e.g. 20 mbar for the DSP515). The quality of the vacuum depends on the sealing of the process chamber and the power of the vacuum pump. If aiming on a high vacuum, cost of the FAST/SPS device significantly increases. After evacuation, the chamber can optionally be flooded with gases such as N2, Ar or Ar/H2 (static atmosphere control) or a continuous gas flow (dynamic atmosphere control). Figure 8 shows the valves for feeding the individual gases from the institute's gas store into the system. The evacuation of the process chamber and the optional supply of protective gases to the process chamber is regulated by the system control and takes place automated. The pressure in the process chamber is continuously recorded in the HP-D 5 device by two sensors with different measuring ranges (coarse sensor 1.0 - 1300 mbar, fine sensor 0.01 - 13 mbar), which are positioned at the gas outlet. For operation of the system under relative pressure (reduced pressure in relation to the ambient pressure), the system is also equipped with a relative pressure sensor, which enables to regulate the relative pressure in the range of 5 - 50 mbar. Static or dynamic operation is also possible in the relative pressure mode. A safety valve is used to protect the processing chamber against overpressure. The valve opens at an overpressure of 100 mbar above the ambient pressure. The pressure curve during the FAST/SPS cycle is recorded continuously. An analysis of the pressure curve can be helpful if components outgas from the sample or if the sample decomposes under the FAST/SPS conditions.

'''-> Figure 8''' 
'''Figure 8:''' ''Valves for flooding the processing chamber with the protective gases Ar, N2, Ar/H2.''

When sintering oxide ceramics via FAST/SPS, it should be noted that the sintering conditions have a reducing effect, i.e. there is a release oxygen atoms from the lattice, which increases with decreasing oxygen partial pressure. The effect is aggravated in the case of direct contact with the graphite tools or the graphite foils. The release of oxygen is visually noticeable in the darkening of the ceramic. This effect is superimposed by the uptake of carbon. If the release of oxygen exceeds a critical value, the sample can undergo chemical expansion, which can be up to several percent (as e.g. the case for gadolinium-doped cerium oxide or barium-strontium-cobalt oxides). Usually, this effect leads to severe cracking of the sample. Furthermore, the crystal lattice can become unstable if the oxygen release progresses further. In worst case, reduction of components down to the metallic phase might appear.

In principle, it is possible to operate a FAST/SPS device with technical air. Such operation must be done with special care, since most materials used for the tools are unstable in air and start to strongly oxidize if the temperature exceeds a critical value (usually around 400°C). It should also be noted that the powder in the tool is encapsulated in such a way that the access of oxygen to the powder is prevented to a large extent.

iv.) '''Performing of the FAST/SPS cycle:''' After the device has been prepared, the selected program is started and runs automatically. '''Figure 9''' shows the graphite die during the heating process. As already mentioned, the operation of FAST/SPS devices is usually temperature-controlled. This means that the controller defines the temperature and the system regulates the current and voltage in such a way that the temperature profile is adhered to the specification as precisely as possible. In order to keep the deviations from the programmed temperature curve as low as possible, the system is equipped with a PID control (PID = Proportional-Integral-Derivative). This control unit iteratively adapt the optimal current and voltage curves for heating the tool to the respective electrical resistance of the tool.

'''-> Figure 9''' 
'''Figure 9:''' ''View on the heated graphite tool (punch diameter 20 mm) in the laboratory device HP-D 5. When operating a FAST/SPS system, it should be noted that the high currents in the system cause strong electromagnetic fields, which can damage pacemakers and others sensitive electronic devices.''

v.) Demoulding of the samples
At the end of the cycle, the sample can be pressed out of the graphite tool using a hand press, as shown in '''Figure 10'''.

'''-> Figure 10''' 
'''Figure 10:''' ''Demoulding the sample from the FAST/SPS tool using a hand press. When removing the tool from the FAST/SPS device, please take care since the tool can still be hot.''

== Tool design and tool materials ==
In most cases, graphite tools are used in FAST/SPS systems. '''Figure 11''' shows a selection of graphite tools for the laboratory system HP-D 5 with punch diameters of 12, 20 and 30 mm and for the hybrid sintering device H-HP-D25 with a punch diameter of 100 mm.

'''-> Figure 11''' 
'''Figure 11:''' ''Graphite tools for performing FAST/SPS cycles '''a.)''' Overview: die, punch with hole for pyrometer, cone for adaptation to the geometry of the electrodes of the FAST/SPS device '''b.)''' Tools for the laboratory device HP-D 5 with a diameter of 12, 20 and 30 mm and '''c.)''' Tools for the hybrid sintering device H-HP-D25 with a diameter of 100 mm.''

The use of graphite has the advantage that it is easy to machine the tools. Furthermore, it has an electrical resistance that is favorable for Joule heating. Temperatures of up to around 2,200 °C can be achieved in graphite tools. The compressive strength of standard grades is approx. 50 - 100 MPa (e.g. Sigrafine R7710, SGL Carbon GmbH), special grades achieve compressive strengths of up to 230 MPa (e.g. Grade 2334, Mersen). It should be noted that the geometry of the tool also has an influence on the maximum permissible pressure, e.g. the notch effect of a hole drilled for temperature measurement can lead to failure of the tool even at low pressures. Above 450 °C, graphite tools can only be used in a vacuum or under protective gas (e.g. Ar). If a tool is used frequently, attention must also be paid to possible wear, which can reduce the dimensional accuracy of the sintered parts.

If pressures well above 100 MPa or long tool life are desired, the following materials can used as alternative to graphite. At temperatures up to 600 °C, the use of a high-speed steel (e.g. W360, Böhler) is recommended, which can resist pressures of up to 400 MPa. If higher temperatures are desired, Mo alloys (e.g. Ti-Zr-Mo TZM, Plansee) can be used, which enable maximum temperature of approx. 1100 ° C and maximum pressure of 350 MPa. The maximum operating temperature of metal tools is limited by the onset of creep processes and severe grain coarsening. Both effects can cause a macroscopic deformation of the tools, so that in the worst case the punch can become jammed in the die. '''Figure 12''' shows as an example tools made of W360 steel and TZM.

'''-> Figure 12''' 
'''Figure 12:''' ''Metallic tools '''a.)''' Overview: Die, punch, and cone of a tool made of W360 steel '''b.)''' Same tool in the assembled state '''c.)''' Similar tool made of TZM.''

If even higher temperatures or pressures are desired, the literature reports on tools made of conductive ceramics. Suitable materials are tungsten carbide or silicon carbide, which are already used in the laboratory up to pressures of 1000 MPa. When using ceramic tools, the high effort in production and the inherent brittleness must be taken into account. Careful handling is strictly required in order to avoid breakage.

When using metallic and ceramic tools, it should be noted that these materials usually have a different electrical resistance than graphite. This has an influence on the system control and may require an adjustment of the PID parameters for precise temperature control (see Chapter 4).

== Measurement of temperature ==
The temperature is the main parameter for controlling the FAST/SPS system. The exact measurement and control of temperature is one of the great challenges when applying of FAST/SPS technology. The high heating rates require a temperature measurement with short response time, short delay time and high reproducibility. A direct measurement of the sample temperature is not possible with reasonable effort. Therefore, the measurement should be conducted as close to the sample as possible. For this purpose, vertical or horizontal holes are usually drilled in the FAST/SPS tool. By adjusting the pyrometer or thermocouple at the bottom of these holes, the temperature can be measured in direct vicinity of the sample.

i.) '''Measurement of the temperature with the pyrometer:''' Pyrometers are preferably used for temperature measurement at high temperatures. The usual measuring range of pyrometers is 600 - 3000 °C. '''Figure 13a''' shows the pyrometer installed in the HP-D 5 laboratory device. In this case, the measurement signal is deflected via a prism so that the measurement can be carried out vertically in a hole drilled in the upper punch.

In FAST / SPS systems with additional heater (e.g. hybrid sintering device H-HP-D 25), the pyrometer for controlling the additional heating is installed on the side. The measurement is carried out through a sight glass in the furnace door.

ii.) '''Measurement of the temperature with thermocouples:''' Thermocouples are necessarily required for a regulated temperature control of the system at temperatures < 600 °C, since pyrometers do not work reliably in this temperature range. There is also the option of using thermocouples at higher temperatures. Thermocouples of type K (Ni-CrNi) are suitable for the temperature range RT - 1100 ° C and are comparatively inexpensive. Because of the ductility of Ni, type K thermocouples are flexible. For protection, the thermocouples are enclosed in a steel jacket. Type C thermocouples (W5Re-W26Re) with a molybdenum housing enable temperature measurement in the range of RT - 2,200 ° C. The materials used are brittle and expensive, so that their application requires careful handling. Regardless of whether the housing is made of steel or molybdenum, care must be taken that there is no chemical interaction with the tool material during the sintering cycle. '''Figure 13b''' shows a graphite tool equipped with multiple type K thermocouples. One of the thermocouples is used for controlling the heating cycle by temperature measurement of the die and is flexibly installed. Two further thermocouples are firmly fixed to the upper and lower electrodes of the system and serve to protect the water-cooled CuBe electrodes from overheating.

'''-> Figure 13''' 
'''Figure 13:''' ''Temperature measurement in the laboratory system HP-D 5 '''a.)''' Pyrometer for measuring the temperature of the upper punch, deflection of the measurement signal via a prism inside the device '''b.)''' Flexible thermocouples of type K. When installing the thermocouples, it must made sure that there is no contact between the thermocouple and the container wall in order to avoid short circuiting.''

In general, it should be noted that temperature differences of significantly more than 10 K can occur between the pyrometer and thermocouples when identical operating parameters are used. In order to be able to predict the temperature distribution in the component with good accuracy, it is highly recommended to carry out an accompanying FEM modeling of the temperature distribution. The combination of experiment and modeling is the basis for reliably designing the tools and achieving high reproducibility of the FAST/SPS cycles. Another possibility for estimating the temperature distribution is the use of a "dummy" tool without powder cavity, which is equipped with thermocouples in as many places as possible. It should also be noted that the temperature gradients increase with tool size. In industrial production, temperature gradients of up to 80 K can occur in multi-component tools (up to 500 components per cycle), especially at the beginning of the cycle. When supporting tool design by FEM modeling, temperature deviations can be reduced to below 20 K.

== Applications of FAST/SPS ==
The FAST/SPS process is established in industrial production, but it competes with conventional production routes like pressing and sintering, which is easier to automate, as well as hot pressing (HP) and hot isostatic pressing (HIP). Application of FAST/SPS technology is established in the following sectors:

i.) '''Diamond-reinforced materials:''' The rapid process control and the comparatively low sintering temperature prevent that the diamond particles are dissolved in the metallic matrix. At the same time, a good connection of the diamonds in the matrix is achieved. The high level of tool wear that occurs in conventional pressing is reliably avoided.

ii.) '''Multi-phase brake pads:''' High-performing brake pads are used in racing cars as well as in motorcycles, high-speed trains, bicycles and wind turbines. The FAST/SPS process is preferred if the required profile of properties cannot be achieved by conventional pressing and sintering.

iii.) '''Sputtering targets:''' Sputtering targets often combine elements and alloys that differ greatly in their physical properties (e.g. melting point). The FAST/SPS enables the direct production of the targets and avoids an additional pressing step at room temperature.

Further applications of FAST/SPS technology in the industrial environment are high-performing seals for pumps and motors, heat sinks for the electronic industry, thermoelectrics, wear materials and components made of boron carbide for defense technology and the nuclear industry.

The FAST / SPS process is widespread in research and development, as samples for material characterization can be easily produced from almost any ceramic or metallic powder with comparatively little experimental effort. However, care must be taken to ensure that the specific boundary conditions of the FAST/SPS process (reducing conditions, interaction with carbon, ...) do not inadmissibly change the material properties.

== Alternative operation modes of FAST/SPS devices ==
At the IEK-1 institute, the hybrid sintering device H-HP-D25 SD/FL /MoSi is operated, which, in addition to the conventional FAST/SPS mode, enables special kinds of field and pressure-assisted sintering. '''Figure 14''' gives a schematic overview of the options possible with this system.

'''-> Figure 14''' 
'''Figure 14:''' ''Special forms of field and pressure-assisted sintering '''a.)''' Hybrid FAST/SPS with additional heater (induction coil, MoSi2 heater) '''b.)''' Flash SPS setup '''c.)''' Flash sintering setup with an insulating die.''

i.) '''Hybrid FAST/SPS:''' The use of an additional heater placed in the processing chamber around the graphite tool enables to increase the heating rate and to improve the uniform temperature distribution in the sintered body. Either an induction heater or a MoSi2 heater can be mounted in the H-HP-D25 SD/FL/MoSi hybrid sintering device. When operating the MoSi2 heater, it must be considered that it is designed for operation in air and that it cannot easily be combined with materials usually applied in FAST/SPS. If a tool made from a non-conductive oxide ceramic (e.g. alumina or zirconia) is installed instead, the system can also be operated as a conventional hot press.

ii.) '''Flash Spark Plasma Sintering:''' The Flash SPS process is derived from Flash Sintering, which was firstly described in 2010. Flash SPS can be carried out with conventional FAST/SPS devices. In the Flash SPS configuration, a pre-pressed or pre-sintered powder compact is positioned between two graphite stamps and subjected to moderate pressure. A high-power current pulse (several tens of kW) of a defined length (usually only a few seconds) is then passed through the sample. The sample heats up at very high heating rates directly via the Joule effect. The Flash SPS process is characterized by the simultaneous compression and hot deformation of the sample. At very moderate pressures (around 30 MPa), high degrees of deformation are achieved. The rapid densification enables that nanoscale structures can be retained, provided that the appropriate starting powder is available. Attempts are currently being made to optimize the process for sintering NdFeB magnets with anisotropic properties. The Flash SPS process has so far only been demonstrated on a laboratory scale.

iii.) '''Flash Sintering:''' The term “flash sintering” was introduced in 2010 by Prof. Rishi Raj, University of Boulder. This special form of sintering is characterized by the almost complete full densification of semi-finished ceramic compacts within a few seconds (usually <5 s). The effect is preferably observed on semiconducting oxide powders. A pre-pressed or pre-sintered body is contacted at the end faces via metallic electrodes (e.g. platinum applied via paste technology). To improve the electrical contact and to support the sintering process, a moderate pressure (a few MPa) can also be brought to the sample via the stamp system. An electric field is then applied via the external power source. The external power source available in the H-HP-D25 SD/FL/MoSi hybrid sintering device supplies direct or alternating voltage of up to 1000 V with a maximum current of 25 A. The relatively low current of the external power source limits the maximum sample diameter to around 20 mm on. To initiate flash sintering, the sample is heated via the external heater to an onset temperature at which a continuous current flow through the sample starts. During the flash, the current flow over the sample increases avalanche like and the sample can be sintered to almost full density within a few seconds. In order to avoid uncontrolled melting of the sample, the current density must be limited to a controlled value immediately after the flash occurs. Flash sintering has so far only been successfully demonstrated in the laboratory. The scaling up of the technology is challenging due to the occurrence of so-called "hot spots" (localized current paths in the powder compact).

Field assisted sintering technology/spark plasma sintering

2021-08-05T07:07:12Z

M.bram: /* Alternative operation modes of FAST/SPS devices */

== General principle of FAST/SPS ==
Field Assisted Sintering Technology/Spark Plasma Sintering (FAST/SPS) is a low-voltage, current-activated and pressure-supported sintering process that is based on Joule heating (= resistance heating) of the conductive tools ('''Figure 1''') and is characterized by high heating rates and short cycle times. If electrically conductive powders are applied, the powder itself is also heated directly via the Joule effect. The FAST/SPS process is established in the industry and particularly promising when powders are to be sintered, which have a low sintering activity or an unfavorable particle morphology and particle size distribution for conventional pressing and sintering. Furthermore, the method is well suited for the production of composite materials, especially when phases will be combined, which have very different physical properties. Some typical application examples of FAST/SPS technology are presented in Chapter 7. Due to the great flexibility, the short cycle times and the comparatively simple and cost-effective production of tools, research and development is another important field of application for FAST/SPS technology and is widespread there.

[[File:Wiki Keramik FAST SPS Abb 01.jpg|thumb|center]]
'''Figure 1:''' ''Heated graphite tool in a FAST / SPS device.''

In principle, a FAST/SPS device is a mechanical press, which at the same time also forms a high-energy current circuit. The FAST/SPS process is carried out in a conductive tool consisting of two punches and a die. Two additional cones establish the contact with the device's electrodes. The pressing force is also applied via these electrodes by means of a hydraulic pressure cylinder. '''Figure 2''' shows a schematic sketch of such a device. FAST/SPS processes are usually carried out in a vacuum or protective gas to protect the tool and the powder inside the tool from oxidation. Accordingly, the pressing device is located in a water-cooled chamber, in which a moderate vacuum (0.5 - 20 mbar) or a defined protective gas atmosphere (e.g. Ar or N2) can be set. The heating of the tool via the Joule effect requires the use of conductive materials for the punch and the die. The standard material for punch and die is graphite, alternatives to this are introduced in Chapter 4.

[[File:Wiki Keramik FAST SPS Abb 02 englisch.jpg|thumb|center]]
'''Figure 2:''' ''Schematic sketch of a FAST/SPS device.''

The tool is heated by a continuous or pulsed direct current with moderate voltages <10 V and high currents in the range from 1 to several 10 kA (depending on the size of the device). Non-conductive powders can also be sintered in good quality via FAST/SPS. Here, the direct contact between the tool and the powder leads to rapid heat transfer and relatively even heating over the entire cross-section of the sample. The heating takes place primarily via thermal conduction. In order to reduce the heat loss through thermal radiation, the die can optionally be thermally insulated, e.g. with a graphite felt. In the standard configuration, heating rates of up to approx. 300 K/min can be achieved in a FAST/SPS device. The high heating rates are one of the main reasons for the fast cycle times, as grain boundary and volume diffusion necessary for mass transport during sintering are activated directly. Due to the thermal mass of the tools, extremely high cooling rates cannot be achieved. Typical cooling rates are around 100 - 150 K/min. It should be noted here that the use of thermal insulation materials further reduces the cooling rates. In addition to the rapid heating, the sintering kinetics are also supported by the applied load. Depending on the type of system and sample size, compaction pressure in the range of 50 - 100 MPa can be achieved with the standard material graphite. Special grades of graphite allow maximum pressures of up to 200 MPa. When using graphite tools, temperatures of up to approx. 2,200 °C can be achieved in FAST/SPS devices. Alternative tools made of highly heat-resistant metals or electrically conductive ceramics enable pressures of up to 400 MPa, but the maximum permissible sintering temperatures are usually significantly lower in these cases. In order to improve the electrical contact between the punches, the die and the sample, a flexible, ideally electrically conductive foil is usually positioned between the punches and the sample. Graphite has also proven to be the standard material for this foil. FAST/SPS systems are usually controlled by programming the temperature-time curve. The measurement of the temperature as a major process parameter is carried out by axially or radially arranged pyrometers or by thermocouples. A direct measurement of the sample temperature is usually not possible. In order to measure the temperature as close as possible to the sample, holes are often drilled in the tools, at the bottom of which the temperature is measured. Furthermore, especially with increasing size of sintered parts and complexity of shape, it is recommended to predict the temperature distribution in the parts using suitable FEM modeling.

== Advantages and limitations of FAST/SPS ==
i.) '''Advantages:''' An essential feature of the FAST/SPS process is the rapid heating of the sample, which is based on the direct heating of the tool and the good heat transfer between the die and the powder. The superimposition of an uniaxial pressure during sintering further accelerates the sintering kinetics, so that the sintering temperature can often be significantly reduced compared to conventional sintering processes. Accordingly, the FAST/SPS process is a promising technology for

* '''Powder with low sintering activity:''' FAST/SPS enables the compaction of powders that have a low sintering activity (e.g. borides, carbides, nitrides and their mixtures).
* '''Powders with unfavorable powder properties:''' Powders can be sintered whose particle size distribution and morphology are unsuitable for conventional pressing and sintering.
* '''Nanoscale powders:''' The rapid processing in the case of FAST/SPS makes it possible to preserve the structure of nanoscale powders in the component.
* '''Materials with limited stability:''' FAST/SPS enables the sintering of materials that tend to decompose at high temperatures and long dwell times and to form undesirable secondary phases.
* '''Materials containing phases out of thermodynamic equilibrium:''' Phases out of thermodynamic equilibrium can be maintained in the sintered part (e.g. amorphous phases). Based on this, properties can be achieved that are not feasible with other sintering methods.
* '''Composite materials:''' FAST/SPS has great potential for sintering of composite materials that combine phases, which have large differences in their physical properties (e.g. very different melting points).
* '''Energy-efficient processing:''' In general, the FAST/SPS process is classified as an energy-efficient process due to the reduced sintering temperature and the short cycle times, but the degree of automation and the number of components per sintering cycle must also be taken carefully into account for an objective comparison with other sintering technologies.

ii.) '''Limitations:''' Despite the obvious advantages of FAST/SPS technology, there are also a number of process-related limitations.
* '''Risk of density and stress gradients in the component:''' If powders with a low thermal conductivity and high electrical resistance are sintered by FAST/SPS, there might arise an inhomogeneous temperature distribution in the component, which becomes more pronounced with increasing sample size. If exceeding a critical value, density and/or stress gradients in the sintered part result. There are also limitations with respect to the maximum height/diameter ratio. Similar to conventional pressing, wall friction can cause density gradients in the sintered part.
* '''Chemical and electrochemical interaction with the tool materials:''' The direct contact of the powder with the tools is advantageous with respect to heat transfer, but in the worst case it also leads to a chemical interaction with the tools or the inserted foils. When using graphite tools or foils, possible contamination of the component with carbon must be taken carefully into account. Therefore, adhering residues of the graphite foil and the reaction zone on the component surface must be removed mechanically, e.g. by grinding. In addition, it must be noted that the electrical field applied to the powder can trigger electrochemical reactions at the interfaces. A well-known effect is electrochemical blackening of oxide ceramics caused by the release of oxygen at low oxygen partial pressures. Furthermore, oxide ceramics that contain transition metals at the A or B position are sensitive to chemical expansion, which in the worst case leads to severe cracking in the component.
* '''Change of conductivity of semi-conductive and mixed-conductive materials:''' When sintering semi-conductive and mixed-conductive materials via FAST/SPS, it should be noted that the conductivity of the powder changes with increasing temperature and density during the FAST/SPS cycle. If the heating at the beginning of the sintering cycle is primarily based on heat conduction, this state might change suddenly if a current flow through the sample becomes possible when the temperature exceeds a specific value. The result is a complex sintering process that becomes difficult to control and which can impair reproducibility. This effect is used for specific kinds of field-assisted sintering, e.g. for flash sintering. For more details, see Chapter 8.
* '''Net-shaping:''' The FAST/SPS process reaches its limits when complex shapes are to be realized. In addition to the challenges of suitable tool design, increasing geometrical complexity might cause inhomogeneous temperature distribution and, in the case of conductive powders, inhomogeneous current flow over the entire sample cross-section. There are a number of approaches to manufacture complex shapes e.g. by using split tools or by sintering near net-shaped green parts in a powder bed directly via FAST/SPS. However, the possibilities for automating these technologies must be evaluated critical.
* '''Automation of the FAST/SPS process:''' At current state of development, cycle times in FAST/SPS systems cannot compete with conventional pressing and sintering, since a complete FAST/SPS cycle takes several minutes despite high heating rates and short dwell times. If insert foils are used to improve the electrical and thermal contact during tool assembly, this slows down the cycle time further. In order to operate FAST/SPS devices with higher productivity, partially automated, multiple tools (capacity up to several hundred components) are in use, which can optionally be filled with a robot system outside the device and then installed in the device via a manipulator. Another concept are FAST/SPS devices with a system of separate chambers in which the individual processing steps of tool assembly, powder filling, compression and cooling are carried out in a separate and sequential manner.

== How to conduct a standard FAST/SPS cycle ==
In this section, the processing steps for sintering a ceramic powder via FAST/SPS are explained in detail. For conducting FAST/SPS cycles, the following three devices are available at the institute IEK-1 ('''Figure 3''').

'''-> Figure 3''' 
'''Figure 3:''' ''FAST/SPS devices at the institute IEK-1 '''a.)''' Laboratory device HP-D 5 '''b.)''' Hybrid sintering system H-HP-D25 SD/FL/MoSi '''c.)''' Sintering press DSP515 on industrial scale.''

The '''HP-D 5 laboratory device''' is characterized by the following operating parameters:
* Type: HP-D 5
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 50 kN
* Maximum heating power: 37 kW
* Maximum sample diameter: 30 mm
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operating mode: FAST / SPS with pulsed direct current

The '''hybrid sintering device H-HP-D25 SD/FL/MoSi''' enables a number of different operating modes in addition to the conventional FAST/SPS mode through the optional application of additional heaters or operation with an external voltage source.
* Type: H-HP-D25 SD/FL/MoSi
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 250 kN
* Maximum sample diameter: 100 mm (FAST/SPS mode), 20 mm (Flash sintering mode)
* Maximum heating power (FAST / SPS): 60 kW
* Maximum heating power (Induction): 80 kW
* Maximum heating power (MoSi2): 10 kW
* Maximum heating power (Hybrid heating): 100 kW
* External voltage source: AC/DC, 1000 V, max. 25 A
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operation modes: i.) FAST / SPS with pulsed direct current ii.) Hybrid FAST/SPS with induction coil or MoSi2 furnace as additional heater iii.) Hot press with MoSi2 heater iv.) Flash SPS with defined heating power v.) Flash sintering with an external voltage source and MoSi2 heater.

The '''DSP515 sintering press''' is a device, which can be used for industrial production and enables the scaling up of promising results from experiments on lab-scale.
* Type: DSP515
* Manufacturer: Dr. Fritsch Sondermaschinen GmbH, Fellbach, Germany
* Maxiumum pressing force: 555 kN
* Electrode size: 180 x 180 mm2
* Maximum sample size: approx. 160 x 160 mm2
* Maximum heating power: 170 kW
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2
* Operating modes: i.) FAST/SPS with constant direct current ii.) Flash SPS with defined heating power.
* Debinding unit: The system is also equipped with a cooling trap for debinding of tape-cast parts.

Below, the steps of a standard FAST/SPS cycle using a graphite tool with a sample diameter of 20 mm are described. An additional graphite foil (thickness approx. 0.35 mm) is inserted into the graphite tool. The thickness of the foil must be taken into account when designing the tool. The inserted foil has two main functions. On the one hand, it improves the electrical and thermal contact between the punch and the die as well as between the powder, the face of the punch and the die. On the other hand, it avoids chemical interactions between powder and tool, so that the tool life is increased. The FAST/SPS cycle shown here was carried out in the HP-D 5 laboratory device.

i.) '''Sample preparation:''' '''Figure 4''' shows the parts of a lab-scale graphite tool (inner diameter 20 mm) as well as the graphite insert foils (thickness 0.35 mm), which are sized with respect to the tool dimensions. In a first step, the graphite foils are positioned on the inner wall of the die and on the faces of the punches. It is important that the foils has a tight contact to the tool components and that there are no kinks or gaps after positioning. For health protection, the graphite tool should be filled in a laboratory hood. Filling can be carried out on a balance. This increases the accuracy of the powder quantity weighed in.

'''-> Figure 4''' 
'''Figure 4:''' ''Preparation of the graphite tool and the insert foil for the FAST/SPS cycle. For accurate sample preparation, the powder should be directly balanced in the tool. Furthermore, it is recommended to handle the powder in a hood.''

After filling in the tool, the powder is covered with an additional graphite foil and pre-pressed in a manual laboratory press with 50 MPa (16 KN for diameter 20 mm tool) ('''Figure 5'''). In order to avoid sticking of powder particles on the face the upper punch, the upper punch is removed again and powder residues are manually removed. Afterwards, the upper punch is placed again in the tool.

'''-> Figure 5''' 
'''Figure 5:''' '''''a.)''' Filling the mold and positioning the graphite foil '''b.)''' Pre-pressing of the FAST/SPS sample in a manual hand press '''c.)''' Removal of the upper punch after the pressing process and removal of adhering powder particles.''

ii.) '''Mounting of the tool and programming the FAST/SPS device:''' At the laboratory system HP-D 5, the programming of the FAST/SPS parameters can be done via a process controller type Stange SE607 ('''Figure 6'''). The main operating parameters temperature, pressing force, pulse length of the current and moving speed of the lower electrode is programmed in individual program segments. During the FAST/SPS cycle, all process data are shown on the controller display as a numerical values and as a time-resolved graph. In parallel, all data are saved via a data logger integrated in the system. By default, the data are transferred to an external PC for data management and further evaluation. Individual parameter sets of the users are also stored on the PC and can be easily transferred to the controller if required.

'''-> Figure 6''' 
'''Figure 6:''' ''Display of the controller of the HP-D 5 device giving a compact overview of all process-relevant data.''

'''Figure 7''' shows the graphite tool mounted into the HP-D 5 devices as well as the CuBe electrodes. Optionally, the graphite tool can be thermally isolated with a jacket made of a graphite felt (not shown here). A graphite cord can be used to fix the graphite felt on the tool.

'''-> Figure 7''' 
'''Figure 7:''' ''View on the processing chamber of the HP-D 5 device with mounted graphite tool. When installing the tool and the two cones, it should be noted that graphite is a brittle and shock-sensitive material and therefore breaks very easily. For this reason, sudden contact of all graphite parts with the other system components (stamp, chamber walls) must be avoided.''

After the graphite tool has been inserted and fixed by lifting the lower punch, the container door is closed and the FAST/SPS cycle can be started.

iii.) '''Choice and regulation of the sintering atmosphere:''' A FAST/SPS cycle is usually carried out in vacuum or under protective gas atmosphere. Accordingly, the process chamber is evacuated by a vacuum pump at the beginning of the cycle. In the laboratory device HP-D 5, a vacuum of approx. 0.5 mbar is achieved; in larger systems, this value can also be higher (e.g. 20 mbar for the DSP515). The quality of the vacuum depends on the sealing of the process chamber and the power of the vacuum pump. If aiming on a high vacuum, cost of the FAST/SPS device significantly increases. After evacuation, the chamber can optionally be flooded with gases such as N2, Ar or Ar/H2 (static atmosphere control) or a continuous gas flow (dynamic atmosphere control). Figure 8 shows the valves for feeding the individual gases from the institute's gas store into the system. The evacuation of the process chamber and the optional supply of protective gases to the process chamber is regulated by the system control and takes place automated. The pressure in the process chamber is continuously recorded in the HP-D 5 device by two sensors with different measuring ranges (coarse sensor 1.0 - 1300 mbar, fine sensor 0.01 - 13 mbar), which are positioned at the gas outlet. For operation of the system under relative pressure (reduced pressure in relation to the ambient pressure), the system is also equipped with a relative pressure sensor, which enables to regulate the relative pressure in the range of 5 - 50 mbar. Static or dynamic operation is also possible in the relative pressure mode. A safety valve is used to protect the processing chamber against overpressure. The valve opens at an overpressure of 100 mbar above the ambient pressure. The pressure curve during the FAST/SPS cycle is recorded continuously. An analysis of the pressure curve can be helpful if components outgas from the sample or if the sample decomposes under the FAST/SPS conditions.

'''-> Figure 8''' 
'''Figure 8:''' ''Valves for flooding the processing chamber with the protective gases Ar, N2, Ar/H2.''

When sintering oxide ceramics via FAST/SPS, it should be noted that the sintering conditions have a reducing effect, i.e. there is a release oxygen atoms from the lattice, which increases with decreasing oxygen partial pressure. The effect is aggravated in the case of direct contact with the graphite tools or the graphite foils. The release of oxygen is visually noticeable in the darkening of the ceramic. This effect is superimposed by the uptake of carbon. If the release of oxygen exceeds a critical value, the sample can undergo chemical expansion, which can be up to several percent (as e.g. the case for gadolinium-doped cerium oxide or barium-strontium-cobalt oxides). Usually, this effect leads to severe cracking of the sample. Furthermore, the crystal lattice can become unstable if the oxygen release progresses further. In worst case, reduction of components down to the metallic phase might appear.

In principle, it is possible to operate a FAST/SPS device with technical air. Such operation must be done with special care, since most materials used for the tools are unstable in air and start to strongly oxidize if the temperature exceeds a critical value (usually around 400°C). It should also be noted that the powder in the tool is encapsulated in such a way that the access of oxygen to the powder is prevented to a large extent.

iv.) '''Performing of the FAST/SPS cycle:''' After the device has been prepared, the selected program is started and runs automatically. '''Figure 9''' shows the graphite die during the heating process. As already mentioned, the operation of FAST/SPS devices is usually temperature-controlled. This means that the controller defines the temperature and the system regulates the current and voltage in such a way that the temperature profile is adhered to the specification as precisely as possible. In order to keep the deviations from the programmed temperature curve as low as possible, the system is equipped with a PID control (PID = Proportional-Integral-Derivative). This control unit iteratively adapt the optimal current and voltage curves for heating the tool to the respective electrical resistance of the tool.

'''-> Figure 9''' 
'''Figure 9:''' ''View on the heated graphite tool (punch diameter 20 mm) in the laboratory device HP-D 5. When operating a FAST/SPS system, it should be noted that the high currents in the system cause strong electromagnetic fields, which can damage pacemakers and others sensitive electronic devices.''

v.) Demoulding of the samples
At the end of the cycle, the sample can be pressed out of the graphite tool using a hand press, as shown in '''Figure 10'''.

'''-> Figure 10''' 
'''Figure 10:''' ''Demoulding the sample from the FAST/SPS tool using a hand press. When removing the tool from the FAST/SPS device, please take care since the tool can still be hot.''

== Tool design and tool materials ==
In most cases, graphite tools are used in FAST/SPS systems. '''Figure 11''' shows a selection of graphite tools for the laboratory system HP-D 5 with punch diameters of 12, 20 and 30 mm and for the hybrid sintering device H-HP-D25 with a punch diameter of 100 mm.

'''-> Figure 11''' 
'''Figure 11:''' ''Graphite tools for performing FAST/SPS cycles '''a.)''' Overview: die, punch with hole for pyrometer, cone for adaptation to the geometry of the electrodes of the FAST/SPS device '''b.)''' Tools for the laboratory device HP-D 5 with a diameter of 12, 20 and 30 mm and '''c.)''' Tools for the hybrid sintering device H-HP-D25 with a diameter of 100 mm.''

The use of graphite has the advantage that it is easy to machine the tools. Furthermore, it has an electrical resistance that is favorable for Joule heating. Temperatures of up to around 2,200 °C can be achieved in graphite tools. The compressive strength of standard grades is approx. 50 - 100 MPa (e.g. Sigrafine R7710, SGL Carbon GmbH), special grades achieve compressive strengths of up to 230 MPa (e.g. Grade 2334, Mersen). It should be noted that the geometry of the tool also has an influence on the maximum permissible pressure, e.g. the notch effect of a hole drilled for temperature measurement can lead to failure of the tool even at low pressures. Above 450 °C, graphite tools can only be used in a vacuum or under protective gas (e.g. Ar). If a tool is used frequently, attention must also be paid to possible wear, which can reduce the dimensional accuracy of the sintered parts.

If pressures well above 100 MPa or long tool life are desired, the following materials can used as alternative to graphite. At temperatures up to 600 °C, the use of a high-speed steel (e.g. W360, Böhler) is recommended, which can resist pressures of up to 400 MPa. If higher temperatures are desired, Mo alloys (e.g. Ti-Zr-Mo TZM, Plansee) can be used, which enable maximum temperature of approx. 1100 ° C and maximum pressure of 350 MPa. The maximum operating temperature of metal tools is limited by the onset of creep processes and severe grain coarsening. Both effects can cause a macroscopic deformation of the tools, so that in the worst case the punch can become jammed in the die. '''Figure 12''' shows as an example tools made of W360 steel and TZM.

'''-> Figure 12''' 
'''Figure 12:''' ''Metallic tools '''a.)''' Overview: Die, punch, and cone of a tool made of W360 steel '''b.)''' Same tool in the assembled state '''c.)''' Similar tool made of TZM.''

If even higher temperatures or pressures are desired, the literature reports on tools made of conductive ceramics. Suitable materials are tungsten carbide or silicon carbide, which are already used in the laboratory up to pressures of 1000 MPa. When using ceramic tools, the high effort in production and the inherent brittleness must be taken into account. Careful handling is strictly required in order to avoid breakage.

When using metallic and ceramic tools, it should be noted that these materials usually have a different electrical resistance than graphite. This has an influence on the system control and may require an adjustment of the PID parameters for precise temperature control (see Chapter 4).

== Measurement of temperature ==
The temperature is the main parameter for controlling the FAST/SPS system. The exact measurement and control of temperature is one of the great challenges when applying of FAST/SPS technology. The high heating rates require a temperature measurement with short response time, short delay time and high reproducibility. A direct measurement of the sample temperature is not possible with reasonable effort. Therefore, the measurement should be conducted as close to the sample as possible. For this purpose, vertical or horizontal holes are usually drilled in the FAST/SPS tool. By adjusting the pyrometer or thermocouple at the bottom of these holes, the temperature can be measured in direct vicinity of the sample.

i.) '''Measurement of the temperature with the pyrometer:''' Pyrometers are preferably used for temperature measurement at high temperatures. The usual measuring range of pyrometers is 600 - 3000 °C. '''Figure 13a''' shows the pyrometer installed in the HP-D 5 laboratory device. In this case, the measurement signal is deflected via a prism so that the measurement can be carried out vertically in a hole drilled in the upper punch.

In FAST / SPS systems with additional heater (e.g. hybrid sintering device H-HP-D 25), the pyrometer for controlling the additional heating is installed on the side. The measurement is carried out through a sight glass in the furnace door.

ii.) '''Measurement of the temperature with thermocouples:''' Thermocouples are necessarily required for a regulated temperature control of the system at temperatures < 600 °C, since pyrometers do not work reliably in this temperature range. There is also the option of using thermocouples at higher temperatures. Thermocouples of type K (Ni-CrNi) are suitable for the temperature range RT - 1100 ° C and are comparatively inexpensive. Because of the ductility of Ni, type K thermocouples are flexible. For protection, the thermocouples are enclosed in a steel jacket. Type C thermocouples (W5Re-W26Re) with a molybdenum housing enable temperature measurement in the range of RT - 2,200 ° C. The materials used are brittle and expensive, so that their application requires careful handling. Regardless of whether the housing is made of steel or molybdenum, care must be taken that there is no chemical interaction with the tool material during the sintering cycle. '''Figure 13b''' shows a graphite tool equipped with multiple type K thermocouples. One of the thermocouples is used for controlling the heating cycle by temperature measurement of the die and is flexibly installed. Two further thermocouples are firmly fixed to the upper and lower electrodes of the system and serve to protect the water-cooled CuBe electrodes from overheating.

'''-> Figure 13''' 
'''Figure 13:''' ''Temperature measurement in the laboratory system HP-D 5 '''a.)''' Pyrometer for measuring the temperature of the upper punch, deflection of the measurement signal via a prism inside the device '''b.)''' Flexible thermocouples of type K. When installing the thermocouples, it must made sure that there is no contact between the thermocouple and the container wall in order to avoid short circuiting.''

In general, it should be noted that temperature differences of significantly more than 10 K can occur between the pyrometer and thermocouples when identical operating parameters are used. In order to be able to predict the temperature distribution in the component with good accuracy, it is highly recommended to carry out an accompanying FEM modeling of the temperature distribution. The combination of experiment and modeling is the basis for reliably designing the tools and achieving high reproducibility of the FAST/SPS cycles. Another possibility for estimating the temperature distribution is the use of a "dummy" tool without powder cavity, which is equipped with thermocouples in as many places as possible. It should also be noted that the temperature gradients increase with tool size. In industrial production, temperature gradients of up to 80 K can occur in multi-component tools (up to 500 components per cycle), especially at the beginning of the cycle. When supporting tool design by FEM modeling, temperature deviations can be reduced to below 20 K.

== Applications of FAST/SPS ==
The FAST/SPS process is established in industrial production, but it competes with conventional production routes like pressing and sintering, which is easier to automate, as well as hot pressing (HP) and hot isostatic pressing (HIP). Application of FAST/SPS technology is established in the following sectors:

i.) '''Diamond-reinforced materials:''' The rapid process control and the comparatively low sintering temperature prevent that the diamond particles are dissolved in the metallic matrix. At the same time, a good connection of the diamonds in the matrix is achieved. The high level of tool wear that occurs in conventional pressing is reliably avoided.

ii.) '''Multi-phase brake pads:''' High-performing brake pads are used in racing cars as well as in motorcycles, high-speed trains, bicycles and wind turbines. The FAST/SPS process is preferred if the required profile of properties cannot be achieved by conventional pressing and sintering.

iii.) '''Sputtering targets:''' Sputtering targets often combine elements and alloys that differ greatly in their physical properties (e.g. melting point). The FAST/SPS enables the direct production of the targets and avoids an additional pressing step at room temperature.

Further applications of FAST/SPS technology in the industrial environment are high-performing seals for pumps and motors, heat sinks for the electronic industry, thermoelectrics, wear materials and components made of boron carbide for defense technology and the nuclear industry.

The FAST / SPS process is widespread in research and development, as samples for material characterization can be easily produced from almost any ceramic or metallic powder with comparatively little experimental effort. However, care must be taken to ensure that the specific boundary conditions of the FAST/SPS process (reducing conditions, interaction with carbon, ...) do not inadmissibly change the material properties.

== Alternative operation modes of FAST/SPS devices ==
At the IEK-1 institute, the hybrid sintering device H-HP-D25 SD/FL /MoSi is operated, which, in addition to the conventional FAST/SPS mode, enables special kinds of field and pressure-assisted sintering. '''Figure 14''' gives a schematic overview of the options possible with this system.

'''-> Figure 14''' 
'''Figure 14:''' ''Special forms of field and pressure-assisted sintering a.) Hybrid FAST/SPS with additional heater (induction coil, MoSi2 heater) b.) Flash SPS setup c.) Flash sintering setup with an insulating die.''

i.) '''Hybrid FAST/SPS:''' The use of an additional heater placed in the processing chamber around the graphite tool enables to increase the heating rate and to improve the uniform temperature distribution in the sintered body. Either an induction heater or a MoSi2 heater can be mounted in the H-HP-D25 SD/FL/MoSi hybrid sintering device. When operating the MoSi2 heater, it must be considered that it is designed for operation in air and that it cannot easily be combined with materials usually applied in FAST/SPS. If a tool made from a non-conductive oxide ceramic (e.g. alumina or zirconia) is installed instead, the system can also be operated as a conventional hot press.

ii.) '''Flash Spark Plasma Sintering:''' The Flash SPS process is derived from Flash Sintering, which was firstly described in 2010. Flash SPS can be carried out with conventional FAST/SPS devices. In the Flash SPS configuration, a pre-pressed or pre-sintered powder compact is positioned between two graphite stamps and subjected to moderate pressure. A high-power current pulse (several tens of kW) of a defined length (usually only a few seconds) is then passed through the sample. The sample heats up at very high heating rates directly via the Joule effect. The Flash SPS process is characterized by the simultaneous compression and hot deformation of the sample. At very moderate pressures (around 30 MPa), high degrees of deformation are achieved. The rapid densification enables that nanoscale structures can be retained, provided that the appropriate starting powder is available. Attempts are currently being made to optimize the process for sintering NdFeB magnets with anisotropic properties. The Flash SPS process has so far only been demonstrated on a laboratory scale.

iii.) '''Flash Sintering:''' The term “flash sintering” was introduced in 2010 by Prof. Rishi Raj, University of Boulder. This special form of sintering is characterized by the almost complete full densification of semi-finished ceramic compacts within a few seconds (usually <5 s). The effect is preferably observed on semiconducting oxide powders. A pre-pressed or pre-sintered body is contacted at the end faces via metallic electrodes (e.g. platinum applied via paste technology). To improve the electrical contact and to support the sintering process, a moderate pressure (a few MPa) can also be brought to the sample via the stamp system. An electric field is then applied via the external power source. The external power source available in the H-HP-D25 SD/FL/MoSi hybrid sintering device supplies direct or alternating voltage of up to 1000 V with a maximum current of 25 A. The relatively low current of the external power source limits the maximum sample diameter to around 20 mm on. To initiate flash sintering, the sample is heated via the external heater to an onset temperature at which a continuous current flow through the sample starts. During the flash, the current flow over the sample increases avalanche like and the sample can be sintered to almost full density within a few seconds. In order to avoid uncontrolled melting of the sample, the current density must be limited to a controlled value immediately after the flash occurs. Flash sintering has so far only been successfully demonstrated in the laboratory. The scaling up of the technology is challenging due to the occurrence of so-called "hot spots" (localized current paths in the powder compact).

File:Wiki Keramik FAST SPS Abb 14 englisch.jpg

2021-08-05T07:04:35Z

M.bram:

Figure 14: Special forms of field and pressure-assisted sintering a.) Hybrid FAST/SPS with additional heater (induction coil, MoSi2 heater) b.) Flash SPS setup c.) Flash sintering setup with an insulating die.

Field assisted sintering technology/spark plasma sintering

2021-08-05T07:03:02Z

M.bram: /* Applications of FAST/SPS */

Field assisted sintering technology/spark plasma sintering

2021-08-05T07:01:31Z

M.bram: /* Measurement of temperature */

== General principle of FAST/SPS ==
Field Assisted Sintering Technology/Spark Plasma Sintering (FAST/SPS) is a low-voltage, current-activated and pressure-supported sintering process that is based on Joule heating (= resistance heating) of the conductive tools ('''Figure 1''') and is characterized by high heating rates and short cycle times. If electrically conductive powders are applied, the powder itself is also heated directly via the Joule effect. The FAST/SPS process is established in the industry and particularly promising when powders are to be sintered, which have a low sintering activity or an unfavorable particle morphology and particle size distribution for conventional pressing and sintering. Furthermore, the method is well suited for the production of composite materials, especially when phases will be combined, which have very different physical properties. Some typical application examples of FAST/SPS technology are presented in Chapter 7. Due to the great flexibility, the short cycle times and the comparatively simple and cost-effective production of tools, research and development is another important field of application for FAST/SPS technology and is widespread there.

[[File:Wiki Keramik FAST SPS Abb 01.jpg|thumb|center]]
'''Figure 1:''' ''Heated graphite tool in a FAST / SPS device.''

In principle, a FAST/SPS device is a mechanical press, which at the same time also forms a high-energy current circuit. The FAST/SPS process is carried out in a conductive tool consisting of two punches and a die. Two additional cones establish the contact with the device's electrodes. The pressing force is also applied via these electrodes by means of a hydraulic pressure cylinder. '''Figure 2''' shows a schematic sketch of such a device. FAST/SPS processes are usually carried out in a vacuum or protective gas to protect the tool and the powder inside the tool from oxidation. Accordingly, the pressing device is located in a water-cooled chamber, in which a moderate vacuum (0.5 - 20 mbar) or a defined protective gas atmosphere (e.g. Ar or N2) can be set. The heating of the tool via the Joule effect requires the use of conductive materials for the punch and the die. The standard material for punch and die is graphite, alternatives to this are introduced in Chapter 4.

[[File:Wiki Keramik FAST SPS Abb 02 englisch.jpg|thumb|center]]
'''Figure 2:''' ''Schematic sketch of a FAST/SPS device.''

The tool is heated by a continuous or pulsed direct current with moderate voltages <10 V and high currents in the range from 1 to several 10 kA (depending on the size of the device). Non-conductive powders can also be sintered in good quality via FAST/SPS. Here, the direct contact between the tool and the powder leads to rapid heat transfer and relatively even heating over the entire cross-section of the sample. The heating takes place primarily via thermal conduction. In order to reduce the heat loss through thermal radiation, the die can optionally be thermally insulated, e.g. with a graphite felt. In the standard configuration, heating rates of up to approx. 300 K/min can be achieved in a FAST/SPS device. The high heating rates are one of the main reasons for the fast cycle times, as grain boundary and volume diffusion necessary for mass transport during sintering are activated directly. Due to the thermal mass of the tools, extremely high cooling rates cannot be achieved. Typical cooling rates are around 100 - 150 K/min. It should be noted here that the use of thermal insulation materials further reduces the cooling rates. In addition to the rapid heating, the sintering kinetics are also supported by the applied load. Depending on the type of system and sample size, compaction pressure in the range of 50 - 100 MPa can be achieved with the standard material graphite. Special grades of graphite allow maximum pressures of up to 200 MPa. When using graphite tools, temperatures of up to approx. 2,200 °C can be achieved in FAST/SPS devices. Alternative tools made of highly heat-resistant metals or electrically conductive ceramics enable pressures of up to 400 MPa, but the maximum permissible sintering temperatures are usually significantly lower in these cases. In order to improve the electrical contact between the punches, the die and the sample, a flexible, ideally electrically conductive foil is usually positioned between the punches and the sample. Graphite has also proven to be the standard material for this foil. FAST/SPS systems are usually controlled by programming the temperature-time curve. The measurement of the temperature as a major process parameter is carried out by axially or radially arranged pyrometers or by thermocouples. A direct measurement of the sample temperature is usually not possible. In order to measure the temperature as close as possible to the sample, holes are often drilled in the tools, at the bottom of which the temperature is measured. Furthermore, especially with increasing size of sintered parts and complexity of shape, it is recommended to predict the temperature distribution in the parts using suitable FEM modeling.

== Advantages and limitations of FAST/SPS ==
i.) '''Advantages:''' An essential feature of the FAST/SPS process is the rapid heating of the sample, which is based on the direct heating of the tool and the good heat transfer between the die and the powder. The superimposition of an uniaxial pressure during sintering further accelerates the sintering kinetics, so that the sintering temperature can often be significantly reduced compared to conventional sintering processes. Accordingly, the FAST/SPS process is a promising technology for

* '''Powder with low sintering activity:''' FAST/SPS enables the compaction of powders that have a low sintering activity (e.g. borides, carbides, nitrides and their mixtures).
* '''Powders with unfavorable powder properties:''' Powders can be sintered whose particle size distribution and morphology are unsuitable for conventional pressing and sintering.
* '''Nanoscale powders:''' The rapid processing in the case of FAST/SPS makes it possible to preserve the structure of nanoscale powders in the component.
* '''Materials with limited stability:''' FAST/SPS enables the sintering of materials that tend to decompose at high temperatures and long dwell times and to form undesirable secondary phases.
* '''Materials containing phases out of thermodynamic equilibrium:''' Phases out of thermodynamic equilibrium can be maintained in the sintered part (e.g. amorphous phases). Based on this, properties can be achieved that are not feasible with other sintering methods.
* '''Composite materials:''' FAST/SPS has great potential for sintering of composite materials that combine phases, which have large differences in their physical properties (e.g. very different melting points).
* '''Energy-efficient processing:''' In general, the FAST/SPS process is classified as an energy-efficient process due to the reduced sintering temperature and the short cycle times, but the degree of automation and the number of components per sintering cycle must also be taken carefully into account for an objective comparison with other sintering technologies.

ii.) '''Limitations:''' Despite the obvious advantages of FAST/SPS technology, there are also a number of process-related limitations.
* '''Risk of density and stress gradients in the component:''' If powders with a low thermal conductivity and high electrical resistance are sintered by FAST/SPS, there might arise an inhomogeneous temperature distribution in the component, which becomes more pronounced with increasing sample size. If exceeding a critical value, density and/or stress gradients in the sintered part result. There are also limitations with respect to the maximum height/diameter ratio. Similar to conventional pressing, wall friction can cause density gradients in the sintered part.
* '''Chemical and electrochemical interaction with the tool materials:''' The direct contact of the powder with the tools is advantageous with respect to heat transfer, but in the worst case it also leads to a chemical interaction with the tools or the inserted foils. When using graphite tools or foils, possible contamination of the component with carbon must be taken carefully into account. Therefore, adhering residues of the graphite foil and the reaction zone on the component surface must be removed mechanically, e.g. by grinding. In addition, it must be noted that the electrical field applied to the powder can trigger electrochemical reactions at the interfaces. A well-known effect is electrochemical blackening of oxide ceramics caused by the release of oxygen at low oxygen partial pressures. Furthermore, oxide ceramics that contain transition metals at the A or B position are sensitive to chemical expansion, which in the worst case leads to severe cracking in the component.
* '''Change of conductivity of semi-conductive and mixed-conductive materials:''' When sintering semi-conductive and mixed-conductive materials via FAST/SPS, it should be noted that the conductivity of the powder changes with increasing temperature and density during the FAST/SPS cycle. If the heating at the beginning of the sintering cycle is primarily based on heat conduction, this state might change suddenly if a current flow through the sample becomes possible when the temperature exceeds a specific value. The result is a complex sintering process that becomes difficult to control and which can impair reproducibility. This effect is used for specific kinds of field-assisted sintering, e.g. for flash sintering. For more details, see Chapter 8.
* '''Net-shaping:''' The FAST/SPS process reaches its limits when complex shapes are to be realized. In addition to the challenges of suitable tool design, increasing geometrical complexity might cause inhomogeneous temperature distribution and, in the case of conductive powders, inhomogeneous current flow over the entire sample cross-section. There are a number of approaches to manufacture complex shapes e.g. by using split tools or by sintering near net-shaped green parts in a powder bed directly via FAST/SPS. However, the possibilities for automating these technologies must be evaluated critical.
* '''Automation of the FAST/SPS process:''' At current state of development, cycle times in FAST/SPS systems cannot compete with conventional pressing and sintering, since a complete FAST/SPS cycle takes several minutes despite high heating rates and short dwell times. If insert foils are used to improve the electrical and thermal contact during tool assembly, this slows down the cycle time further. In order to operate FAST/SPS devices with higher productivity, partially automated, multiple tools (capacity up to several hundred components) are in use, which can optionally be filled with a robot system outside the device and then installed in the device via a manipulator. Another concept are FAST/SPS devices with a system of separate chambers in which the individual processing steps of tool assembly, powder filling, compression and cooling are carried out in a separate and sequential manner.

== How to conduct a standard FAST/SPS cycle ==
In this section, the processing steps for sintering a ceramic powder via FAST/SPS are explained in detail. For conducting FAST/SPS cycles, the following three devices are available at the institute IEK-1 ('''Figure 3''').

'''-> Figure 3''' 
'''Figure 3:''' ''FAST/SPS devices at the institute IEK-1 '''a.)''' Laboratory device HP-D 5 '''b.)''' Hybrid sintering system H-HP-D25 SD/FL/MoSi '''c.)''' Sintering press DSP515 on industrial scale.''

The '''HP-D 5 laboratory device''' is characterized by the following operating parameters:
* Type: HP-D 5
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 50 kN
* Maximum heating power: 37 kW
* Maximum sample diameter: 30 mm
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operating mode: FAST / SPS with pulsed direct current

The '''hybrid sintering device H-HP-D25 SD/FL/MoSi''' enables a number of different operating modes in addition to the conventional FAST/SPS mode through the optional application of additional heaters or operation with an external voltage source.
* Type: H-HP-D25 SD/FL/MoSi
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 250 kN
* Maximum sample diameter: 100 mm (FAST/SPS mode), 20 mm (Flash sintering mode)
* Maximum heating power (FAST / SPS): 60 kW
* Maximum heating power (Induction): 80 kW
* Maximum heating power (MoSi2): 10 kW
* Maximum heating power (Hybrid heating): 100 kW
* External voltage source: AC/DC, 1000 V, max. 25 A
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operation modes: i.) FAST / SPS with pulsed direct current ii.) Hybrid FAST/SPS with induction coil or MoSi2 furnace as additional heater iii.) Hot press with MoSi2 heater iv.) Flash SPS with defined heating power v.) Flash sintering with an external voltage source and MoSi2 heater.

The '''DSP515 sintering press''' is a device, which can be used for industrial production and enables the scaling up of promising results from experiments on lab-scale.
* Type: DSP515
* Manufacturer: Dr. Fritsch Sondermaschinen GmbH, Fellbach, Germany
* Maxiumum pressing force: 555 kN
* Electrode size: 180 x 180 mm2
* Maximum sample size: approx. 160 x 160 mm2
* Maximum heating power: 170 kW
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2
* Operating modes: i.) FAST/SPS with constant direct current ii.) Flash SPS with defined heating power.
* Debinding unit: The system is also equipped with a cooling trap for debinding of tape-cast parts.

Below, the steps of a standard FAST/SPS cycle using a graphite tool with a sample diameter of 20 mm are described. An additional graphite foil (thickness approx. 0.35 mm) is inserted into the graphite tool. The thickness of the foil must be taken into account when designing the tool. The inserted foil has two main functions. On the one hand, it improves the electrical and thermal contact between the punch and the die as well as between the powder, the face of the punch and the die. On the other hand, it avoids chemical interactions between powder and tool, so that the tool life is increased. The FAST/SPS cycle shown here was carried out in the HP-D 5 laboratory device.

i.) '''Sample preparation:''' '''Figure 4''' shows the parts of a lab-scale graphite tool (inner diameter 20 mm) as well as the graphite insert foils (thickness 0.35 mm), which are sized with respect to the tool dimensions. In a first step, the graphite foils are positioned on the inner wall of the die and on the faces of the punches. It is important that the foils has a tight contact to the tool components and that there are no kinks or gaps after positioning. For health protection, the graphite tool should be filled in a laboratory hood. Filling can be carried out on a balance. This increases the accuracy of the powder quantity weighed in.

'''-> Figure 4''' 
'''Figure 4:''' ''Preparation of the graphite tool and the insert foil for the FAST/SPS cycle. For accurate sample preparation, the powder should be directly balanced in the tool. Furthermore, it is recommended to handle the powder in a hood.''

After filling in the tool, the powder is covered with an additional graphite foil and pre-pressed in a manual laboratory press with 50 MPa (16 KN for diameter 20 mm tool) ('''Figure 5'''). In order to avoid sticking of powder particles on the face the upper punch, the upper punch is removed again and powder residues are manually removed. Afterwards, the upper punch is placed again in the tool.

'''-> Figure 5''' 
'''Figure 5:''' '''''a.)''' Filling the mold and positioning the graphite foil '''b.)''' Pre-pressing of the FAST/SPS sample in a manual hand press '''c.)''' Removal of the upper punch after the pressing process and removal of adhering powder particles.''

ii.) '''Mounting of the tool and programming the FAST/SPS device:''' At the laboratory system HP-D 5, the programming of the FAST/SPS parameters can be done via a process controller type Stange SE607 ('''Figure 6'''). The main operating parameters temperature, pressing force, pulse length of the current and moving speed of the lower electrode is programmed in individual program segments. During the FAST/SPS cycle, all process data are shown on the controller display as a numerical values and as a time-resolved graph. In parallel, all data are saved via a data logger integrated in the system. By default, the data are transferred to an external PC for data management and further evaluation. Individual parameter sets of the users are also stored on the PC and can be easily transferred to the controller if required.

'''-> Figure 6''' 
'''Figure 6:''' ''Display of the controller of the HP-D 5 device giving a compact overview of all process-relevant data.''

'''Figure 7''' shows the graphite tool mounted into the HP-D 5 devices as well as the CuBe electrodes. Optionally, the graphite tool can be thermally isolated with a jacket made of a graphite felt (not shown here). A graphite cord can be used to fix the graphite felt on the tool.

'''-> Figure 7''' 
'''Figure 7:''' ''View on the processing chamber of the HP-D 5 device with mounted graphite tool. When installing the tool and the two cones, it should be noted that graphite is a brittle and shock-sensitive material and therefore breaks very easily. For this reason, sudden contact of all graphite parts with the other system components (stamp, chamber walls) must be avoided.''

After the graphite tool has been inserted and fixed by lifting the lower punch, the container door is closed and the FAST/SPS cycle can be started.

iii.) '''Choice and regulation of the sintering atmosphere:''' A FAST/SPS cycle is usually carried out in vacuum or under protective gas atmosphere. Accordingly, the process chamber is evacuated by a vacuum pump at the beginning of the cycle. In the laboratory device HP-D 5, a vacuum of approx. 0.5 mbar is achieved; in larger systems, this value can also be higher (e.g. 20 mbar for the DSP515). The quality of the vacuum depends on the sealing of the process chamber and the power of the vacuum pump. If aiming on a high vacuum, cost of the FAST/SPS device significantly increases. After evacuation, the chamber can optionally be flooded with gases such as N2, Ar or Ar/H2 (static atmosphere control) or a continuous gas flow (dynamic atmosphere control). Figure 8 shows the valves for feeding the individual gases from the institute's gas store into the system. The evacuation of the process chamber and the optional supply of protective gases to the process chamber is regulated by the system control and takes place automated. The pressure in the process chamber is continuously recorded in the HP-D 5 device by two sensors with different measuring ranges (coarse sensor 1.0 - 1300 mbar, fine sensor 0.01 - 13 mbar), which are positioned at the gas outlet. For operation of the system under relative pressure (reduced pressure in relation to the ambient pressure), the system is also equipped with a relative pressure sensor, which enables to regulate the relative pressure in the range of 5 - 50 mbar. Static or dynamic operation is also possible in the relative pressure mode. A safety valve is used to protect the processing chamber against overpressure. The valve opens at an overpressure of 100 mbar above the ambient pressure. The pressure curve during the FAST/SPS cycle is recorded continuously. An analysis of the pressure curve can be helpful if components outgas from the sample or if the sample decomposes under the FAST/SPS conditions.

'''-> Figure 8''' 
'''Figure 8:''' ''Valves for flooding the processing chamber with the protective gases Ar, N2, Ar/H2.''

When sintering oxide ceramics via FAST/SPS, it should be noted that the sintering conditions have a reducing effect, i.e. there is a release oxygen atoms from the lattice, which increases with decreasing oxygen partial pressure. The effect is aggravated in the case of direct contact with the graphite tools or the graphite foils. The release of oxygen is visually noticeable in the darkening of the ceramic. This effect is superimposed by the uptake of carbon. If the release of oxygen exceeds a critical value, the sample can undergo chemical expansion, which can be up to several percent (as e.g. the case for gadolinium-doped cerium oxide or barium-strontium-cobalt oxides). Usually, this effect leads to severe cracking of the sample. Furthermore, the crystal lattice can become unstable if the oxygen release progresses further. In worst case, reduction of components down to the metallic phase might appear.

In principle, it is possible to operate a FAST/SPS device with technical air. Such operation must be done with special care, since most materials used for the tools are unstable in air and start to strongly oxidize if the temperature exceeds a critical value (usually around 400°C). It should also be noted that the powder in the tool is encapsulated in such a way that the access of oxygen to the powder is prevented to a large extent.

iv.) '''Performing of the FAST/SPS cycle:''' After the device has been prepared, the selected program is started and runs automatically. '''Figure 9''' shows the graphite die during the heating process. As already mentioned, the operation of FAST/SPS devices is usually temperature-controlled. This means that the controller defines the temperature and the system regulates the current and voltage in such a way that the temperature profile is adhered to the specification as precisely as possible. In order to keep the deviations from the programmed temperature curve as low as possible, the system is equipped with a PID control (PID = Proportional-Integral-Derivative). This control unit iteratively adapt the optimal current and voltage curves for heating the tool to the respective electrical resistance of the tool.

'''-> Figure 9''' 
'''Figure 9:''' ''View on the heated graphite tool (punch diameter 20 mm) in the laboratory device HP-D 5. When operating a FAST/SPS system, it should be noted that the high currents in the system cause strong electromagnetic fields, which can damage pacemakers and others sensitive electronic devices.''

v.) Demoulding of the samples
At the end of the cycle, the sample can be pressed out of the graphite tool using a hand press, as shown in '''Figure 10'''.

'''-> Figure 10''' 
'''Figure 10:''' ''Demoulding the sample from the FAST/SPS tool using a hand press. When removing the tool from the FAST/SPS device, please take care since the tool can still be hot.''

== Tool design and tool materials ==
In most cases, graphite tools are used in FAST/SPS systems. '''Figure 11''' shows a selection of graphite tools for the laboratory system HP-D 5 with punch diameters of 12, 20 and 30 mm and for the hybrid sintering device H-HP-D25 with a punch diameter of 100 mm.

'''-> Figure 11''' 
'''Figure 11:''' ''Graphite tools for performing FAST/SPS cycles '''a.)''' Overview: die, punch with hole for pyrometer, cone for adaptation to the geometry of the electrodes of the FAST/SPS device '''b.)''' Tools for the laboratory device HP-D 5 with a diameter of 12, 20 and 30 mm and '''c.)''' Tools for the hybrid sintering device H-HP-D25 with a diameter of 100 mm.''

The use of graphite has the advantage that it is easy to machine the tools. Furthermore, it has an electrical resistance that is favorable for Joule heating. Temperatures of up to around 2,200 °C can be achieved in graphite tools. The compressive strength of standard grades is approx. 50 - 100 MPa (e.g. Sigrafine R7710, SGL Carbon GmbH), special grades achieve compressive strengths of up to 230 MPa (e.g. Grade 2334, Mersen). It should be noted that the geometry of the tool also has an influence on the maximum permissible pressure, e.g. the notch effect of a hole drilled for temperature measurement can lead to failure of the tool even at low pressures. Above 450 °C, graphite tools can only be used in a vacuum or under protective gas (e.g. Ar). If a tool is used frequently, attention must also be paid to possible wear, which can reduce the dimensional accuracy of the sintered parts.

If pressures well above 100 MPa or long tool life are desired, the following materials can used as alternative to graphite. At temperatures up to 600 °C, the use of a high-speed steel (e.g. W360, Böhler) is recommended, which can resist pressures of up to 400 MPa. If higher temperatures are desired, Mo alloys (e.g. Ti-Zr-Mo TZM, Plansee) can be used, which enable maximum temperature of approx. 1100 ° C and maximum pressure of 350 MPa. The maximum operating temperature of metal tools is limited by the onset of creep processes and severe grain coarsening. Both effects can cause a macroscopic deformation of the tools, so that in the worst case the punch can become jammed in the die. '''Figure 12''' shows as an example tools made of W360 steel and TZM.

'''-> Figure 12''' 
'''Figure 12:''' ''Metallic tools '''a.)''' Overview: Die, punch, and cone of a tool made of W360 steel '''b.)''' Same tool in the assembled state '''c.)''' Similar tool made of TZM.''

If even higher temperatures or pressures are desired, the literature reports on tools made of conductive ceramics. Suitable materials are tungsten carbide or silicon carbide, which are already used in the laboratory up to pressures of 1000 MPa. When using ceramic tools, the high effort in production and the inherent brittleness must be taken into account. Careful handling is strictly required in order to avoid breakage.

When using metallic and ceramic tools, it should be noted that these materials usually have a different electrical resistance than graphite. This has an influence on the system control and may require an adjustment of the PID parameters for precise temperature control (see Chapter 4).

== Measurement of temperature ==
The temperature is the main parameter for controlling the FAST/SPS system. The exact measurement and control of temperature is one of the great challenges when applying of FAST/SPS technology. The high heating rates require a temperature measurement with short response time, short delay time and high reproducibility. A direct measurement of the sample temperature is not possible with reasonable effort. Therefore, the measurement should be conducted as close to the sample as possible. For this purpose, vertical or horizontal holes are usually drilled in the FAST/SPS tool. By adjusting the pyrometer or thermocouple at the bottom of these holes, the temperature can be measured in direct vicinity of the sample.

i.) '''Measurement of the temperature with the pyrometer:''' Pyrometers are preferably used for temperature measurement at high temperatures. The usual measuring range of pyrometers is 600 - 3000 °C. '''Figure 13a''' shows the pyrometer installed in the HP-D 5 laboratory device. In this case, the measurement signal is deflected via a prism so that the measurement can be carried out vertically in a hole drilled in the upper punch.

In FAST / SPS systems with additional heater (e.g. hybrid sintering device H-HP-D 25), the pyrometer for controlling the additional heating is installed on the side. The measurement is carried out through a sight glass in the furnace door.

ii.) '''Measurement of the temperature with thermocouples:''' Thermocouples are necessarily required for a regulated temperature control of the system at temperatures < 600 °C, since pyrometers do not work reliably in this temperature range. There is also the option of using thermocouples at higher temperatures. Thermocouples of type K (Ni-CrNi) are suitable for the temperature range RT - 1100 ° C and are comparatively inexpensive. Because of the ductility of Ni, type K thermocouples are flexible. For protection, the thermocouples are enclosed in a steel jacket. Type C thermocouples (W5Re-W26Re) with a molybdenum housing enable temperature measurement in the range of RT - 2,200 ° C. The materials used are brittle and expensive, so that their application requires careful handling. Regardless of whether the housing is made of steel or molybdenum, care must be taken that there is no chemical interaction with the tool material during the sintering cycle. '''Figure 13b''' shows a graphite tool equipped with multiple type K thermocouples. One of the thermocouples is used for controlling the heating cycle by temperature measurement of the die and is flexibly installed. Two further thermocouples are firmly fixed to the upper and lower electrodes of the system and serve to protect the water-cooled CuBe electrodes from overheating.

'''-> Figure 13''' 
'''Figure 13:''' ''Temperature measurement in the laboratory system HP-D 5 '''a.)''' Pyrometer for measuring the temperature of the upper punch, deflection of the measurement signal via a prism inside the device '''b.)''' Flexible thermocouples of type K. When installing the thermocouples, it must made sure that there is no contact between the thermocouple and the container wall in order to avoid short circuiting.''

In general, it should be noted that temperature differences of significantly more than 10 K can occur between the pyrometer and thermocouples when identical operating parameters are used. In order to be able to predict the temperature distribution in the component with good accuracy, it is highly recommended to carry out an accompanying FEM modeling of the temperature distribution. The combination of experiment and modeling is the basis for reliably designing the tools and achieving high reproducibility of the FAST/SPS cycles. Another possibility for estimating the temperature distribution is the use of a "dummy" tool without powder cavity, which is equipped with thermocouples in as many places as possible. It should also be noted that the temperature gradients increase with tool size. In industrial production, temperature gradients of up to 80 K can occur in multi-component tools (up to 500 components per cycle), especially at the beginning of the cycle. When supporting tool design by FEM modeling, temperature deviations can be reduced to below 20 K.

== Applications of FAST/SPS ==

== Alternative operation modes of FAST/SPS devices ==

Field assisted sintering technology/spark plasma sintering

2021-08-05T07:00:43Z

M.bram: /* Tool design and tool materials */

== General principle of FAST/SPS ==
Field Assisted Sintering Technology/Spark Plasma Sintering (FAST/SPS) is a low-voltage, current-activated and pressure-supported sintering process that is based on Joule heating (= resistance heating) of the conductive tools ('''Figure 1''') and is characterized by high heating rates and short cycle times. If electrically conductive powders are applied, the powder itself is also heated directly via the Joule effect. The FAST/SPS process is established in the industry and particularly promising when powders are to be sintered, which have a low sintering activity or an unfavorable particle morphology and particle size distribution for conventional pressing and sintering. Furthermore, the method is well suited for the production of composite materials, especially when phases will be combined, which have very different physical properties. Some typical application examples of FAST/SPS technology are presented in Chapter 7. Due to the great flexibility, the short cycle times and the comparatively simple and cost-effective production of tools, research and development is another important field of application for FAST/SPS technology and is widespread there.

[[File:Wiki Keramik FAST SPS Abb 01.jpg|thumb|center]]
'''Figure 1:''' ''Heated graphite tool in a FAST / SPS device.''

In principle, a FAST/SPS device is a mechanical press, which at the same time also forms a high-energy current circuit. The FAST/SPS process is carried out in a conductive tool consisting of two punches and a die. Two additional cones establish the contact with the device's electrodes. The pressing force is also applied via these electrodes by means of a hydraulic pressure cylinder. '''Figure 2''' shows a schematic sketch of such a device. FAST/SPS processes are usually carried out in a vacuum or protective gas to protect the tool and the powder inside the tool from oxidation. Accordingly, the pressing device is located in a water-cooled chamber, in which a moderate vacuum (0.5 - 20 mbar) or a defined protective gas atmosphere (e.g. Ar or N2) can be set. The heating of the tool via the Joule effect requires the use of conductive materials for the punch and the die. The standard material for punch and die is graphite, alternatives to this are introduced in Chapter 4.

[[File:Wiki Keramik FAST SPS Abb 02 englisch.jpg|thumb|center]]
'''Figure 2:''' ''Schematic sketch of a FAST/SPS device.''

The tool is heated by a continuous or pulsed direct current with moderate voltages <10 V and high currents in the range from 1 to several 10 kA (depending on the size of the device). Non-conductive powders can also be sintered in good quality via FAST/SPS. Here, the direct contact between the tool and the powder leads to rapid heat transfer and relatively even heating over the entire cross-section of the sample. The heating takes place primarily via thermal conduction. In order to reduce the heat loss through thermal radiation, the die can optionally be thermally insulated, e.g. with a graphite felt. In the standard configuration, heating rates of up to approx. 300 K/min can be achieved in a FAST/SPS device. The high heating rates are one of the main reasons for the fast cycle times, as grain boundary and volume diffusion necessary for mass transport during sintering are activated directly. Due to the thermal mass of the tools, extremely high cooling rates cannot be achieved. Typical cooling rates are around 100 - 150 K/min. It should be noted here that the use of thermal insulation materials further reduces the cooling rates. In addition to the rapid heating, the sintering kinetics are also supported by the applied load. Depending on the type of system and sample size, compaction pressure in the range of 50 - 100 MPa can be achieved with the standard material graphite. Special grades of graphite allow maximum pressures of up to 200 MPa. When using graphite tools, temperatures of up to approx. 2,200 °C can be achieved in FAST/SPS devices. Alternative tools made of highly heat-resistant metals or electrically conductive ceramics enable pressures of up to 400 MPa, but the maximum permissible sintering temperatures are usually significantly lower in these cases. In order to improve the electrical contact between the punches, the die and the sample, a flexible, ideally electrically conductive foil is usually positioned between the punches and the sample. Graphite has also proven to be the standard material for this foil. FAST/SPS systems are usually controlled by programming the temperature-time curve. The measurement of the temperature as a major process parameter is carried out by axially or radially arranged pyrometers or by thermocouples. A direct measurement of the sample temperature is usually not possible. In order to measure the temperature as close as possible to the sample, holes are often drilled in the tools, at the bottom of which the temperature is measured. Furthermore, especially with increasing size of sintered parts and complexity of shape, it is recommended to predict the temperature distribution in the parts using suitable FEM modeling.

== Advantages and limitations of FAST/SPS ==
i.) '''Advantages:''' An essential feature of the FAST/SPS process is the rapid heating of the sample, which is based on the direct heating of the tool and the good heat transfer between the die and the powder. The superimposition of an uniaxial pressure during sintering further accelerates the sintering kinetics, so that the sintering temperature can often be significantly reduced compared to conventional sintering processes. Accordingly, the FAST/SPS process is a promising technology for

* '''Powder with low sintering activity:''' FAST/SPS enables the compaction of powders that have a low sintering activity (e.g. borides, carbides, nitrides and their mixtures).
* '''Powders with unfavorable powder properties:''' Powders can be sintered whose particle size distribution and morphology are unsuitable for conventional pressing and sintering.
* '''Nanoscale powders:''' The rapid processing in the case of FAST/SPS makes it possible to preserve the structure of nanoscale powders in the component.
* '''Materials with limited stability:''' FAST/SPS enables the sintering of materials that tend to decompose at high temperatures and long dwell times and to form undesirable secondary phases.
* '''Materials containing phases out of thermodynamic equilibrium:''' Phases out of thermodynamic equilibrium can be maintained in the sintered part (e.g. amorphous phases). Based on this, properties can be achieved that are not feasible with other sintering methods.
* '''Composite materials:''' FAST/SPS has great potential for sintering of composite materials that combine phases, which have large differences in their physical properties (e.g. very different melting points).
* '''Energy-efficient processing:''' In general, the FAST/SPS process is classified as an energy-efficient process due to the reduced sintering temperature and the short cycle times, but the degree of automation and the number of components per sintering cycle must also be taken carefully into account for an objective comparison with other sintering technologies.

ii.) '''Limitations:''' Despite the obvious advantages of FAST/SPS technology, there are also a number of process-related limitations.
* '''Risk of density and stress gradients in the component:''' If powders with a low thermal conductivity and high electrical resistance are sintered by FAST/SPS, there might arise an inhomogeneous temperature distribution in the component, which becomes more pronounced with increasing sample size. If exceeding a critical value, density and/or stress gradients in the sintered part result. There are also limitations with respect to the maximum height/diameter ratio. Similar to conventional pressing, wall friction can cause density gradients in the sintered part.
* '''Chemical and electrochemical interaction with the tool materials:''' The direct contact of the powder with the tools is advantageous with respect to heat transfer, but in the worst case it also leads to a chemical interaction with the tools or the inserted foils. When using graphite tools or foils, possible contamination of the component with carbon must be taken carefully into account. Therefore, adhering residues of the graphite foil and the reaction zone on the component surface must be removed mechanically, e.g. by grinding. In addition, it must be noted that the electrical field applied to the powder can trigger electrochemical reactions at the interfaces. A well-known effect is electrochemical blackening of oxide ceramics caused by the release of oxygen at low oxygen partial pressures. Furthermore, oxide ceramics that contain transition metals at the A or B position are sensitive to chemical expansion, which in the worst case leads to severe cracking in the component.
* '''Change of conductivity of semi-conductive and mixed-conductive materials:''' When sintering semi-conductive and mixed-conductive materials via FAST/SPS, it should be noted that the conductivity of the powder changes with increasing temperature and density during the FAST/SPS cycle. If the heating at the beginning of the sintering cycle is primarily based on heat conduction, this state might change suddenly if a current flow through the sample becomes possible when the temperature exceeds a specific value. The result is a complex sintering process that becomes difficult to control and which can impair reproducibility. This effect is used for specific kinds of field-assisted sintering, e.g. for flash sintering. For more details, see Chapter 8.
* '''Net-shaping:''' The FAST/SPS process reaches its limits when complex shapes are to be realized. In addition to the challenges of suitable tool design, increasing geometrical complexity might cause inhomogeneous temperature distribution and, in the case of conductive powders, inhomogeneous current flow over the entire sample cross-section. There are a number of approaches to manufacture complex shapes e.g. by using split tools or by sintering near net-shaped green parts in a powder bed directly via FAST/SPS. However, the possibilities for automating these technologies must be evaluated critical.
* '''Automation of the FAST/SPS process:''' At current state of development, cycle times in FAST/SPS systems cannot compete with conventional pressing and sintering, since a complete FAST/SPS cycle takes several minutes despite high heating rates and short dwell times. If insert foils are used to improve the electrical and thermal contact during tool assembly, this slows down the cycle time further. In order to operate FAST/SPS devices with higher productivity, partially automated, multiple tools (capacity up to several hundred components) are in use, which can optionally be filled with a robot system outside the device and then installed in the device via a manipulator. Another concept are FAST/SPS devices with a system of separate chambers in which the individual processing steps of tool assembly, powder filling, compression and cooling are carried out in a separate and sequential manner.

== How to conduct a standard FAST/SPS cycle ==
In this section, the processing steps for sintering a ceramic powder via FAST/SPS are explained in detail. For conducting FAST/SPS cycles, the following three devices are available at the institute IEK-1 ('''Figure 3''').

'''-> Figure 3''' 
'''Figure 3:''' ''FAST/SPS devices at the institute IEK-1 '''a.)''' Laboratory device HP-D 5 '''b.)''' Hybrid sintering system H-HP-D25 SD/FL/MoSi '''c.)''' Sintering press DSP515 on industrial scale.''

The '''HP-D 5 laboratory device''' is characterized by the following operating parameters:
* Type: HP-D 5
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 50 kN
* Maximum heating power: 37 kW
* Maximum sample diameter: 30 mm
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operating mode: FAST / SPS with pulsed direct current

The '''hybrid sintering device H-HP-D25 SD/FL/MoSi''' enables a number of different operating modes in addition to the conventional FAST/SPS mode through the optional application of additional heaters or operation with an external voltage source.
* Type: H-HP-D25 SD/FL/MoSi
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 250 kN
* Maximum sample diameter: 100 mm (FAST/SPS mode), 20 mm (Flash sintering mode)
* Maximum heating power (FAST / SPS): 60 kW
* Maximum heating power (Induction): 80 kW
* Maximum heating power (MoSi2): 10 kW
* Maximum heating power (Hybrid heating): 100 kW
* External voltage source: AC/DC, 1000 V, max. 25 A
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operation modes: i.) FAST / SPS with pulsed direct current ii.) Hybrid FAST/SPS with induction coil or MoSi2 furnace as additional heater iii.) Hot press with MoSi2 heater iv.) Flash SPS with defined heating power v.) Flash sintering with an external voltage source and MoSi2 heater.

The '''DSP515 sintering press''' is a device, which can be used for industrial production and enables the scaling up of promising results from experiments on lab-scale.
* Type: DSP515
* Manufacturer: Dr. Fritsch Sondermaschinen GmbH, Fellbach, Germany
* Maxiumum pressing force: 555 kN
* Electrode size: 180 x 180 mm2
* Maximum sample size: approx. 160 x 160 mm2
* Maximum heating power: 170 kW
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2
* Operating modes: i.) FAST/SPS with constant direct current ii.) Flash SPS with defined heating power.
* Debinding unit: The system is also equipped with a cooling trap for debinding of tape-cast parts.

Below, the steps of a standard FAST/SPS cycle using a graphite tool with a sample diameter of 20 mm are described. An additional graphite foil (thickness approx. 0.35 mm) is inserted into the graphite tool. The thickness of the foil must be taken into account when designing the tool. The inserted foil has two main functions. On the one hand, it improves the electrical and thermal contact between the punch and the die as well as between the powder, the face of the punch and the die. On the other hand, it avoids chemical interactions between powder and tool, so that the tool life is increased. The FAST/SPS cycle shown here was carried out in the HP-D 5 laboratory device.

i.) '''Sample preparation:''' '''Figure 4''' shows the parts of a lab-scale graphite tool (inner diameter 20 mm) as well as the graphite insert foils (thickness 0.35 mm), which are sized with respect to the tool dimensions. In a first step, the graphite foils are positioned on the inner wall of the die and on the faces of the punches. It is important that the foils has a tight contact to the tool components and that there are no kinks or gaps after positioning. For health protection, the graphite tool should be filled in a laboratory hood. Filling can be carried out on a balance. This increases the accuracy of the powder quantity weighed in.

'''-> Figure 4''' 
'''Figure 4:''' ''Preparation of the graphite tool and the insert foil for the FAST/SPS cycle. For accurate sample preparation, the powder should be directly balanced in the tool. Furthermore, it is recommended to handle the powder in a hood.''

After filling in the tool, the powder is covered with an additional graphite foil and pre-pressed in a manual laboratory press with 50 MPa (16 KN for diameter 20 mm tool) ('''Figure 5'''). In order to avoid sticking of powder particles on the face the upper punch, the upper punch is removed again and powder residues are manually removed. Afterwards, the upper punch is placed again in the tool.

'''-> Figure 5''' 
'''Figure 5:''' '''''a.)''' Filling the mold and positioning the graphite foil '''b.)''' Pre-pressing of the FAST/SPS sample in a manual hand press '''c.)''' Removal of the upper punch after the pressing process and removal of adhering powder particles.''

ii.) '''Mounting of the tool and programming the FAST/SPS device:''' At the laboratory system HP-D 5, the programming of the FAST/SPS parameters can be done via a process controller type Stange SE607 ('''Figure 6'''). The main operating parameters temperature, pressing force, pulse length of the current and moving speed of the lower electrode is programmed in individual program segments. During the FAST/SPS cycle, all process data are shown on the controller display as a numerical values and as a time-resolved graph. In parallel, all data are saved via a data logger integrated in the system. By default, the data are transferred to an external PC for data management and further evaluation. Individual parameter sets of the users are also stored on the PC and can be easily transferred to the controller if required.

'''-> Figure 6''' 
'''Figure 6:''' ''Display of the controller of the HP-D 5 device giving a compact overview of all process-relevant data.''

'''Figure 7''' shows the graphite tool mounted into the HP-D 5 devices as well as the CuBe electrodes. Optionally, the graphite tool can be thermally isolated with a jacket made of a graphite felt (not shown here). A graphite cord can be used to fix the graphite felt on the tool.

'''-> Figure 7''' 
'''Figure 7:''' ''View on the processing chamber of the HP-D 5 device with mounted graphite tool. When installing the tool and the two cones, it should be noted that graphite is a brittle and shock-sensitive material and therefore breaks very easily. For this reason, sudden contact of all graphite parts with the other system components (stamp, chamber walls) must be avoided.''

After the graphite tool has been inserted and fixed by lifting the lower punch, the container door is closed and the FAST/SPS cycle can be started.

iii.) '''Choice and regulation of the sintering atmosphere:''' A FAST/SPS cycle is usually carried out in vacuum or under protective gas atmosphere. Accordingly, the process chamber is evacuated by a vacuum pump at the beginning of the cycle. In the laboratory device HP-D 5, a vacuum of approx. 0.5 mbar is achieved; in larger systems, this value can also be higher (e.g. 20 mbar for the DSP515). The quality of the vacuum depends on the sealing of the process chamber and the power of the vacuum pump. If aiming on a high vacuum, cost of the FAST/SPS device significantly increases. After evacuation, the chamber can optionally be flooded with gases such as N2, Ar or Ar/H2 (static atmosphere control) or a continuous gas flow (dynamic atmosphere control). Figure 8 shows the valves for feeding the individual gases from the institute's gas store into the system. The evacuation of the process chamber and the optional supply of protective gases to the process chamber is regulated by the system control and takes place automated. The pressure in the process chamber is continuously recorded in the HP-D 5 device by two sensors with different measuring ranges (coarse sensor 1.0 - 1300 mbar, fine sensor 0.01 - 13 mbar), which are positioned at the gas outlet. For operation of the system under relative pressure (reduced pressure in relation to the ambient pressure), the system is also equipped with a relative pressure sensor, which enables to regulate the relative pressure in the range of 5 - 50 mbar. Static or dynamic operation is also possible in the relative pressure mode. A safety valve is used to protect the processing chamber against overpressure. The valve opens at an overpressure of 100 mbar above the ambient pressure. The pressure curve during the FAST/SPS cycle is recorded continuously. An analysis of the pressure curve can be helpful if components outgas from the sample or if the sample decomposes under the FAST/SPS conditions.

'''-> Figure 8''' 
'''Figure 8:''' ''Valves for flooding the processing chamber with the protective gases Ar, N2, Ar/H2.''

When sintering oxide ceramics via FAST/SPS, it should be noted that the sintering conditions have a reducing effect, i.e. there is a release oxygen atoms from the lattice, which increases with decreasing oxygen partial pressure. The effect is aggravated in the case of direct contact with the graphite tools or the graphite foils. The release of oxygen is visually noticeable in the darkening of the ceramic. This effect is superimposed by the uptake of carbon. If the release of oxygen exceeds a critical value, the sample can undergo chemical expansion, which can be up to several percent (as e.g. the case for gadolinium-doped cerium oxide or barium-strontium-cobalt oxides). Usually, this effect leads to severe cracking of the sample. Furthermore, the crystal lattice can become unstable if the oxygen release progresses further. In worst case, reduction of components down to the metallic phase might appear.

In principle, it is possible to operate a FAST/SPS device with technical air. Such operation must be done with special care, since most materials used for the tools are unstable in air and start to strongly oxidize if the temperature exceeds a critical value (usually around 400°C). It should also be noted that the powder in the tool is encapsulated in such a way that the access of oxygen to the powder is prevented to a large extent.

iv.) '''Performing of the FAST/SPS cycle:''' After the device has been prepared, the selected program is started and runs automatically. '''Figure 9''' shows the graphite die during the heating process. As already mentioned, the operation of FAST/SPS devices is usually temperature-controlled. This means that the controller defines the temperature and the system regulates the current and voltage in such a way that the temperature profile is adhered to the specification as precisely as possible. In order to keep the deviations from the programmed temperature curve as low as possible, the system is equipped with a PID control (PID = Proportional-Integral-Derivative). This control unit iteratively adapt the optimal current and voltage curves for heating the tool to the respective electrical resistance of the tool.

'''-> Figure 9''' 
'''Figure 9:''' ''View on the heated graphite tool (punch diameter 20 mm) in the laboratory device HP-D 5. When operating a FAST/SPS system, it should be noted that the high currents in the system cause strong electromagnetic fields, which can damage pacemakers and others sensitive electronic devices.''

v.) Demoulding of the samples
At the end of the cycle, the sample can be pressed out of the graphite tool using a hand press, as shown in '''Figure 10'''.

'''-> Figure 10''' 
'''Figure 10:''' ''Demoulding the sample from the FAST/SPS tool using a hand press. When removing the tool from the FAST/SPS device, please take care since the tool can still be hot.''

== Tool design and tool materials ==
In most cases, graphite tools are used in FAST/SPS systems. '''Figure 11''' shows a selection of graphite tools for the laboratory system HP-D 5 with punch diameters of 12, 20 and 30 mm and for the hybrid sintering device H-HP-D25 with a punch diameter of 100 mm.

'''-> Figure 11''' 
'''Figure 11:''' ''Graphite tools for performing FAST/SPS cycles '''a.)''' Overview: die, punch with hole for pyrometer, cone for adaptation to the geometry of the electrodes of the FAST/SPS device '''b.)''' Tools for the laboratory device HP-D 5 with a diameter of 12, 20 and 30 mm and '''c.)''' Tools for the hybrid sintering device H-HP-D25 with a diameter of 100 mm.''

The use of graphite has the advantage that it is easy to machine the tools. Furthermore, it has an electrical resistance that is favorable for Joule heating. Temperatures of up to around 2,200 °C can be achieved in graphite tools. The compressive strength of standard grades is approx. 50 - 100 MPa (e.g. Sigrafine R7710, SGL Carbon GmbH), special grades achieve compressive strengths of up to 230 MPa (e.g. Grade 2334, Mersen). It should be noted that the geometry of the tool also has an influence on the maximum permissible pressure, e.g. the notch effect of a hole drilled for temperature measurement can lead to failure of the tool even at low pressures. Above 450 °C, graphite tools can only be used in a vacuum or under protective gas (e.g. Ar). If a tool is used frequently, attention must also be paid to possible wear, which can reduce the dimensional accuracy of the sintered parts.

If pressures well above 100 MPa or long tool life are desired, the following materials can used as alternative to graphite. At temperatures up to 600 °C, the use of a high-speed steel (e.g. W360, Böhler) is recommended, which can resist pressures of up to 400 MPa. If higher temperatures are desired, Mo alloys (e.g. Ti-Zr-Mo TZM, Plansee) can be used, which enable maximum temperature of approx. 1100 ° C and maximum pressure of 350 MPa. The maximum operating temperature of metal tools is limited by the onset of creep processes and severe grain coarsening. Both effects can cause a macroscopic deformation of the tools, so that in the worst case the punch can become jammed in the die. '''Figure 12''' shows as an example tools made of W360 steel and TZM.

'''-> Figure 12''' 
'''Figure 12:''' ''Metallic tools '''a.)''' Overview: Die, punch, and cone of a tool made of W360 steel '''b.)''' Same tool in the assembled state '''c.)''' Similar tool made of TZM.''

If even higher temperatures or pressures are desired, the literature reports on tools made of conductive ceramics. Suitable materials are tungsten carbide or silicon carbide, which are already used in the laboratory up to pressures of 1000 MPa. When using ceramic tools, the high effort in production and the inherent brittleness must be taken into account. Careful handling is strictly required in order to avoid breakage.

When using metallic and ceramic tools, it should be noted that these materials usually have a different electrical resistance than graphite. This has an influence on the system control and may require an adjustment of the PID parameters for precise temperature control (see Chapter 4).

== Measurement of temperature ==
The temperature is the main parameter for controlling the FAST/SPS system. The exact measurement and control of temperature is one of the great challenges when applying of FAST/SPS technology. The high heating rates require a temperature measurement with short response time, short delay time and high reproducibility. A direct measurement of the sample temperature is not possible with reasonable effort. Therefore, the measurement should be conducted as close to the sample as possible. For this purpose, vertical or horizontal holes are usually drilled in the FAST/SPS tool. By adjusting the pyrometer or thermocouple at the bottom of these holes, the temperature can be measured in direct vicinity of the sample.

i.) '''Measurement of the temperature with the pyrometer:''' Pyrometers are preferably used for temperature measurement at high temperatures. The usual measuring range of pyrometers is 600 - 3000 °C. '''Figure 12a''' shows the pyrometer installed in the HP-D 5 laboratory device. In this case, the measurement signal is deflected via a prism so that the measurement can be carried out vertically in a hole drilled in the upper punch.

In FAST / SPS systems with additional heater (e.g. hybrid sintering device H-HP-D 25), the pyrometer for controlling the additional heating is installed on the side. The measurement is carried out through a sight glass in the furnace door.

ii.) '''Measurement of the temperature with thermocouples:''' Thermocouples are necessarily required for a regulated temperature control of the system at temperatures < 600 °C, since pyrometers do not work reliably in this temperature range. There is also the option of using thermocouples at higher temperatures. Thermocouples of type K (Ni-CrNi) are suitable for the temperature range RT - 1100 ° C and are comparatively inexpensive. Because of the ductility of Ni, type K thermocouples are flexible. For protection, the thermocouples are enclosed in a steel jacket. Type C thermocouples (W5Re-W26Re) with a molybdenum housing enable temperature measurement in the range of RT - 2,200 ° C. The materials used are brittle and expensive, so that their application requires careful handling. Regardless of whether the housing is made of steel or molybdenum, care must be taken that there is no chemical interaction with the tool material during the sintering cycle. '''Figure 12b''' shows a graphite tool equipped with multiple type K thermocouples. One of the thermocouples is used for controlling the heating cycle by temperature measurement of the die and is flexibly installed. Two further thermocouples are firmly fixed to the upper and lower electrodes of the system and serve to protect the water-cooled CuBe electrodes from overheating.

'''-> Figure 12'''
'''Figure 12:''' ''Temperature measurement in the laboratory system HP-D 5 '''a.)''' Pyrometer for measuring the temperature of the upper punch, deflection of the measurement signal via a prism inside the device '''b.)''' Flexible thermocouples of type K. When installing the thermocouples, it must made sure that there is no contact between the thermocouple and the container wall in order to avoid short circuiting.''

In general, it should be noted that temperature differences of significantly more than 10 K can occur between the pyrometer and thermocouples when identical operating parameters are used. In order to be able to predict the temperature distribution in the component with good accuracy, it is highly recommended to carry out an accompanying FEM modeling of the temperature distribution. The combination of experiment and modeling is the basis for reliably designing the tools and achieving high reproducibility of the FAST/SPS cycles. Another possibility for estimating the temperature distribution is the use of a "dummy" tool without powder cavity, which is equipped with thermocouples in as many places as possible. It should also be noted that the temperature gradients increase with tool size. In industrial production, temperature gradients of up to 80 K can occur in multi-component tools (up to 500 components per cycle), especially at the beginning of the cycle. When supporting tool design by FEM modeling, temperature deviations can be reduced to below 20 K.

== Applications of FAST/SPS ==

== Alternative operation modes of FAST/SPS devices ==

Field assisted sintering technology/spark plasma sintering

2021-08-05T07:00:10Z

M.bram: /* Tool design and tool materials */

== General principle of FAST/SPS ==
Field Assisted Sintering Technology/Spark Plasma Sintering (FAST/SPS) is a low-voltage, current-activated and pressure-supported sintering process that is based on Joule heating (= resistance heating) of the conductive tools ('''Figure 1''') and is characterized by high heating rates and short cycle times. If electrically conductive powders are applied, the powder itself is also heated directly via the Joule effect. The FAST/SPS process is established in the industry and particularly promising when powders are to be sintered, which have a low sintering activity or an unfavorable particle morphology and particle size distribution for conventional pressing and sintering. Furthermore, the method is well suited for the production of composite materials, especially when phases will be combined, which have very different physical properties. Some typical application examples of FAST/SPS technology are presented in Chapter 7. Due to the great flexibility, the short cycle times and the comparatively simple and cost-effective production of tools, research and development is another important field of application for FAST/SPS technology and is widespread there.

[[File:Wiki Keramik FAST SPS Abb 01.jpg|thumb|center]]
'''Figure 1:''' ''Heated graphite tool in a FAST / SPS device.''

In principle, a FAST/SPS device is a mechanical press, which at the same time also forms a high-energy current circuit. The FAST/SPS process is carried out in a conductive tool consisting of two punches and a die. Two additional cones establish the contact with the device's electrodes. The pressing force is also applied via these electrodes by means of a hydraulic pressure cylinder. '''Figure 2''' shows a schematic sketch of such a device. FAST/SPS processes are usually carried out in a vacuum or protective gas to protect the tool and the powder inside the tool from oxidation. Accordingly, the pressing device is located in a water-cooled chamber, in which a moderate vacuum (0.5 - 20 mbar) or a defined protective gas atmosphere (e.g. Ar or N2) can be set. The heating of the tool via the Joule effect requires the use of conductive materials for the punch and the die. The standard material for punch and die is graphite, alternatives to this are introduced in Chapter 4.

[[File:Wiki Keramik FAST SPS Abb 02 englisch.jpg|thumb|center]]
'''Figure 2:''' ''Schematic sketch of a FAST/SPS device.''

The tool is heated by a continuous or pulsed direct current with moderate voltages <10 V and high currents in the range from 1 to several 10 kA (depending on the size of the device). Non-conductive powders can also be sintered in good quality via FAST/SPS. Here, the direct contact between the tool and the powder leads to rapid heat transfer and relatively even heating over the entire cross-section of the sample. The heating takes place primarily via thermal conduction. In order to reduce the heat loss through thermal radiation, the die can optionally be thermally insulated, e.g. with a graphite felt. In the standard configuration, heating rates of up to approx. 300 K/min can be achieved in a FAST/SPS device. The high heating rates are one of the main reasons for the fast cycle times, as grain boundary and volume diffusion necessary for mass transport during sintering are activated directly. Due to the thermal mass of the tools, extremely high cooling rates cannot be achieved. Typical cooling rates are around 100 - 150 K/min. It should be noted here that the use of thermal insulation materials further reduces the cooling rates. In addition to the rapid heating, the sintering kinetics are also supported by the applied load. Depending on the type of system and sample size, compaction pressure in the range of 50 - 100 MPa can be achieved with the standard material graphite. Special grades of graphite allow maximum pressures of up to 200 MPa. When using graphite tools, temperatures of up to approx. 2,200 °C can be achieved in FAST/SPS devices. Alternative tools made of highly heat-resistant metals or electrically conductive ceramics enable pressures of up to 400 MPa, but the maximum permissible sintering temperatures are usually significantly lower in these cases. In order to improve the electrical contact between the punches, the die and the sample, a flexible, ideally electrically conductive foil is usually positioned between the punches and the sample. Graphite has also proven to be the standard material for this foil. FAST/SPS systems are usually controlled by programming the temperature-time curve. The measurement of the temperature as a major process parameter is carried out by axially or radially arranged pyrometers or by thermocouples. A direct measurement of the sample temperature is usually not possible. In order to measure the temperature as close as possible to the sample, holes are often drilled in the tools, at the bottom of which the temperature is measured. Furthermore, especially with increasing size of sintered parts and complexity of shape, it is recommended to predict the temperature distribution in the parts using suitable FEM modeling.

== Advantages and limitations of FAST/SPS ==
i.) '''Advantages:''' An essential feature of the FAST/SPS process is the rapid heating of the sample, which is based on the direct heating of the tool and the good heat transfer between the die and the powder. The superimposition of an uniaxial pressure during sintering further accelerates the sintering kinetics, so that the sintering temperature can often be significantly reduced compared to conventional sintering processes. Accordingly, the FAST/SPS process is a promising technology for

* '''Powder with low sintering activity:''' FAST/SPS enables the compaction of powders that have a low sintering activity (e.g. borides, carbides, nitrides and their mixtures).
* '''Powders with unfavorable powder properties:''' Powders can be sintered whose particle size distribution and morphology are unsuitable for conventional pressing and sintering.
* '''Nanoscale powders:''' The rapid processing in the case of FAST/SPS makes it possible to preserve the structure of nanoscale powders in the component.
* '''Materials with limited stability:''' FAST/SPS enables the sintering of materials that tend to decompose at high temperatures and long dwell times and to form undesirable secondary phases.
* '''Materials containing phases out of thermodynamic equilibrium:''' Phases out of thermodynamic equilibrium can be maintained in the sintered part (e.g. amorphous phases). Based on this, properties can be achieved that are not feasible with other sintering methods.
* '''Composite materials:''' FAST/SPS has great potential for sintering of composite materials that combine phases, which have large differences in their physical properties (e.g. very different melting points).
* '''Energy-efficient processing:''' In general, the FAST/SPS process is classified as an energy-efficient process due to the reduced sintering temperature and the short cycle times, but the degree of automation and the number of components per sintering cycle must also be taken carefully into account for an objective comparison with other sintering technologies.

ii.) '''Limitations:''' Despite the obvious advantages of FAST/SPS technology, there are also a number of process-related limitations.
* '''Risk of density and stress gradients in the component:''' If powders with a low thermal conductivity and high electrical resistance are sintered by FAST/SPS, there might arise an inhomogeneous temperature distribution in the component, which becomes more pronounced with increasing sample size. If exceeding a critical value, density and/or stress gradients in the sintered part result. There are also limitations with respect to the maximum height/diameter ratio. Similar to conventional pressing, wall friction can cause density gradients in the sintered part.
* '''Chemical and electrochemical interaction with the tool materials:''' The direct contact of the powder with the tools is advantageous with respect to heat transfer, but in the worst case it also leads to a chemical interaction with the tools or the inserted foils. When using graphite tools or foils, possible contamination of the component with carbon must be taken carefully into account. Therefore, adhering residues of the graphite foil and the reaction zone on the component surface must be removed mechanically, e.g. by grinding. In addition, it must be noted that the electrical field applied to the powder can trigger electrochemical reactions at the interfaces. A well-known effect is electrochemical blackening of oxide ceramics caused by the release of oxygen at low oxygen partial pressures. Furthermore, oxide ceramics that contain transition metals at the A or B position are sensitive to chemical expansion, which in the worst case leads to severe cracking in the component.
* '''Change of conductivity of semi-conductive and mixed-conductive materials:''' When sintering semi-conductive and mixed-conductive materials via FAST/SPS, it should be noted that the conductivity of the powder changes with increasing temperature and density during the FAST/SPS cycle. If the heating at the beginning of the sintering cycle is primarily based on heat conduction, this state might change suddenly if a current flow through the sample becomes possible when the temperature exceeds a specific value. The result is a complex sintering process that becomes difficult to control and which can impair reproducibility. This effect is used for specific kinds of field-assisted sintering, e.g. for flash sintering. For more details, see Chapter 8.
* '''Net-shaping:''' The FAST/SPS process reaches its limits when complex shapes are to be realized. In addition to the challenges of suitable tool design, increasing geometrical complexity might cause inhomogeneous temperature distribution and, in the case of conductive powders, inhomogeneous current flow over the entire sample cross-section. There are a number of approaches to manufacture complex shapes e.g. by using split tools or by sintering near net-shaped green parts in a powder bed directly via FAST/SPS. However, the possibilities for automating these technologies must be evaluated critical.
* '''Automation of the FAST/SPS process:''' At current state of development, cycle times in FAST/SPS systems cannot compete with conventional pressing and sintering, since a complete FAST/SPS cycle takes several minutes despite high heating rates and short dwell times. If insert foils are used to improve the electrical and thermal contact during tool assembly, this slows down the cycle time further. In order to operate FAST/SPS devices with higher productivity, partially automated, multiple tools (capacity up to several hundred components) are in use, which can optionally be filled with a robot system outside the device and then installed in the device via a manipulator. Another concept are FAST/SPS devices with a system of separate chambers in which the individual processing steps of tool assembly, powder filling, compression and cooling are carried out in a separate and sequential manner.

== How to conduct a standard FAST/SPS cycle ==
In this section, the processing steps for sintering a ceramic powder via FAST/SPS are explained in detail. For conducting FAST/SPS cycles, the following three devices are available at the institute IEK-1 ('''Figure 3''').

'''-> Figure 3''' 
'''Figure 3:''' ''FAST/SPS devices at the institute IEK-1 '''a.)''' Laboratory device HP-D 5 '''b.)''' Hybrid sintering system H-HP-D25 SD/FL/MoSi '''c.)''' Sintering press DSP515 on industrial scale.''

The '''HP-D 5 laboratory device''' is characterized by the following operating parameters:
* Type: HP-D 5
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 50 kN
* Maximum heating power: 37 kW
* Maximum sample diameter: 30 mm
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operating mode: FAST / SPS with pulsed direct current

The '''hybrid sintering device H-HP-D25 SD/FL/MoSi''' enables a number of different operating modes in addition to the conventional FAST/SPS mode through the optional application of additional heaters or operation with an external voltage source.
* Type: H-HP-D25 SD/FL/MoSi
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 250 kN
* Maximum sample diameter: 100 mm (FAST/SPS mode), 20 mm (Flash sintering mode)
* Maximum heating power (FAST / SPS): 60 kW
* Maximum heating power (Induction): 80 kW
* Maximum heating power (MoSi2): 10 kW
* Maximum heating power (Hybrid heating): 100 kW
* External voltage source: AC/DC, 1000 V, max. 25 A
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operation modes: i.) FAST / SPS with pulsed direct current ii.) Hybrid FAST/SPS with induction coil or MoSi2 furnace as additional heater iii.) Hot press with MoSi2 heater iv.) Flash SPS with defined heating power v.) Flash sintering with an external voltage source and MoSi2 heater.

The '''DSP515 sintering press''' is a device, which can be used for industrial production and enables the scaling up of promising results from experiments on lab-scale.
* Type: DSP515
* Manufacturer: Dr. Fritsch Sondermaschinen GmbH, Fellbach, Germany
* Maxiumum pressing force: 555 kN
* Electrode size: 180 x 180 mm2
* Maximum sample size: approx. 160 x 160 mm2
* Maximum heating power: 170 kW
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2
* Operating modes: i.) FAST/SPS with constant direct current ii.) Flash SPS with defined heating power.
* Debinding unit: The system is also equipped with a cooling trap for debinding of tape-cast parts.

Below, the steps of a standard FAST/SPS cycle using a graphite tool with a sample diameter of 20 mm are described. An additional graphite foil (thickness approx. 0.35 mm) is inserted into the graphite tool. The thickness of the foil must be taken into account when designing the tool. The inserted foil has two main functions. On the one hand, it improves the electrical and thermal contact between the punch and the die as well as between the powder, the face of the punch and the die. On the other hand, it avoids chemical interactions between powder and tool, so that the tool life is increased. The FAST/SPS cycle shown here was carried out in the HP-D 5 laboratory device.

i.) '''Sample preparation:''' '''Figure 4''' shows the parts of a lab-scale graphite tool (inner diameter 20 mm) as well as the graphite insert foils (thickness 0.35 mm), which are sized with respect to the tool dimensions. In a first step, the graphite foils are positioned on the inner wall of the die and on the faces of the punches. It is important that the foils has a tight contact to the tool components and that there are no kinks or gaps after positioning. For health protection, the graphite tool should be filled in a laboratory hood. Filling can be carried out on a balance. This increases the accuracy of the powder quantity weighed in.

'''-> Figure 4''' 
'''Figure 4:''' ''Preparation of the graphite tool and the insert foil for the FAST/SPS cycle. For accurate sample preparation, the powder should be directly balanced in the tool. Furthermore, it is recommended to handle the powder in a hood.''

After filling in the tool, the powder is covered with an additional graphite foil and pre-pressed in a manual laboratory press with 50 MPa (16 KN for diameter 20 mm tool) ('''Figure 5'''). In order to avoid sticking of powder particles on the face the upper punch, the upper punch is removed again and powder residues are manually removed. Afterwards, the upper punch is placed again in the tool.

'''-> Figure 5''' 
'''Figure 5:''' '''''a.)''' Filling the mold and positioning the graphite foil '''b.)''' Pre-pressing of the FAST/SPS sample in a manual hand press '''c.)''' Removal of the upper punch after the pressing process and removal of adhering powder particles.''

ii.) '''Mounting of the tool and programming the FAST/SPS device:''' At the laboratory system HP-D 5, the programming of the FAST/SPS parameters can be done via a process controller type Stange SE607 ('''Figure 6'''). The main operating parameters temperature, pressing force, pulse length of the current and moving speed of the lower electrode is programmed in individual program segments. During the FAST/SPS cycle, all process data are shown on the controller display as a numerical values and as a time-resolved graph. In parallel, all data are saved via a data logger integrated in the system. By default, the data are transferred to an external PC for data management and further evaluation. Individual parameter sets of the users are also stored on the PC and can be easily transferred to the controller if required.

'''-> Figure 6''' 
'''Figure 6:''' ''Display of the controller of the HP-D 5 device giving a compact overview of all process-relevant data.''

'''Figure 7''' shows the graphite tool mounted into the HP-D 5 devices as well as the CuBe electrodes. Optionally, the graphite tool can be thermally isolated with a jacket made of a graphite felt (not shown here). A graphite cord can be used to fix the graphite felt on the tool.

'''-> Figure 7''' 
'''Figure 7:''' ''View on the processing chamber of the HP-D 5 device with mounted graphite tool. When installing the tool and the two cones, it should be noted that graphite is a brittle and shock-sensitive material and therefore breaks very easily. For this reason, sudden contact of all graphite parts with the other system components (stamp, chamber walls) must be avoided.''

After the graphite tool has been inserted and fixed by lifting the lower punch, the container door is closed and the FAST/SPS cycle can be started.

iii.) '''Choice and regulation of the sintering atmosphere:''' A FAST/SPS cycle is usually carried out in vacuum or under protective gas atmosphere. Accordingly, the process chamber is evacuated by a vacuum pump at the beginning of the cycle. In the laboratory device HP-D 5, a vacuum of approx. 0.5 mbar is achieved; in larger systems, this value can also be higher (e.g. 20 mbar for the DSP515). The quality of the vacuum depends on the sealing of the process chamber and the power of the vacuum pump. If aiming on a high vacuum, cost of the FAST/SPS device significantly increases. After evacuation, the chamber can optionally be flooded with gases such as N2, Ar or Ar/H2 (static atmosphere control) or a continuous gas flow (dynamic atmosphere control). Figure 8 shows the valves for feeding the individual gases from the institute's gas store into the system. The evacuation of the process chamber and the optional supply of protective gases to the process chamber is regulated by the system control and takes place automated. The pressure in the process chamber is continuously recorded in the HP-D 5 device by two sensors with different measuring ranges (coarse sensor 1.0 - 1300 mbar, fine sensor 0.01 - 13 mbar), which are positioned at the gas outlet. For operation of the system under relative pressure (reduced pressure in relation to the ambient pressure), the system is also equipped with a relative pressure sensor, which enables to regulate the relative pressure in the range of 5 - 50 mbar. Static or dynamic operation is also possible in the relative pressure mode. A safety valve is used to protect the processing chamber against overpressure. The valve opens at an overpressure of 100 mbar above the ambient pressure. The pressure curve during the FAST/SPS cycle is recorded continuously. An analysis of the pressure curve can be helpful if components outgas from the sample or if the sample decomposes under the FAST/SPS conditions.

'''-> Figure 8''' 
'''Figure 8:''' ''Valves for flooding the processing chamber with the protective gases Ar, N2, Ar/H2.''

When sintering oxide ceramics via FAST/SPS, it should be noted that the sintering conditions have a reducing effect, i.e. there is a release oxygen atoms from the lattice, which increases with decreasing oxygen partial pressure. The effect is aggravated in the case of direct contact with the graphite tools or the graphite foils. The release of oxygen is visually noticeable in the darkening of the ceramic. This effect is superimposed by the uptake of carbon. If the release of oxygen exceeds a critical value, the sample can undergo chemical expansion, which can be up to several percent (as e.g. the case for gadolinium-doped cerium oxide or barium-strontium-cobalt oxides). Usually, this effect leads to severe cracking of the sample. Furthermore, the crystal lattice can become unstable if the oxygen release progresses further. In worst case, reduction of components down to the metallic phase might appear.

In principle, it is possible to operate a FAST/SPS device with technical air. Such operation must be done with special care, since most materials used for the tools are unstable in air and start to strongly oxidize if the temperature exceeds a critical value (usually around 400°C). It should also be noted that the powder in the tool is encapsulated in such a way that the access of oxygen to the powder is prevented to a large extent.

iv.) '''Performing of the FAST/SPS cycle:''' After the device has been prepared, the selected program is started and runs automatically. '''Figure 9''' shows the graphite die during the heating process. As already mentioned, the operation of FAST/SPS devices is usually temperature-controlled. This means that the controller defines the temperature and the system regulates the current and voltage in such a way that the temperature profile is adhered to the specification as precisely as possible. In order to keep the deviations from the programmed temperature curve as low as possible, the system is equipped with a PID control (PID = Proportional-Integral-Derivative). This control unit iteratively adapt the optimal current and voltage curves for heating the tool to the respective electrical resistance of the tool.

'''-> Figure 9''' 
'''Figure 9:''' ''View on the heated graphite tool (punch diameter 20 mm) in the laboratory device HP-D 5. When operating a FAST/SPS system, it should be noted that the high currents in the system cause strong electromagnetic fields, which can damage pacemakers and others sensitive electronic devices.''

v.) Demoulding of the samples
At the end of the cycle, the sample can be pressed out of the graphite tool using a hand press, as shown in '''Figure 10'''.

'''-> Figure 10''' 
'''Figure 10:''' ''Demoulding the sample from the FAST/SPS tool using a hand press. When removing the tool from the FAST/SPS device, please take care since the tool can still be hot.''

== Tool design and tool materials ==
In most cases, graphite tools are used in FAST/SPS systems. '''Figure 11''' shows a selection of graphite tools for the laboratory system HP-D 5 with punch diameters of 12, 20 and 30 mm and for the hybrid sintering device H-HP-D25 with a punch diameter of 100 mm.

'''-> Figure 11'''
'''Figure 11:''' ''Graphite tools for performing FAST/SPS cycles '''a.)''' Overview: die, punch with hole for pyrometer, cone for adaptation to the geometry of the electrodes of the FAST/SPS device '''b.)''' Tools for the laboratory device HP-D 5 with a diameter of 12, 20 and 30 mm and '''c.)''' Tools for the hybrid sintering device H-HP-D25 with a diameter of 100 mm.''

The use of graphite has the advantage that it is easy to machine the tools. Furthermore, it has an electrical resistance that is favorable for Joule heating. Temperatures of up to around 2,200 °C can be achieved in graphite tools. The compressive strength of standard grades is approx. 50 - 100 MPa (e.g. Sigrafine R7710, SGL Carbon GmbH), special grades achieve compressive strengths of up to 230 MPa (e.g. Grade 2334, Mersen). It should be noted that the geometry of the tool also has an influence on the maximum permissible pressure, e.g. the notch effect of a hole drilled for temperature measurement can lead to failure of the tool even at low pressures. Above 450 °C, graphite tools can only be used in a vacuum or under protective gas (e.g. Ar). If a tool is used frequently, attention must also be paid to possible wear, which can reduce the dimensional accuracy of the sintered parts.

If pressures well above 100 MPa or long tool life are desired, the following materials can used as alternative to graphite. At temperatures up to 600 °C, the use of a high-speed steel (e.g. W360, Böhler) is recommended, which can resist pressures of up to 400 MPa. If higher temperatures are desired, Mo alloys (e.g. Ti-Zr-Mo TZM, Plansee) can be used, which enable maximum temperature of approx. 1100 ° C and maximum pressure of 350 MPa. The maximum operating temperature of metal tools is limited by the onset of creep processes and severe grain coarsening. Both effects can cause a macroscopic deformation of the tools, so that in the worst case the punch can become jammed in the die. '''Figure 12''' shows as an example tools made of W360 steel and TZM.

'''-> Figure 12'''
'''Figure 12:''' ''Metallic tools '''a.)''' Overview: Die, punch, and cone of a tool made of W360 steel '''b.)''' Same tool in the assembled state '''c.)''' Similar tool made of TZM.''

If even higher temperatures or pressures are desired, the literature reports on tools made of conductive ceramics. Suitable materials are tungsten carbide or silicon carbide, which are already used in the laboratory up to pressures of 1000 MPa. When using ceramic tools, the high effort in production and the inherent brittleness must be taken into account. Careful handling is strictly required in order to avoid breakage.

When using metallic and ceramic tools, it should be noted that these materials usually have a different electrical resistance than graphite. This has an influence on the system control and may require an adjustment of the PID parameters for precise temperature control (see Chapter 4).

== Measurement of temperature ==
The temperature is the main parameter for controlling the FAST/SPS system. The exact measurement and control of temperature is one of the great challenges when applying of FAST/SPS technology. The high heating rates require a temperature measurement with short response time, short delay time and high reproducibility. A direct measurement of the sample temperature is not possible with reasonable effort. Therefore, the measurement should be conducted as close to the sample as possible. For this purpose, vertical or horizontal holes are usually drilled in the FAST/SPS tool. By adjusting the pyrometer or thermocouple at the bottom of these holes, the temperature can be measured in direct vicinity of the sample.

i.) '''Measurement of the temperature with the pyrometer:''' Pyrometers are preferably used for temperature measurement at high temperatures. The usual measuring range of pyrometers is 600 - 3000 °C. '''Figure 12a''' shows the pyrometer installed in the HP-D 5 laboratory device. In this case, the measurement signal is deflected via a prism so that the measurement can be carried out vertically in a hole drilled in the upper punch.

In FAST / SPS systems with additional heater (e.g. hybrid sintering device H-HP-D 25), the pyrometer for controlling the additional heating is installed on the side. The measurement is carried out through a sight glass in the furnace door.

ii.) '''Measurement of the temperature with thermocouples:''' Thermocouples are necessarily required for a regulated temperature control of the system at temperatures < 600 °C, since pyrometers do not work reliably in this temperature range. There is also the option of using thermocouples at higher temperatures. Thermocouples of type K (Ni-CrNi) are suitable for the temperature range RT - 1100 ° C and are comparatively inexpensive. Because of the ductility of Ni, type K thermocouples are flexible. For protection, the thermocouples are enclosed in a steel jacket. Type C thermocouples (W5Re-W26Re) with a molybdenum housing enable temperature measurement in the range of RT - 2,200 ° C. The materials used are brittle and expensive, so that their application requires careful handling. Regardless of whether the housing is made of steel or molybdenum, care must be taken that there is no chemical interaction with the tool material during the sintering cycle. '''Figure 12b''' shows a graphite tool equipped with multiple type K thermocouples. One of the thermocouples is used for controlling the heating cycle by temperature measurement of the die and is flexibly installed. Two further thermocouples are firmly fixed to the upper and lower electrodes of the system and serve to protect the water-cooled CuBe electrodes from overheating.

'''-> Figure 12'''
'''Figure 12:''' ''Temperature measurement in the laboratory system HP-D 5 '''a.)''' Pyrometer for measuring the temperature of the upper punch, deflection of the measurement signal via a prism inside the device '''b.)''' Flexible thermocouples of type K. When installing the thermocouples, it must made sure that there is no contact between the thermocouple and the container wall in order to avoid short circuiting.''

In general, it should be noted that temperature differences of significantly more than 10 K can occur between the pyrometer and thermocouples when identical operating parameters are used. In order to be able to predict the temperature distribution in the component with good accuracy, it is highly recommended to carry out an accompanying FEM modeling of the temperature distribution. The combination of experiment and modeling is the basis for reliably designing the tools and achieving high reproducibility of the FAST/SPS cycles. Another possibility for estimating the temperature distribution is the use of a "dummy" tool without powder cavity, which is equipped with thermocouples in as many places as possible. It should also be noted that the temperature gradients increase with tool size. In industrial production, temperature gradients of up to 80 K can occur in multi-component tools (up to 500 components per cycle), especially at the beginning of the cycle. When supporting tool design by FEM modeling, temperature deviations can be reduced to below 20 K.

== Applications of FAST/SPS ==

== Alternative operation modes of FAST/SPS devices ==

Field assisted sintering technology/spark plasma sintering

2021-08-05T06:59:04Z

M.bram: /* How to conduct a standard FAST/SPS cycle */

== General principle of FAST/SPS ==
Field Assisted Sintering Technology/Spark Plasma Sintering (FAST/SPS) is a low-voltage, current-activated and pressure-supported sintering process that is based on Joule heating (= resistance heating) of the conductive tools ('''Figure 1''') and is characterized by high heating rates and short cycle times. If electrically conductive powders are applied, the powder itself is also heated directly via the Joule effect. The FAST/SPS process is established in the industry and particularly promising when powders are to be sintered, which have a low sintering activity or an unfavorable particle morphology and particle size distribution for conventional pressing and sintering. Furthermore, the method is well suited for the production of composite materials, especially when phases will be combined, which have very different physical properties. Some typical application examples of FAST/SPS technology are presented in Chapter 7. Due to the great flexibility, the short cycle times and the comparatively simple and cost-effective production of tools, research and development is another important field of application for FAST/SPS technology and is widespread there.

[[File:Wiki Keramik FAST SPS Abb 01.jpg|thumb|center]]
'''Figure 1:''' ''Heated graphite tool in a FAST / SPS device.''

In principle, a FAST/SPS device is a mechanical press, which at the same time also forms a high-energy current circuit. The FAST/SPS process is carried out in a conductive tool consisting of two punches and a die. Two additional cones establish the contact with the device's electrodes. The pressing force is also applied via these electrodes by means of a hydraulic pressure cylinder. '''Figure 2''' shows a schematic sketch of such a device. FAST/SPS processes are usually carried out in a vacuum or protective gas to protect the tool and the powder inside the tool from oxidation. Accordingly, the pressing device is located in a water-cooled chamber, in which a moderate vacuum (0.5 - 20 mbar) or a defined protective gas atmosphere (e.g. Ar or N2) can be set. The heating of the tool via the Joule effect requires the use of conductive materials for the punch and the die. The standard material for punch and die is graphite, alternatives to this are introduced in Chapter 4.

[[File:Wiki Keramik FAST SPS Abb 02 englisch.jpg|thumb|center]]
'''Figure 2:''' ''Schematic sketch of a FAST/SPS device.''

The tool is heated by a continuous or pulsed direct current with moderate voltages <10 V and high currents in the range from 1 to several 10 kA (depending on the size of the device). Non-conductive powders can also be sintered in good quality via FAST/SPS. Here, the direct contact between the tool and the powder leads to rapid heat transfer and relatively even heating over the entire cross-section of the sample. The heating takes place primarily via thermal conduction. In order to reduce the heat loss through thermal radiation, the die can optionally be thermally insulated, e.g. with a graphite felt. In the standard configuration, heating rates of up to approx. 300 K/min can be achieved in a FAST/SPS device. The high heating rates are one of the main reasons for the fast cycle times, as grain boundary and volume diffusion necessary for mass transport during sintering are activated directly. Due to the thermal mass of the tools, extremely high cooling rates cannot be achieved. Typical cooling rates are around 100 - 150 K/min. It should be noted here that the use of thermal insulation materials further reduces the cooling rates. In addition to the rapid heating, the sintering kinetics are also supported by the applied load. Depending on the type of system and sample size, compaction pressure in the range of 50 - 100 MPa can be achieved with the standard material graphite. Special grades of graphite allow maximum pressures of up to 200 MPa. When using graphite tools, temperatures of up to approx. 2,200 °C can be achieved in FAST/SPS devices. Alternative tools made of highly heat-resistant metals or electrically conductive ceramics enable pressures of up to 400 MPa, but the maximum permissible sintering temperatures are usually significantly lower in these cases. In order to improve the electrical contact between the punches, the die and the sample, a flexible, ideally electrically conductive foil is usually positioned between the punches and the sample. Graphite has also proven to be the standard material for this foil. FAST/SPS systems are usually controlled by programming the temperature-time curve. The measurement of the temperature as a major process parameter is carried out by axially or radially arranged pyrometers or by thermocouples. A direct measurement of the sample temperature is usually not possible. In order to measure the temperature as close as possible to the sample, holes are often drilled in the tools, at the bottom of which the temperature is measured. Furthermore, especially with increasing size of sintered parts and complexity of shape, it is recommended to predict the temperature distribution in the parts using suitable FEM modeling.

== Advantages and limitations of FAST/SPS ==
i.) '''Advantages:''' An essential feature of the FAST/SPS process is the rapid heating of the sample, which is based on the direct heating of the tool and the good heat transfer between the die and the powder. The superimposition of an uniaxial pressure during sintering further accelerates the sintering kinetics, so that the sintering temperature can often be significantly reduced compared to conventional sintering processes. Accordingly, the FAST/SPS process is a promising technology for

* '''Powder with low sintering activity:''' FAST/SPS enables the compaction of powders that have a low sintering activity (e.g. borides, carbides, nitrides and their mixtures).
* '''Powders with unfavorable powder properties:''' Powders can be sintered whose particle size distribution and morphology are unsuitable for conventional pressing and sintering.
* '''Nanoscale powders:''' The rapid processing in the case of FAST/SPS makes it possible to preserve the structure of nanoscale powders in the component.
* '''Materials with limited stability:''' FAST/SPS enables the sintering of materials that tend to decompose at high temperatures and long dwell times and to form undesirable secondary phases.
* '''Materials containing phases out of thermodynamic equilibrium:''' Phases out of thermodynamic equilibrium can be maintained in the sintered part (e.g. amorphous phases). Based on this, properties can be achieved that are not feasible with other sintering methods.
* '''Composite materials:''' FAST/SPS has great potential for sintering of composite materials that combine phases, which have large differences in their physical properties (e.g. very different melting points).
* '''Energy-efficient processing:''' In general, the FAST/SPS process is classified as an energy-efficient process due to the reduced sintering temperature and the short cycle times, but the degree of automation and the number of components per sintering cycle must also be taken carefully into account for an objective comparison with other sintering technologies.

ii.) '''Limitations:''' Despite the obvious advantages of FAST/SPS technology, there are also a number of process-related limitations.
* '''Risk of density and stress gradients in the component:''' If powders with a low thermal conductivity and high electrical resistance are sintered by FAST/SPS, there might arise an inhomogeneous temperature distribution in the component, which becomes more pronounced with increasing sample size. If exceeding a critical value, density and/or stress gradients in the sintered part result. There are also limitations with respect to the maximum height/diameter ratio. Similar to conventional pressing, wall friction can cause density gradients in the sintered part.
* '''Chemical and electrochemical interaction with the tool materials:''' The direct contact of the powder with the tools is advantageous with respect to heat transfer, but in the worst case it also leads to a chemical interaction with the tools or the inserted foils. When using graphite tools or foils, possible contamination of the component with carbon must be taken carefully into account. Therefore, adhering residues of the graphite foil and the reaction zone on the component surface must be removed mechanically, e.g. by grinding. In addition, it must be noted that the electrical field applied to the powder can trigger electrochemical reactions at the interfaces. A well-known effect is electrochemical blackening of oxide ceramics caused by the release of oxygen at low oxygen partial pressures. Furthermore, oxide ceramics that contain transition metals at the A or B position are sensitive to chemical expansion, which in the worst case leads to severe cracking in the component.
* '''Change of conductivity of semi-conductive and mixed-conductive materials:''' When sintering semi-conductive and mixed-conductive materials via FAST/SPS, it should be noted that the conductivity of the powder changes with increasing temperature and density during the FAST/SPS cycle. If the heating at the beginning of the sintering cycle is primarily based on heat conduction, this state might change suddenly if a current flow through the sample becomes possible when the temperature exceeds a specific value. The result is a complex sintering process that becomes difficult to control and which can impair reproducibility. This effect is used for specific kinds of field-assisted sintering, e.g. for flash sintering. For more details, see Chapter 8.
* '''Net-shaping:''' The FAST/SPS process reaches its limits when complex shapes are to be realized. In addition to the challenges of suitable tool design, increasing geometrical complexity might cause inhomogeneous temperature distribution and, in the case of conductive powders, inhomogeneous current flow over the entire sample cross-section. There are a number of approaches to manufacture complex shapes e.g. by using split tools or by sintering near net-shaped green parts in a powder bed directly via FAST/SPS. However, the possibilities for automating these technologies must be evaluated critical.
* '''Automation of the FAST/SPS process:''' At current state of development, cycle times in FAST/SPS systems cannot compete with conventional pressing and sintering, since a complete FAST/SPS cycle takes several minutes despite high heating rates and short dwell times. If insert foils are used to improve the electrical and thermal contact during tool assembly, this slows down the cycle time further. In order to operate FAST/SPS devices with higher productivity, partially automated, multiple tools (capacity up to several hundred components) are in use, which can optionally be filled with a robot system outside the device and then installed in the device via a manipulator. Another concept are FAST/SPS devices with a system of separate chambers in which the individual processing steps of tool assembly, powder filling, compression and cooling are carried out in a separate and sequential manner.

== How to conduct a standard FAST/SPS cycle ==
In this section, the processing steps for sintering a ceramic powder via FAST/SPS are explained in detail. For conducting FAST/SPS cycles, the following three devices are available at the institute IEK-1 ('''Figure 3''').

'''-> Figure 3''' 
'''Figure 3:''' ''FAST/SPS devices at the institute IEK-1 '''a.)''' Laboratory device HP-D 5 '''b.)''' Hybrid sintering system H-HP-D25 SD/FL/MoSi '''c.)''' Sintering press DSP515 on industrial scale.''

The '''HP-D 5 laboratory device''' is characterized by the following operating parameters:
* Type: HP-D 5
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 50 kN
* Maximum heating power: 37 kW
* Maximum sample diameter: 30 mm
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operating mode: FAST / SPS with pulsed direct current

The '''hybrid sintering device H-HP-D25 SD/FL/MoSi''' enables a number of different operating modes in addition to the conventional FAST/SPS mode through the optional application of additional heaters or operation with an external voltage source.
* Type: H-HP-D25 SD/FL/MoSi
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 250 kN
* Maximum sample diameter: 100 mm (FAST/SPS mode), 20 mm (Flash sintering mode)
* Maximum heating power (FAST / SPS): 60 kW
* Maximum heating power (Induction): 80 kW
* Maximum heating power (MoSi2): 10 kW
* Maximum heating power (Hybrid heating): 100 kW
* External voltage source: AC/DC, 1000 V, max. 25 A
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operation modes: i.) FAST / SPS with pulsed direct current ii.) Hybrid FAST/SPS with induction coil or MoSi2 furnace as additional heater iii.) Hot press with MoSi2 heater iv.) Flash SPS with defined heating power v.) Flash sintering with an external voltage source and MoSi2 heater.

The '''DSP515 sintering press''' is a device, which can be used for industrial production and enables the scaling up of promising results from experiments on lab-scale.
* Type: DSP515
* Manufacturer: Dr. Fritsch Sondermaschinen GmbH, Fellbach, Germany
* Maxiumum pressing force: 555 kN
* Electrode size: 180 x 180 mm2
* Maximum sample size: approx. 160 x 160 mm2
* Maximum heating power: 170 kW
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2
* Operating modes: i.) FAST/SPS with constant direct current ii.) Flash SPS with defined heating power.
* Debinding unit: The system is also equipped with a cooling trap for debinding of tape-cast parts.

Below, the steps of a standard FAST/SPS cycle using a graphite tool with a sample diameter of 20 mm are described. An additional graphite foil (thickness approx. 0.35 mm) is inserted into the graphite tool. The thickness of the foil must be taken into account when designing the tool. The inserted foil has two main functions. On the one hand, it improves the electrical and thermal contact between the punch and the die as well as between the powder, the face of the punch and the die. On the other hand, it avoids chemical interactions between powder and tool, so that the tool life is increased. The FAST/SPS cycle shown here was carried out in the HP-D 5 laboratory device.

i.) '''Sample preparation:''' '''Figure 4''' shows the parts of a lab-scale graphite tool (inner diameter 20 mm) as well as the graphite insert foils (thickness 0.35 mm), which are sized with respect to the tool dimensions. In a first step, the graphite foils are positioned on the inner wall of the die and on the faces of the punches. It is important that the foils has a tight contact to the tool components and that there are no kinks or gaps after positioning. For health protection, the graphite tool should be filled in a laboratory hood. Filling can be carried out on a balance. This increases the accuracy of the powder quantity weighed in.

'''-> Figure 4''' 
'''Figure 4:''' ''Preparation of the graphite tool and the insert foil for the FAST/SPS cycle. For accurate sample preparation, the powder should be directly balanced in the tool. Furthermore, it is recommended to handle the powder in a hood.''

After filling in the tool, the powder is covered with an additional graphite foil and pre-pressed in a manual laboratory press with 50 MPa (16 KN for diameter 20 mm tool) ('''Figure 5'''). In order to avoid sticking of powder particles on the face the upper punch, the upper punch is removed again and powder residues are manually removed. Afterwards, the upper punch is placed again in the tool.

'''-> Figure 5''' 
'''Figure 5:''' '''''a.)''' Filling the mold and positioning the graphite foil '''b.)''' Pre-pressing of the FAST/SPS sample in a manual hand press '''c.)''' Removal of the upper punch after the pressing process and removal of adhering powder particles.''

ii.) '''Mounting of the tool and programming the FAST/SPS device:''' At the laboratory system HP-D 5, the programming of the FAST/SPS parameters can be done via a process controller type Stange SE607 ('''Figure 6'''). The main operating parameters temperature, pressing force, pulse length of the current and moving speed of the lower electrode is programmed in individual program segments. During the FAST/SPS cycle, all process data are shown on the controller display as a numerical values and as a time-resolved graph. In parallel, all data are saved via a data logger integrated in the system. By default, the data are transferred to an external PC for data management and further evaluation. Individual parameter sets of the users are also stored on the PC and can be easily transferred to the controller if required.

'''-> Figure 6''' 
'''Figure 6:''' ''Display of the controller of the HP-D 5 device giving a compact overview of all process-relevant data.''

'''Figure 7''' shows the graphite tool mounted into the HP-D 5 devices as well as the CuBe electrodes. Optionally, the graphite tool can be thermally isolated with a jacket made of a graphite felt (not shown here). A graphite cord can be used to fix the graphite felt on the tool.

'''-> Figure 7''' 
'''Figure 7:''' ''View on the processing chamber of the HP-D 5 device with mounted graphite tool. When installing the tool and the two cones, it should be noted that graphite is a brittle and shock-sensitive material and therefore breaks very easily. For this reason, sudden contact of all graphite parts with the other system components (stamp, chamber walls) must be avoided.''

After the graphite tool has been inserted and fixed by lifting the lower punch, the container door is closed and the FAST/SPS cycle can be started.

iii.) '''Choice and regulation of the sintering atmosphere:''' A FAST/SPS cycle is usually carried out in vacuum or under protective gas atmosphere. Accordingly, the process chamber is evacuated by a vacuum pump at the beginning of the cycle. In the laboratory device HP-D 5, a vacuum of approx. 0.5 mbar is achieved; in larger systems, this value can also be higher (e.g. 20 mbar for the DSP515). The quality of the vacuum depends on the sealing of the process chamber and the power of the vacuum pump. If aiming on a high vacuum, cost of the FAST/SPS device significantly increases. After evacuation, the chamber can optionally be flooded with gases such as N2, Ar or Ar/H2 (static atmosphere control) or a continuous gas flow (dynamic atmosphere control). Figure 8 shows the valves for feeding the individual gases from the institute's gas store into the system. The evacuation of the process chamber and the optional supply of protective gases to the process chamber is regulated by the system control and takes place automated. The pressure in the process chamber is continuously recorded in the HP-D 5 device by two sensors with different measuring ranges (coarse sensor 1.0 - 1300 mbar, fine sensor 0.01 - 13 mbar), which are positioned at the gas outlet. For operation of the system under relative pressure (reduced pressure in relation to the ambient pressure), the system is also equipped with a relative pressure sensor, which enables to regulate the relative pressure in the range of 5 - 50 mbar. Static or dynamic operation is also possible in the relative pressure mode. A safety valve is used to protect the processing chamber against overpressure. The valve opens at an overpressure of 100 mbar above the ambient pressure. The pressure curve during the FAST/SPS cycle is recorded continuously. An analysis of the pressure curve can be helpful if components outgas from the sample or if the sample decomposes under the FAST/SPS conditions.

'''-> Figure 8''' 
'''Figure 8:''' ''Valves for flooding the processing chamber with the protective gases Ar, N2, Ar/H2.''

When sintering oxide ceramics via FAST/SPS, it should be noted that the sintering conditions have a reducing effect, i.e. there is a release oxygen atoms from the lattice, which increases with decreasing oxygen partial pressure. The effect is aggravated in the case of direct contact with the graphite tools or the graphite foils. The release of oxygen is visually noticeable in the darkening of the ceramic. This effect is superimposed by the uptake of carbon. If the release of oxygen exceeds a critical value, the sample can undergo chemical expansion, which can be up to several percent (as e.g. the case for gadolinium-doped cerium oxide or barium-strontium-cobalt oxides). Usually, this effect leads to severe cracking of the sample. Furthermore, the crystal lattice can become unstable if the oxygen release progresses further. In worst case, reduction of components down to the metallic phase might appear.

In principle, it is possible to operate a FAST/SPS device with technical air. Such operation must be done with special care, since most materials used for the tools are unstable in air and start to strongly oxidize if the temperature exceeds a critical value (usually around 400°C). It should also be noted that the powder in the tool is encapsulated in such a way that the access of oxygen to the powder is prevented to a large extent.

iv.) '''Performing of the FAST/SPS cycle:''' After the device has been prepared, the selected program is started and runs automatically. '''Figure 9''' shows the graphite die during the heating process. As already mentioned, the operation of FAST/SPS devices is usually temperature-controlled. This means that the controller defines the temperature and the system regulates the current and voltage in such a way that the temperature profile is adhered to the specification as precisely as possible. In order to keep the deviations from the programmed temperature curve as low as possible, the system is equipped with a PID control (PID = Proportional-Integral-Derivative). This control unit iteratively adapt the optimal current and voltage curves for heating the tool to the respective electrical resistance of the tool.

'''-> Figure 9''' 
'''Figure 9:''' ''View on the heated graphite tool (punch diameter 20 mm) in the laboratory device HP-D 5. When operating a FAST/SPS system, it should be noted that the high currents in the system cause strong electromagnetic fields, which can damage pacemakers and others sensitive electronic devices.''

v.) Demoulding of the samples
At the end of the cycle, the sample can be pressed out of the graphite tool using a hand press, as shown in '''Figure 10'''.

'''-> Figure 10''' 
'''Figure 10:''' ''Demoulding the sample from the FAST/SPS tool using a hand press. When removing the tool from the FAST/SPS device, please take care since the tool can still be hot.''

== Tool design and tool materials ==
In most cases, graphite tools are used in FAST/SPS systems. '''Figure 10''' shows a selection of graphite tools for the laboratory system HP-D 5 with punch diameters of 12, 20 and 30 mm and for the hybrid sintering device H-HP-D25 with a punch diameter of 100 mm.

'''-> Figure 10'''
'''Figure 10:''' ''Graphite tools for performing FAST/SPS cycles '''a.)''' Overview: die, punch with hole for pyrometer, cone for adaptation to the geometry of the electrodes of the FAST/SPS device '''b.)''' Tools for the laboratory device HP-D 5 with a diameter of 12, 20 and 30 mm and '''c.)''' Tools for the hybrid sintering device H-HP-D25 with a diameter of 100 mm.''

The use of graphite has the advantage that it is easy to machine the tools. Furthermore, it has an electrical resistance that is favorable for Joule heating. Temperatures of up to around 2,200 °C can be achieved in graphite tools. The compressive strength of standard grades is approx. 50 - 100 MPa (e.g. Sigrafine R7710, SGL Carbon GmbH), special grades achieve compressive strengths of up to 230 MPa (e.g. Grade 2334, Mersen). It should be noted that the geometry of the tool also has an influence on the maximum permissible pressure, e.g. the notch effect of a hole drilled for temperature measurement can lead to failure of the tool even at low pressures. Above 450 °C, graphite tools can only be used in a vacuum or under protective gas (e.g. Ar). If a tool is used frequently, attention must also be paid to possible wear, which can reduce the dimensional accuracy of the sintered parts.

If pressures well above 100 MPa or long tool life are desired, the following materials can used as alternative to graphite. At temperatures up to 600 °C, the use of a high-speed steel (e.g. W360, Böhler) is recommended, which can resist pressures of up to 400 MPa. If higher temperatures are desired, Mo alloys (e.g. Ti-Zr-Mo TZM, Plansee) can be used, which enable maximum temperature of approx. 1100 ° C and maximum pressure of 350 MPa. The maximum operating temperature of metal tools is limited by the onset of creep processes and severe grain coarsening. Both effects can cause a macroscopic deformation of the tools, so that in the worst case the punch can become jammed in the die. '''Figure 11''' shows as an example tools made of W360 steel and TZM.

'''-> Figure 11'''
'''Figure 11:''' ''Metallic tools '''a.)''' Overview: Die, punch, and cone of a tool made of W360 steel '''b.)''' Same tool in the assembled state '''c.)''' Similar tool made of TZM.''

If even higher temperatures or pressures are desired, the literature reports on tools made of conductive ceramics. Suitable materials are tungsten carbide or silicon carbide, which are already used in the laboratory up to pressures of 1000 MPa. When using ceramic tools, the high effort in production and the inherent brittleness must be taken into account. Careful handling is strictly required in order to avoid breakage.

When using metallic and ceramic tools, it should be noted that these materials usually have a different electrical resistance than graphite. This has an influence on the system control and may require an adjustment of the PID parameters for precise temperature control (see Chapter 4).

== Measurement of temperature ==
The temperature is the main parameter for controlling the FAST/SPS system. The exact measurement and control of temperature is one of the great challenges when applying of FAST/SPS technology. The high heating rates require a temperature measurement with short response time, short delay time and high reproducibility. A direct measurement of the sample temperature is not possible with reasonable effort. Therefore, the measurement should be conducted as close to the sample as possible. For this purpose, vertical or horizontal holes are usually drilled in the FAST/SPS tool. By adjusting the pyrometer or thermocouple at the bottom of these holes, the temperature can be measured in direct vicinity of the sample.

i.) '''Measurement of the temperature with the pyrometer:''' Pyrometers are preferably used for temperature measurement at high temperatures. The usual measuring range of pyrometers is 600 - 3000 °C. '''Figure 12a''' shows the pyrometer installed in the HP-D 5 laboratory device. In this case, the measurement signal is deflected via a prism so that the measurement can be carried out vertically in a hole drilled in the upper punch.

In FAST / SPS systems with additional heater (e.g. hybrid sintering device H-HP-D 25), the pyrometer for controlling the additional heating is installed on the side. The measurement is carried out through a sight glass in the furnace door.

ii.) '''Measurement of the temperature with thermocouples:''' Thermocouples are necessarily required for a regulated temperature control of the system at temperatures < 600 °C, since pyrometers do not work reliably in this temperature range. There is also the option of using thermocouples at higher temperatures. Thermocouples of type K (Ni-CrNi) are suitable for the temperature range RT - 1100 ° C and are comparatively inexpensive. Because of the ductility of Ni, type K thermocouples are flexible. For protection, the thermocouples are enclosed in a steel jacket. Type C thermocouples (W5Re-W26Re) with a molybdenum housing enable temperature measurement in the range of RT - 2,200 ° C. The materials used are brittle and expensive, so that their application requires careful handling. Regardless of whether the housing is made of steel or molybdenum, care must be taken that there is no chemical interaction with the tool material during the sintering cycle. '''Figure 12b''' shows a graphite tool equipped with multiple type K thermocouples. One of the thermocouples is used for controlling the heating cycle by temperature measurement of the die and is flexibly installed. Two further thermocouples are firmly fixed to the upper and lower electrodes of the system and serve to protect the water-cooled CuBe electrodes from overheating.

'''-> Figure 12'''
'''Figure 12:''' ''Temperature measurement in the laboratory system HP-D 5 '''a.)''' Pyrometer for measuring the temperature of the upper punch, deflection of the measurement signal via a prism inside the device '''b.)''' Flexible thermocouples of type K. When installing the thermocouples, it must made sure that there is no contact between the thermocouple and the container wall in order to avoid short circuiting.''

In general, it should be noted that temperature differences of significantly more than 10 K can occur between the pyrometer and thermocouples when identical operating parameters are used. In order to be able to predict the temperature distribution in the component with good accuracy, it is highly recommended to carry out an accompanying FEM modeling of the temperature distribution. The combination of experiment and modeling is the basis for reliably designing the tools and achieving high reproducibility of the FAST/SPS cycles. Another possibility for estimating the temperature distribution is the use of a "dummy" tool without powder cavity, which is equipped with thermocouples in as many places as possible. It should also be noted that the temperature gradients increase with tool size. In industrial production, temperature gradients of up to 80 K can occur in multi-component tools (up to 500 components per cycle), especially at the beginning of the cycle. When supporting tool design by FEM modeling, temperature deviations can be reduced to below 20 K.

== Applications of FAST/SPS ==

== Alternative operation modes of FAST/SPS devices ==

Field assisted sintering technology/spark plasma sintering

2021-08-05T06:58:30Z

M.bram: /* How to conduct a standard FAST/SPS cycle */

== General principle of FAST/SPS ==
Field Assisted Sintering Technology/Spark Plasma Sintering (FAST/SPS) is a low-voltage, current-activated and pressure-supported sintering process that is based on Joule heating (= resistance heating) of the conductive tools ('''Figure 1''') and is characterized by high heating rates and short cycle times. If electrically conductive powders are applied, the powder itself is also heated directly via the Joule effect. The FAST/SPS process is established in the industry and particularly promising when powders are to be sintered, which have a low sintering activity or an unfavorable particle morphology and particle size distribution for conventional pressing and sintering. Furthermore, the method is well suited for the production of composite materials, especially when phases will be combined, which have very different physical properties. Some typical application examples of FAST/SPS technology are presented in Chapter 7. Due to the great flexibility, the short cycle times and the comparatively simple and cost-effective production of tools, research and development is another important field of application for FAST/SPS technology and is widespread there.

[[File:Wiki Keramik FAST SPS Abb 01.jpg|thumb|center]]
'''Figure 1:''' ''Heated graphite tool in a FAST / SPS device.''

In principle, a FAST/SPS device is a mechanical press, which at the same time also forms a high-energy current circuit. The FAST/SPS process is carried out in a conductive tool consisting of two punches and a die. Two additional cones establish the contact with the device's electrodes. The pressing force is also applied via these electrodes by means of a hydraulic pressure cylinder. '''Figure 2''' shows a schematic sketch of such a device. FAST/SPS processes are usually carried out in a vacuum or protective gas to protect the tool and the powder inside the tool from oxidation. Accordingly, the pressing device is located in a water-cooled chamber, in which a moderate vacuum (0.5 - 20 mbar) or a defined protective gas atmosphere (e.g. Ar or N2) can be set. The heating of the tool via the Joule effect requires the use of conductive materials for the punch and the die. The standard material for punch and die is graphite, alternatives to this are introduced in Chapter 4.

[[File:Wiki Keramik FAST SPS Abb 02 englisch.jpg|thumb|center]]
'''Figure 2:''' ''Schematic sketch of a FAST/SPS device.''

The tool is heated by a continuous or pulsed direct current with moderate voltages <10 V and high currents in the range from 1 to several 10 kA (depending on the size of the device). Non-conductive powders can also be sintered in good quality via FAST/SPS. Here, the direct contact between the tool and the powder leads to rapid heat transfer and relatively even heating over the entire cross-section of the sample. The heating takes place primarily via thermal conduction. In order to reduce the heat loss through thermal radiation, the die can optionally be thermally insulated, e.g. with a graphite felt. In the standard configuration, heating rates of up to approx. 300 K/min can be achieved in a FAST/SPS device. The high heating rates are one of the main reasons for the fast cycle times, as grain boundary and volume diffusion necessary for mass transport during sintering are activated directly. Due to the thermal mass of the tools, extremely high cooling rates cannot be achieved. Typical cooling rates are around 100 - 150 K/min. It should be noted here that the use of thermal insulation materials further reduces the cooling rates. In addition to the rapid heating, the sintering kinetics are also supported by the applied load. Depending on the type of system and sample size, compaction pressure in the range of 50 - 100 MPa can be achieved with the standard material graphite. Special grades of graphite allow maximum pressures of up to 200 MPa. When using graphite tools, temperatures of up to approx. 2,200 °C can be achieved in FAST/SPS devices. Alternative tools made of highly heat-resistant metals or electrically conductive ceramics enable pressures of up to 400 MPa, but the maximum permissible sintering temperatures are usually significantly lower in these cases. In order to improve the electrical contact between the punches, the die and the sample, a flexible, ideally electrically conductive foil is usually positioned between the punches and the sample. Graphite has also proven to be the standard material for this foil. FAST/SPS systems are usually controlled by programming the temperature-time curve. The measurement of the temperature as a major process parameter is carried out by axially or radially arranged pyrometers or by thermocouples. A direct measurement of the sample temperature is usually not possible. In order to measure the temperature as close as possible to the sample, holes are often drilled in the tools, at the bottom of which the temperature is measured. Furthermore, especially with increasing size of sintered parts and complexity of shape, it is recommended to predict the temperature distribution in the parts using suitable FEM modeling.

== Advantages and limitations of FAST/SPS ==
i.) '''Advantages:''' An essential feature of the FAST/SPS process is the rapid heating of the sample, which is based on the direct heating of the tool and the good heat transfer between the die and the powder. The superimposition of an uniaxial pressure during sintering further accelerates the sintering kinetics, so that the sintering temperature can often be significantly reduced compared to conventional sintering processes. Accordingly, the FAST/SPS process is a promising technology for

* '''Powder with low sintering activity:''' FAST/SPS enables the compaction of powders that have a low sintering activity (e.g. borides, carbides, nitrides and their mixtures).
* '''Powders with unfavorable powder properties:''' Powders can be sintered whose particle size distribution and morphology are unsuitable for conventional pressing and sintering.
* '''Nanoscale powders:''' The rapid processing in the case of FAST/SPS makes it possible to preserve the structure of nanoscale powders in the component.
* '''Materials with limited stability:''' FAST/SPS enables the sintering of materials that tend to decompose at high temperatures and long dwell times and to form undesirable secondary phases.
* '''Materials containing phases out of thermodynamic equilibrium:''' Phases out of thermodynamic equilibrium can be maintained in the sintered part (e.g. amorphous phases). Based on this, properties can be achieved that are not feasible with other sintering methods.
* '''Composite materials:''' FAST/SPS has great potential for sintering of composite materials that combine phases, which have large differences in their physical properties (e.g. very different melting points).
* '''Energy-efficient processing:''' In general, the FAST/SPS process is classified as an energy-efficient process due to the reduced sintering temperature and the short cycle times, but the degree of automation and the number of components per sintering cycle must also be taken carefully into account for an objective comparison with other sintering technologies.

ii.) '''Limitations:''' Despite the obvious advantages of FAST/SPS technology, there are also a number of process-related limitations.
* '''Risk of density and stress gradients in the component:''' If powders with a low thermal conductivity and high electrical resistance are sintered by FAST/SPS, there might arise an inhomogeneous temperature distribution in the component, which becomes more pronounced with increasing sample size. If exceeding a critical value, density and/or stress gradients in the sintered part result. There are also limitations with respect to the maximum height/diameter ratio. Similar to conventional pressing, wall friction can cause density gradients in the sintered part.
* '''Chemical and electrochemical interaction with the tool materials:''' The direct contact of the powder with the tools is advantageous with respect to heat transfer, but in the worst case it also leads to a chemical interaction with the tools or the inserted foils. When using graphite tools or foils, possible contamination of the component with carbon must be taken carefully into account. Therefore, adhering residues of the graphite foil and the reaction zone on the component surface must be removed mechanically, e.g. by grinding. In addition, it must be noted that the electrical field applied to the powder can trigger electrochemical reactions at the interfaces. A well-known effect is electrochemical blackening of oxide ceramics caused by the release of oxygen at low oxygen partial pressures. Furthermore, oxide ceramics that contain transition metals at the A or B position are sensitive to chemical expansion, which in the worst case leads to severe cracking in the component.
* '''Change of conductivity of semi-conductive and mixed-conductive materials:''' When sintering semi-conductive and mixed-conductive materials via FAST/SPS, it should be noted that the conductivity of the powder changes with increasing temperature and density during the FAST/SPS cycle. If the heating at the beginning of the sintering cycle is primarily based on heat conduction, this state might change suddenly if a current flow through the sample becomes possible when the temperature exceeds a specific value. The result is a complex sintering process that becomes difficult to control and which can impair reproducibility. This effect is used for specific kinds of field-assisted sintering, e.g. for flash sintering. For more details, see Chapter 8.
* '''Net-shaping:''' The FAST/SPS process reaches its limits when complex shapes are to be realized. In addition to the challenges of suitable tool design, increasing geometrical complexity might cause inhomogeneous temperature distribution and, in the case of conductive powders, inhomogeneous current flow over the entire sample cross-section. There are a number of approaches to manufacture complex shapes e.g. by using split tools or by sintering near net-shaped green parts in a powder bed directly via FAST/SPS. However, the possibilities for automating these technologies must be evaluated critical.
* '''Automation of the FAST/SPS process:''' At current state of development, cycle times in FAST/SPS systems cannot compete with conventional pressing and sintering, since a complete FAST/SPS cycle takes several minutes despite high heating rates and short dwell times. If insert foils are used to improve the electrical and thermal contact during tool assembly, this slows down the cycle time further. In order to operate FAST/SPS devices with higher productivity, partially automated, multiple tools (capacity up to several hundred components) are in use, which can optionally be filled with a robot system outside the device and then installed in the device via a manipulator. Another concept are FAST/SPS devices with a system of separate chambers in which the individual processing steps of tool assembly, powder filling, compression and cooling are carried out in a separate and sequential manner.

== How to conduct a standard FAST/SPS cycle ==
In this section, the processing steps for sintering a ceramic powder via FAST/SPS are explained in detail. For conducting FAST/SPS cycles, the following three devices are available at the institute IEK-1 ('''Figure 3''').

'''-> Figure 3''' 
'''Figure 3:''' ''FAST/SPS devices at the institute IEK-1 '''a.)''' Laboratory device HP-D 5 '''b.)''' Hybrid sintering system H-HP-D25 SD/FL/MoSi '''c.)''' Sintering press DSP515 on industrial scale.''

The '''HP-D 5 laboratory device''' is characterized by the following operating parameters:
* Type: HP-D 5
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 50 kN
* Maximum heating power: 37 kW
* Maximum sample diameter: 30 mm
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operating mode: FAST / SPS with pulsed direct current

The '''hybrid sintering device H-HP-D25 SD/FL/MoSi''' enables a number of different operating modes in addition to the conventional FAST/SPS mode through the optional application of additional heaters or operation with an external voltage source.
* Type: H-HP-D25 SD/FL/MoSi
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 250 kN
* Maximum sample diameter: 100 mm (FAST/SPS mode), 20 mm (Flash sintering mode)
* Maximum heating power (FAST / SPS): 60 kW
* Maximum heating power (Induction): 80 kW
* Maximum heating power (MoSi2): 10 kW
* Maximum heating power (Hybrid heating): 100 kW
* External voltage source: AC/DC, 1000 V, max. 25 A
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operation modes: i.) FAST / SPS with pulsed direct current ii.) Hybrid FAST/SPS with induction coil or MoSi2 furnace as additional heater iii.) Hot press with MoSi2 heater iv.) Flash SPS with defined heating power v.) Flash sintering with an external voltage source and MoSi2 heater.

The '''DSP515 sintering press''' is a device, which can be used for industrial production and enables the scaling up of promising results from experiments on lab-scale.
* Type: DSP515
* Manufacturer: Dr. Fritsch Sondermaschinen GmbH, Fellbach, Germany
* Maxiumum pressing force: 555 kN
* Electrode size: 180 x 180 mm2
* Maximum sample size: approx. 160 x 160 mm2
* Maximum heating power: 170 kW
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2
* Operating modes: i.) FAST/SPS with constant direct current ii.) Flash SPS with defined heating power.
* Debinding unit: The system is also equipped with a cooling trap for debinding of tape-cast parts.

Below, the steps of a standard FAST/SPS cycle using a graphite tool with a sample diameter of 20 mm are described. An additional graphite foil (thickness approx. 0.35 mm) is inserted into the graphite tool. The thickness of the foil must be taken into account when designing the tool. The inserted foil has two main functions. On the one hand, it improves the electrical and thermal contact between the punch and the die as well as between the powder, the face of the punch and the die. On the other hand, it avoids chemical interactions between powder and tool, so that the tool life is increased. The FAST/SPS cycle shown here was carried out in the HP-D 5 laboratory device.

i.) '''Sample preparation:''' '''Figure 4''' shows the parts of a lab-scale graphite tool (inner diameter 20 mm) as well as the graphite insert foils (thickness 0.35 mm), which are sized with respect to the tool dimensions. In a first step, the graphite foils are positioned on the inner wall of the die and on the faces of the punches. It is important that the foils has a tight contact to the tool components and that there are no kinks or gaps after positioning. For health protection, the graphite tool should be filled in a laboratory hood. Filling can be carried out on a balance. This increases the accuracy of the powder quantity weighed in.

'''-> Figure 4''' 
'''Figure 4:''' ''Preparation of the graphite tool and the insert foil for the FAST/SPS cycle. For accurate sample preparation, the powder should be directly balanced in the tool. Furthermore, it is recommended to handle the powder in a hood.''

After filling in the tool, the powder is covered with an additional graphite foil and pre-pressed in a manual laboratory press with 50 MPa (16 KN for diameter 20 mm tool) ('''Figure 5'''). In order to avoid sticking of powder particles on the face the upper punch, the upper punch is removed again and powder residues are manually removed. Afterwards, the upper punch is placed again in the tool.

'''-> Figure 5''' 
'''Figure 5:''' '''''a.)''' Filling the mold and positioning the graphite foil '''b.)''' Pre-pressing of the FAST/SPS sample in a manual hand press '''c.)''' Removal of the upper punch after the pressing process and removal of adhering powder particles.''

ii.) '''Mounting of the tool and programming the FAST/SPS device:''' At the laboratory system HP-D 5, the programming of the FAST/SPS parameters can be done via a process controller type Stange SE607 ('''Figure 6'''). The main operating parameters temperature, pressing force, pulse length of the current and moving speed of the lower electrode is programmed in individual program segments. During the FAST/SPS cycle, all process data are shown on the controller display as a numerical values and as a time-resolved graph. In parallel, all data are saved via a data logger integrated in the system. By default, the data are transferred to an external PC for data management and further evaluation. Individual parameter sets of the users are also stored on the PC and can be easily transferred to the controller if required.

'''-> Figure 6''' 
'''Figure 6:''' ''Display of the controller of the HP-D 5 device giving a compact overview of all process-relevant data.''

'''Figure 7''' shows the graphite tool mounted into the HP-D 5 devices as well as the CuBe electrodes. Optionally, the graphite tool can be thermally isolated with a jacket made of a graphite felt (not shown here). A graphite cord can be used to fix the graphite felt on the tool.

'''-> Figure 7''' 
'''Figure 7:''' ''View on the processing chamber of the HP-D 5 device with mounted graphite tool. When installing the tool and the two cones, it should be noted that graphite is a brittle and shock-sensitive material and therefore breaks very easily. For this reason, sudden contact of all graphite parts with the other system components (stamp, chamber walls) must be avoided.''

After the graphite tool has been inserted and fixed by lifting the lower punch, the container door is closed and the FAST/SPS cycle can be started.

iii.) '''Choice and regulation of the sintering atmosphere:''' A FAST/SPS cycle is usually carried out in vacuum or under protective gas atmosphere. Accordingly, the process chamber is evacuated by a vacuum pump at the beginning of the cycle. In the laboratory device HP-D 5, a vacuum of approx. 0.5 mbar is achieved; in larger systems, this value can also be higher (e.g. 20 mbar for the DSP515). The quality of the vacuum depends on the sealing of the process chamber and the power of the vacuum pump. If aiming on a high vacuum, cost of the FAST/SPS device significantly increases. After evacuation, the chamber can optionally be flooded with gases such as N2, Ar or Ar/H2 (static atmosphere control) or a continuous gas flow (dynamic atmosphere control). Figure 8 shows the valves for feeding the individual gases from the institute's gas store into the system. The evacuation of the process chamber and the optional supply of protective gases to the process chamber is regulated by the system control and takes place automated. The pressure in the process chamber is continuously recorded in the HP-D 5 device by two sensors with different measuring ranges (coarse sensor 1.0 - 1300 mbar, fine sensor 0.01 - 13 mbar), which are positioned at the gas outlet. For operation of the system under relative pressure (reduced pressure in relation to the ambient pressure), the system is also equipped with a relative pressure sensor, which enables to regulate the relative pressure in the range of 5 - 50 mbar. Static or dynamic operation is also possible in the relative pressure mode. A safety valve is used to protect the processing chamber against overpressure. The valve opens at an overpressure of 100 mbar above the ambient pressure. The pressure curve during the FAST/SPS cycle is recorded continuously. An analysis of the pressure curve can be helpful if components outgas from the sample or if the sample decomposes under the FAST/SPS conditions.

'''-> Figure 8''' 
'''Figure 8:''' ''Valves for flooding the processing chamber with the protective gases Ar, N2, Ar/H2.''

When sintering oxide ceramics via FAST/SPS, it should be noted that the sintering conditions have a reducing effect, i.e. there is a release oxygen atoms from the lattice, which increases with decreasing oxygen partial pressure. The effect is aggravated in the case of direct contact with the graphite tools or the graphite foils. The release of oxygen is visually noticeable in the darkening of the ceramic. This effect is superimposed by the uptake of carbon. If the release of oxygen exceeds a critical value, the sample can undergo chemical expansion, which can be up to several percent (as e.g. the case for gadolinium-doped cerium oxide or barium-strontium-cobalt oxides). Usually, this effect leads to severe cracking of the sample. Furthermore, the crystal lattice can become unstable if the oxygen release progresses further. In worst case, reduction of components down to the metallic phase might appear.

In principle, it is possible to operate a FAST/SPS device with technical air. Such operation must be done with special care, since most materials used for the tools are unstable in air and start to strongly oxidize if the temperature exceeds a critical value (usually around 400°C). It should also be noted that the powder in the tool is encapsulated in such a way that the access of oxygen to the powder is prevented to a large extent.

iv.) '''Performing of the FAST/SPS cycle:''' After the device has been prepared, the selected program is started and runs automatically. '''Figure 9''' shows the graphite die during the heating process. As already mentioned, the operation of FAST/SPS devices is usually temperature-controlled. This means that the controller defines the temperature and the system regulates the current and voltage in such a way that the temperature profile is adhered to the specification as precisely as possible. In order to keep the deviations from the programmed temperature curve as low as possible, the system is equipped with a PID control (PID = Proportional-Integral-Derivative). This control unit iteratively adapt the optimal current and voltage curves for heating the tool to the respective electrical resistance of the tool.

'''-> Figure 9''' 
'''Figure 9:''' ''View on the heated graphite tool (punch diameter 20 mm) in the laboratory device HP-D 5. When operating a FAST/SPS system, it should be noted that the high currents in the system cause strong electromagnetic fields, which can damage pacemakers and others sensitive electronic devices.''

v.) Demoulding of the samples
At the end of the cycle, the sample can be pressed out of the graphite tool using a hand press, as shown in '''Figure 10'''.

'''-> Figure 10'''
'''Figure 10:''' Demoulding the sample from the FAST/SPS tool using a hand press. When removing the tool from the FAST/SPS device, please take care since the tool can still be hot.

== Tool design and tool materials ==
In most cases, graphite tools are used in FAST/SPS systems. '''Figure 10''' shows a selection of graphite tools for the laboratory system HP-D 5 with punch diameters of 12, 20 and 30 mm and for the hybrid sintering device H-HP-D25 with a punch diameter of 100 mm.

'''-> Figure 10'''
'''Figure 10:''' ''Graphite tools for performing FAST/SPS cycles '''a.)''' Overview: die, punch with hole for pyrometer, cone for adaptation to the geometry of the electrodes of the FAST/SPS device '''b.)''' Tools for the laboratory device HP-D 5 with a diameter of 12, 20 and 30 mm and '''c.)''' Tools for the hybrid sintering device H-HP-D25 with a diameter of 100 mm.''

The use of graphite has the advantage that it is easy to machine the tools. Furthermore, it has an electrical resistance that is favorable for Joule heating. Temperatures of up to around 2,200 °C can be achieved in graphite tools. The compressive strength of standard grades is approx. 50 - 100 MPa (e.g. Sigrafine R7710, SGL Carbon GmbH), special grades achieve compressive strengths of up to 230 MPa (e.g. Grade 2334, Mersen). It should be noted that the geometry of the tool also has an influence on the maximum permissible pressure, e.g. the notch effect of a hole drilled for temperature measurement can lead to failure of the tool even at low pressures. Above 450 °C, graphite tools can only be used in a vacuum or under protective gas (e.g. Ar). If a tool is used frequently, attention must also be paid to possible wear, which can reduce the dimensional accuracy of the sintered parts.

If pressures well above 100 MPa or long tool life are desired, the following materials can used as alternative to graphite. At temperatures up to 600 °C, the use of a high-speed steel (e.g. W360, Böhler) is recommended, which can resist pressures of up to 400 MPa. If higher temperatures are desired, Mo alloys (e.g. Ti-Zr-Mo TZM, Plansee) can be used, which enable maximum temperature of approx. 1100 ° C and maximum pressure of 350 MPa. The maximum operating temperature of metal tools is limited by the onset of creep processes and severe grain coarsening. Both effects can cause a macroscopic deformation of the tools, so that in the worst case the punch can become jammed in the die. '''Figure 11''' shows as an example tools made of W360 steel and TZM.

'''-> Figure 11'''
'''Figure 11:''' ''Metallic tools '''a.)''' Overview: Die, punch, and cone of a tool made of W360 steel '''b.)''' Same tool in the assembled state '''c.)''' Similar tool made of TZM.''

If even higher temperatures or pressures are desired, the literature reports on tools made of conductive ceramics. Suitable materials are tungsten carbide or silicon carbide, which are already used in the laboratory up to pressures of 1000 MPa. When using ceramic tools, the high effort in production and the inherent brittleness must be taken into account. Careful handling is strictly required in order to avoid breakage.

When using metallic and ceramic tools, it should be noted that these materials usually have a different electrical resistance than graphite. This has an influence on the system control and may require an adjustment of the PID parameters for precise temperature control (see Chapter 4).

== Measurement of temperature ==
The temperature is the main parameter for controlling the FAST/SPS system. The exact measurement and control of temperature is one of the great challenges when applying of FAST/SPS technology. The high heating rates require a temperature measurement with short response time, short delay time and high reproducibility. A direct measurement of the sample temperature is not possible with reasonable effort. Therefore, the measurement should be conducted as close to the sample as possible. For this purpose, vertical or horizontal holes are usually drilled in the FAST/SPS tool. By adjusting the pyrometer or thermocouple at the bottom of these holes, the temperature can be measured in direct vicinity of the sample.

i.) '''Measurement of the temperature with the pyrometer:''' Pyrometers are preferably used for temperature measurement at high temperatures. The usual measuring range of pyrometers is 600 - 3000 °C. '''Figure 12a''' shows the pyrometer installed in the HP-D 5 laboratory device. In this case, the measurement signal is deflected via a prism so that the measurement can be carried out vertically in a hole drilled in the upper punch.

In FAST / SPS systems with additional heater (e.g. hybrid sintering device H-HP-D 25), the pyrometer for controlling the additional heating is installed on the side. The measurement is carried out through a sight glass in the furnace door.

ii.) '''Measurement of the temperature with thermocouples:''' Thermocouples are necessarily required for a regulated temperature control of the system at temperatures < 600 °C, since pyrometers do not work reliably in this temperature range. There is also the option of using thermocouples at higher temperatures. Thermocouples of type K (Ni-CrNi) are suitable for the temperature range RT - 1100 ° C and are comparatively inexpensive. Because of the ductility of Ni, type K thermocouples are flexible. For protection, the thermocouples are enclosed in a steel jacket. Type C thermocouples (W5Re-W26Re) with a molybdenum housing enable temperature measurement in the range of RT - 2,200 ° C. The materials used are brittle and expensive, so that their application requires careful handling. Regardless of whether the housing is made of steel or molybdenum, care must be taken that there is no chemical interaction with the tool material during the sintering cycle. '''Figure 12b''' shows a graphite tool equipped with multiple type K thermocouples. One of the thermocouples is used for controlling the heating cycle by temperature measurement of the die and is flexibly installed. Two further thermocouples are firmly fixed to the upper and lower electrodes of the system and serve to protect the water-cooled CuBe electrodes from overheating.

'''-> Figure 12'''
'''Figure 12:''' ''Temperature measurement in the laboratory system HP-D 5 '''a.)''' Pyrometer for measuring the temperature of the upper punch, deflection of the measurement signal via a prism inside the device '''b.)''' Flexible thermocouples of type K. When installing the thermocouples, it must made sure that there is no contact between the thermocouple and the container wall in order to avoid short circuiting.''

In general, it should be noted that temperature differences of significantly more than 10 K can occur between the pyrometer and thermocouples when identical operating parameters are used. In order to be able to predict the temperature distribution in the component with good accuracy, it is highly recommended to carry out an accompanying FEM modeling of the temperature distribution. The combination of experiment and modeling is the basis for reliably designing the tools and achieving high reproducibility of the FAST/SPS cycles. Another possibility for estimating the temperature distribution is the use of a "dummy" tool without powder cavity, which is equipped with thermocouples in as many places as possible. It should also be noted that the temperature gradients increase with tool size. In industrial production, temperature gradients of up to 80 K can occur in multi-component tools (up to 500 components per cycle), especially at the beginning of the cycle. When supporting tool design by FEM modeling, temperature deviations can be reduced to below 20 K.

== Applications of FAST/SPS ==

== Alternative operation modes of FAST/SPS devices ==

Field assisted sintering technology/spark plasma sintering

2021-08-05T06:54:30Z

M.bram: /* Measurement of temperature */

== General principle of FAST/SPS ==
Field Assisted Sintering Technology/Spark Plasma Sintering (FAST/SPS) is a low-voltage, current-activated and pressure-supported sintering process that is based on Joule heating (= resistance heating) of the conductive tools ('''Figure 1''') and is characterized by high heating rates and short cycle times. If electrically conductive powders are applied, the powder itself is also heated directly via the Joule effect. The FAST/SPS process is established in the industry and particularly promising when powders are to be sintered, which have a low sintering activity or an unfavorable particle morphology and particle size distribution for conventional pressing and sintering. Furthermore, the method is well suited for the production of composite materials, especially when phases will be combined, which have very different physical properties. Some typical application examples of FAST/SPS technology are presented in Chapter 7. Due to the great flexibility, the short cycle times and the comparatively simple and cost-effective production of tools, research and development is another important field of application for FAST/SPS technology and is widespread there.

[[File:Wiki Keramik FAST SPS Abb 01.jpg|thumb|center]]
'''Figure 1:''' ''Heated graphite tool in a FAST / SPS device.''

In principle, a FAST/SPS device is a mechanical press, which at the same time also forms a high-energy current circuit. The FAST/SPS process is carried out in a conductive tool consisting of two punches and a die. Two additional cones establish the contact with the device's electrodes. The pressing force is also applied via these electrodes by means of a hydraulic pressure cylinder. '''Figure 2''' shows a schematic sketch of such a device. FAST/SPS processes are usually carried out in a vacuum or protective gas to protect the tool and the powder inside the tool from oxidation. Accordingly, the pressing device is located in a water-cooled chamber, in which a moderate vacuum (0.5 - 20 mbar) or a defined protective gas atmosphere (e.g. Ar or N2) can be set. The heating of the tool via the Joule effect requires the use of conductive materials for the punch and the die. The standard material for punch and die is graphite, alternatives to this are introduced in Chapter 4.

[[File:Wiki Keramik FAST SPS Abb 02 englisch.jpg|thumb|center]]
'''Figure 2:''' ''Schematic sketch of a FAST/SPS device.''

The tool is heated by a continuous or pulsed direct current with moderate voltages <10 V and high currents in the range from 1 to several 10 kA (depending on the size of the device). Non-conductive powders can also be sintered in good quality via FAST/SPS. Here, the direct contact between the tool and the powder leads to rapid heat transfer and relatively even heating over the entire cross-section of the sample. The heating takes place primarily via thermal conduction. In order to reduce the heat loss through thermal radiation, the die can optionally be thermally insulated, e.g. with a graphite felt. In the standard configuration, heating rates of up to approx. 300 K/min can be achieved in a FAST/SPS device. The high heating rates are one of the main reasons for the fast cycle times, as grain boundary and volume diffusion necessary for mass transport during sintering are activated directly. Due to the thermal mass of the tools, extremely high cooling rates cannot be achieved. Typical cooling rates are around 100 - 150 K/min. It should be noted here that the use of thermal insulation materials further reduces the cooling rates. In addition to the rapid heating, the sintering kinetics are also supported by the applied load. Depending on the type of system and sample size, compaction pressure in the range of 50 - 100 MPa can be achieved with the standard material graphite. Special grades of graphite allow maximum pressures of up to 200 MPa. When using graphite tools, temperatures of up to approx. 2,200 °C can be achieved in FAST/SPS devices. Alternative tools made of highly heat-resistant metals or electrically conductive ceramics enable pressures of up to 400 MPa, but the maximum permissible sintering temperatures are usually significantly lower in these cases. In order to improve the electrical contact between the punches, the die and the sample, a flexible, ideally electrically conductive foil is usually positioned between the punches and the sample. Graphite has also proven to be the standard material for this foil. FAST/SPS systems are usually controlled by programming the temperature-time curve. The measurement of the temperature as a major process parameter is carried out by axially or radially arranged pyrometers or by thermocouples. A direct measurement of the sample temperature is usually not possible. In order to measure the temperature as close as possible to the sample, holes are often drilled in the tools, at the bottom of which the temperature is measured. Furthermore, especially with increasing size of sintered parts and complexity of shape, it is recommended to predict the temperature distribution in the parts using suitable FEM modeling.

== Advantages and limitations of FAST/SPS ==
i.) '''Advantages:''' An essential feature of the FAST/SPS process is the rapid heating of the sample, which is based on the direct heating of the tool and the good heat transfer between the die and the powder. The superimposition of an uniaxial pressure during sintering further accelerates the sintering kinetics, so that the sintering temperature can often be significantly reduced compared to conventional sintering processes. Accordingly, the FAST/SPS process is a promising technology for

* '''Powder with low sintering activity:''' FAST/SPS enables the compaction of powders that have a low sintering activity (e.g. borides, carbides, nitrides and their mixtures).
* '''Powders with unfavorable powder properties:''' Powders can be sintered whose particle size distribution and morphology are unsuitable for conventional pressing and sintering.
* '''Nanoscale powders:''' The rapid processing in the case of FAST/SPS makes it possible to preserve the structure of nanoscale powders in the component.
* '''Materials with limited stability:''' FAST/SPS enables the sintering of materials that tend to decompose at high temperatures and long dwell times and to form undesirable secondary phases.
* '''Materials containing phases out of thermodynamic equilibrium:''' Phases out of thermodynamic equilibrium can be maintained in the sintered part (e.g. amorphous phases). Based on this, properties can be achieved that are not feasible with other sintering methods.
* '''Composite materials:''' FAST/SPS has great potential for sintering of composite materials that combine phases, which have large differences in their physical properties (e.g. very different melting points).
* '''Energy-efficient processing:''' In general, the FAST/SPS process is classified as an energy-efficient process due to the reduced sintering temperature and the short cycle times, but the degree of automation and the number of components per sintering cycle must also be taken carefully into account for an objective comparison with other sintering technologies.

ii.) '''Limitations:''' Despite the obvious advantages of FAST/SPS technology, there are also a number of process-related limitations.
* '''Risk of density and stress gradients in the component:''' If powders with a low thermal conductivity and high electrical resistance are sintered by FAST/SPS, there might arise an inhomogeneous temperature distribution in the component, which becomes more pronounced with increasing sample size. If exceeding a critical value, density and/or stress gradients in the sintered part result. There are also limitations with respect to the maximum height/diameter ratio. Similar to conventional pressing, wall friction can cause density gradients in the sintered part.
* '''Chemical and electrochemical interaction with the tool materials:''' The direct contact of the powder with the tools is advantageous with respect to heat transfer, but in the worst case it also leads to a chemical interaction with the tools or the inserted foils. When using graphite tools or foils, possible contamination of the component with carbon must be taken carefully into account. Therefore, adhering residues of the graphite foil and the reaction zone on the component surface must be removed mechanically, e.g. by grinding. In addition, it must be noted that the electrical field applied to the powder can trigger electrochemical reactions at the interfaces. A well-known effect is electrochemical blackening of oxide ceramics caused by the release of oxygen at low oxygen partial pressures. Furthermore, oxide ceramics that contain transition metals at the A or B position are sensitive to chemical expansion, which in the worst case leads to severe cracking in the component.
* '''Change of conductivity of semi-conductive and mixed-conductive materials:''' When sintering semi-conductive and mixed-conductive materials via FAST/SPS, it should be noted that the conductivity of the powder changes with increasing temperature and density during the FAST/SPS cycle. If the heating at the beginning of the sintering cycle is primarily based on heat conduction, this state might change suddenly if a current flow through the sample becomes possible when the temperature exceeds a specific value. The result is a complex sintering process that becomes difficult to control and which can impair reproducibility. This effect is used for specific kinds of field-assisted sintering, e.g. for flash sintering. For more details, see Chapter 8.
* '''Net-shaping:''' The FAST/SPS process reaches its limits when complex shapes are to be realized. In addition to the challenges of suitable tool design, increasing geometrical complexity might cause inhomogeneous temperature distribution and, in the case of conductive powders, inhomogeneous current flow over the entire sample cross-section. There are a number of approaches to manufacture complex shapes e.g. by using split tools or by sintering near net-shaped green parts in a powder bed directly via FAST/SPS. However, the possibilities for automating these technologies must be evaluated critical.
* '''Automation of the FAST/SPS process:''' At current state of development, cycle times in FAST/SPS systems cannot compete with conventional pressing and sintering, since a complete FAST/SPS cycle takes several minutes despite high heating rates and short dwell times. If insert foils are used to improve the electrical and thermal contact during tool assembly, this slows down the cycle time further. In order to operate FAST/SPS devices with higher productivity, partially automated, multiple tools (capacity up to several hundred components) are in use, which can optionally be filled with a robot system outside the device and then installed in the device via a manipulator. Another concept are FAST/SPS devices with a system of separate chambers in which the individual processing steps of tool assembly, powder filling, compression and cooling are carried out in a separate and sequential manner.

== How to conduct a standard FAST/SPS cycle ==
In this section, the processing steps for sintering a ceramic powder via FAST/SPS are explained in detail. For conducting FAST/SPS cycles, the following three devices are available at the institute IEK-1 ('''Figure 3''').

'''-> Figure 3''' 
'''Figure 3:''' ''FAST/SPS devices at the institute IEK-1 '''a.)''' Laboratory device HP-D 5 '''b.)''' Hybrid sintering system H-HP-D25 SD/FL/MoSi '''c.)''' Sintering press DSP515 on industrial scale.''

The '''HP-D 5 laboratory device''' is characterized by the following operating parameters:
* Type: HP-D 5
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 50 kN
* Maximum heating power: 37 kW
* Maximum sample diameter: 30 mm
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operating mode: FAST / SPS with pulsed direct current

The '''hybrid sintering device H-HP-D25 SD/FL/MoSi''' enables a number of different operating modes in addition to the conventional FAST/SPS mode through the optional application of additional heaters or operation with an external voltage source.
* Type: H-HP-D25 SD/FL/MoSi
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 250 kN
* Maximum sample diameter: 100 mm (FAST/SPS mode), 20 mm (Flash sintering mode)
* Maximum heating power (FAST / SPS): 60 kW
* Maximum heating power (Induction): 80 kW
* Maximum heating power (MoSi2): 10 kW
* Maximum heating power (Hybrid heating): 100 kW
* External voltage source: AC/DC, 1000 V, max. 25 A
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operation modes: i.) FAST / SPS with pulsed direct current ii.) Hybrid FAST/SPS with induction coil or MoSi2 furnace as additional heater iii.) Hot press with MoSi2 heater iv.) Flash SPS with defined heating power v.) Flash sintering with an external voltage source and MoSi2 heater.

The '''DSP515 sintering press''' is a device, which can be used for industrial production and enables the scaling up of promising results from experiments on lab-scale.
* Type: DSP515
* Manufacturer: Dr. Fritsch Sondermaschinen GmbH, Fellbach, Germany
* Maxiumum pressing force: 555 kN
* Electrode size: 180 x 180 mm2
* Maximum sample size: approx. 160 x 160 mm2
* Maximum heating power: 170 kW
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2
* Operating modes: i.) FAST/SPS with constant direct current ii.) Flash SPS with defined heating power.
* Debinding unit: The system is also equipped with a cooling trap for debinding of tape-cast parts.

Below, the steps of a standard FAST/SPS cycle using a graphite tool with a sample diameter of 20 mm are described. An additional graphite foil (thickness approx. 0.35 mm) is inserted into the graphite tool. The thickness of the foil must be taken into account when designing the tool. The inserted foil has two main functions. On the one hand, it improves the electrical and thermal contact between the punch and the die as well as between the powder, the face of the punch and the die. On the other hand, it avoids chemical interactions between powder and tool, so that the tool life is increased. The FAST/SPS cycle shown here was carried out in the HP-D 5 laboratory device.

i.) '''Sample preparation:''' '''Figure 4''' shows the parts of a lab-scale graphite tool (inner diameter 20 mm) as well as the graphite insert foils (thickness 0.35 mm), which are sized with respect to the tool dimensions. In a first step, the graphite foils are positioned on the inner wall of the die and on the faces of the punches. It is important that the foils has a tight contact to the tool components and that there are no kinks or gaps after positioning. For health protection, the graphite tool should be filled in a laboratory hood. Filling can be carried out on a balance. This increases the accuracy of the powder quantity weighed in.

'''-> Figure 4''' 
'''Figure 4:''' ''Preparation of the graphite tool and the insert foil for the FAST/SPS cycle. For accurate sample preparation, the powder should be directly balanced in the tool. Furthermore, it is recommended to handle the powder in a hood.''

After filling in the tool, the powder is covered with an additional graphite foil and pre-pressed in a manual laboratory press with 50 MPa (16 KN for diameter 20 mm tool) ('''Figure 5'''). In order to avoid sticking of powder particles on the face the upper punch, the upper punch is removed again and powder residues are manually removed. Afterwards, the upper punch is placed again in the tool.

'''-> Figure 5''' 
'''Figure 5:''' '''''a.)''' Filling the mold and positioning the graphite foil '''b.)''' Pre-pressing of the FAST/SPS sample in a manual hand press '''c.)''' Removal of the upper punch after the pressing process and removal of adhering powder particles.''

ii.) '''Mounting of the tool and programming the FAST/SPS device:''' At the laboratory system HP-D 5, the programming of the FAST/SPS parameters can be done via a process controller type Stange SE607 ('''Figure 6'''). The main operating parameters temperature, pressing force, pulse length of the current and moving speed of the lower electrode is programmed in individual program segments. During the FAST/SPS cycle, all process data are shown on the controller display as a numerical values and as a time-resolved graph. In parallel, all data are saved via a data logger integrated in the system. By default, the data are transferred to an external PC for data management and further evaluation. Individual parameter sets of the users are also stored on the PC and can be easily transferred to the controller if required.

'''-> Figure 6''' 
'''Figure 6:''' ''Display of the controller of the HP-D 5 device giving a compact overview of all process-relevant data.''

'''Figure 7''' shows the graphite tool mounted into the HP-D 5 devices as well as the CuBe electrodes. Optionally, the graphite tool can be thermally isolated with a jacket made of a graphite felt (not shown here). A graphite cord can be used to fix the graphite felt on the tool.

'''-> Figure 7''' 
'''Figure 7:''' ''View on the processing chamber of the HP-D 5 device with mounted graphite tool. When installing the tool and the two cones, it should be noted that graphite is a brittle and shock-sensitive material and therefore breaks very easily. For this reason, sudden contact of all graphite parts with the other system components (stamp, chamber walls) must be avoided.''

After the graphite tool has been inserted and fixed by lifting the lower punch, the container door is closed and the FAST/SPS cycle can be started.

iii.) '''Choice and regulation of the sintering atmosphere:''' A FAST/SPS cycle is usually carried out in vacuum or under protective gas atmosphere. Accordingly, the process chamber is evacuated by a vacuum pump at the beginning of the cycle. In the laboratory device HP-D 5, a vacuum of approx. 0.5 mbar is achieved; in larger systems, this value can also be higher (e.g. 20 mbar for the DSP515). The quality of the vacuum depends on the sealing of the process chamber and the power of the vacuum pump. If aiming on a high vacuum, cost of the FAST/SPS device significantly increases. After evacuation, the chamber can optionally be flooded with gases such as N2, Ar or Ar/H2 (static atmosphere control) or a continuous gas flow (dynamic atmosphere control). Figure 8 shows the valves for feeding the individual gases from the institute's gas store into the system. The evacuation of the process chamber and the optional supply of protective gases to the process chamber is regulated by the system control and takes place automated. The pressure in the process chamber is continuously recorded in the HP-D 5 device by two sensors with different measuring ranges (coarse sensor 1.0 - 1300 mbar, fine sensor 0.01 - 13 mbar), which are positioned at the gas outlet. For operation of the system under relative pressure (reduced pressure in relation to the ambient pressure), the system is also equipped with a relative pressure sensor, which enables to regulate the relative pressure in the range of 5 - 50 mbar. Static or dynamic operation is also possible in the relative pressure mode. A safety valve is used to protect the processing chamber against overpressure. The valve opens at an overpressure of 100 mbar above the ambient pressure. The pressure curve during the FAST/SPS cycle is recorded continuously. An analysis of the pressure curve can be helpful if components outgas from the sample or if the sample decomposes under the FAST/SPS conditions.

'''-> Figure 8''' 
'''Figure 8:''' ''Valves for flooding the processing chamber with the protective gases Ar, N2, Ar/H2.''

When sintering oxide ceramics via FAST/SPS, it should be noted that the sintering conditions have a reducing effect, i.e. there is a release oxygen atoms from the lattice, which increases with decreasing oxygen partial pressure. The effect is aggravated in the case of direct contact with the graphite tools or the graphite foils. The release of oxygen is visually noticeable in the darkening of the ceramic. This effect is superimposed by the uptake of carbon. If the release of oxygen exceeds a critical value, the sample can undergo chemical expansion, which can be up to several percent (as e.g. the case for gadolinium-doped cerium oxide or barium-strontium-cobalt oxides). Usually, this effect leads to severe cracking of the sample. Furthermore, the crystal lattice can become unstable if the oxygen release progresses further. In worst case, reduction of components down to the metallic phase might appear.

In principle, it is possible to operate a FAST/SPS device with technical air. Such operation must be done with special care, since most materials used for the tools are unstable in air and start to strongly oxidize if the temperature exceeds a critical value (usually around 400°C). It should also be noted that the powder in the tool is encapsulated in such a way that the access of oxygen to the powder is prevented to a large extent.

iv.) '''Performing of the FAST/SPS cycle:''' After the device has been prepared, the selected program is started and runs automatically. '''Figure 9''' shows the graphite die during the heating process. As already mentioned, the operation of FAST/SPS devices is usually temperature-controlled. This means that the controller defines the temperature and the system regulates the current and voltage in such a way that the temperature profile is adhered to the specification as precisely as possible. In order to keep the deviations from the programmed temperature curve as low as possible, the system is equipped with a PID control (PID = Proportional-Integral-Derivative). This control unit iteratively adapt the optimal current and voltage curves for heating the tool to the respective electrical resistance of the tool.

'''-> Figure 9''' 
'''Figure 9:''' ''View on the heated graphite tool (punch diameter 20 mm) in the laboratory device HP-D 5. When operating a FAST/SPS system, it should be noted that the high currents in the system cause strong electromagnetic fields, which can damage pacemakers and others sensitive electronic devices.''

== Tool design and tool materials ==
In most cases, graphite tools are used in FAST/SPS systems. '''Figure 10''' shows a selection of graphite tools for the laboratory system HP-D 5 with punch diameters of 12, 20 and 30 mm and for the hybrid sintering device H-HP-D25 with a punch diameter of 100 mm.

'''-> Figure 10'''
'''Figure 10:''' ''Graphite tools for performing FAST/SPS cycles '''a.)''' Overview: die, punch with hole for pyrometer, cone for adaptation to the geometry of the electrodes of the FAST/SPS device '''b.)''' Tools for the laboratory device HP-D 5 with a diameter of 12, 20 and 30 mm and '''c.)''' Tools for the hybrid sintering device H-HP-D25 with a diameter of 100 mm.''

The use of graphite has the advantage that it is easy to machine the tools. Furthermore, it has an electrical resistance that is favorable for Joule heating. Temperatures of up to around 2,200 °C can be achieved in graphite tools. The compressive strength of standard grades is approx. 50 - 100 MPa (e.g. Sigrafine R7710, SGL Carbon GmbH), special grades achieve compressive strengths of up to 230 MPa (e.g. Grade 2334, Mersen). It should be noted that the geometry of the tool also has an influence on the maximum permissible pressure, e.g. the notch effect of a hole drilled for temperature measurement can lead to failure of the tool even at low pressures. Above 450 °C, graphite tools can only be used in a vacuum or under protective gas (e.g. Ar). If a tool is used frequently, attention must also be paid to possible wear, which can reduce the dimensional accuracy of the sintered parts.

If pressures well above 100 MPa or long tool life are desired, the following materials can used as alternative to graphite. At temperatures up to 600 °C, the use of a high-speed steel (e.g. W360, Böhler) is recommended, which can resist pressures of up to 400 MPa. If higher temperatures are desired, Mo alloys (e.g. Ti-Zr-Mo TZM, Plansee) can be used, which enable maximum temperature of approx. 1100 ° C and maximum pressure of 350 MPa. The maximum operating temperature of metal tools is limited by the onset of creep processes and severe grain coarsening. Both effects can cause a macroscopic deformation of the tools, so that in the worst case the punch can become jammed in the die. '''Figure 11''' shows as an example tools made of W360 steel and TZM.

'''-> Figure 11'''
'''Figure 11:''' ''Metallic tools '''a.)''' Overview: Die, punch, and cone of a tool made of W360 steel '''b.)''' Same tool in the assembled state '''c.)''' Similar tool made of TZM.''

If even higher temperatures or pressures are desired, the literature reports on tools made of conductive ceramics. Suitable materials are tungsten carbide or silicon carbide, which are already used in the laboratory up to pressures of 1000 MPa. When using ceramic tools, the high effort in production and the inherent brittleness must be taken into account. Careful handling is strictly required in order to avoid breakage.

When using metallic and ceramic tools, it should be noted that these materials usually have a different electrical resistance than graphite. This has an influence on the system control and may require an adjustment of the PID parameters for precise temperature control (see Chapter 4).

== Measurement of temperature ==
The temperature is the main parameter for controlling the FAST/SPS system. The exact measurement and control of temperature is one of the great challenges when applying of FAST/SPS technology. The high heating rates require a temperature measurement with short response time, short delay time and high reproducibility. A direct measurement of the sample temperature is not possible with reasonable effort. Therefore, the measurement should be conducted as close to the sample as possible. For this purpose, vertical or horizontal holes are usually drilled in the FAST/SPS tool. By adjusting the pyrometer or thermocouple at the bottom of these holes, the temperature can be measured in direct vicinity of the sample.

i.) '''Measurement of the temperature with the pyrometer:''' Pyrometers are preferably used for temperature measurement at high temperatures. The usual measuring range of pyrometers is 600 - 3000 °C. '''Figure 12a''' shows the pyrometer installed in the HP-D 5 laboratory device. In this case, the measurement signal is deflected via a prism so that the measurement can be carried out vertically in a hole drilled in the upper punch.

In FAST / SPS systems with additional heater (e.g. hybrid sintering device H-HP-D 25), the pyrometer for controlling the additional heating is installed on the side. The measurement is carried out through a sight glass in the furnace door.

ii.) '''Measurement of the temperature with thermocouples:''' Thermocouples are necessarily required for a regulated temperature control of the system at temperatures < 600 °C, since pyrometers do not work reliably in this temperature range. There is also the option of using thermocouples at higher temperatures. Thermocouples of type K (Ni-CrNi) are suitable for the temperature range RT - 1100 ° C and are comparatively inexpensive. Because of the ductility of Ni, type K thermocouples are flexible. For protection, the thermocouples are enclosed in a steel jacket. Type C thermocouples (W5Re-W26Re) with a molybdenum housing enable temperature measurement in the range of RT - 2,200 ° C. The materials used are brittle and expensive, so that their application requires careful handling. Regardless of whether the housing is made of steel or molybdenum, care must be taken that there is no chemical interaction with the tool material during the sintering cycle. '''Figure 12b''' shows a graphite tool equipped with multiple type K thermocouples. One of the thermocouples is used for controlling the heating cycle by temperature measurement of the die and is flexibly installed. Two further thermocouples are firmly fixed to the upper and lower electrodes of the system and serve to protect the water-cooled CuBe electrodes from overheating.

'''-> Figure 12'''
'''Figure 12:''' ''Temperature measurement in the laboratory system HP-D 5 '''a.)''' Pyrometer for measuring the temperature of the upper punch, deflection of the measurement signal via a prism inside the device '''b.)''' Flexible thermocouples of type K. When installing the thermocouples, it must made sure that there is no contact between the thermocouple and the container wall in order to avoid short circuiting.''

In general, it should be noted that temperature differences of significantly more than 10 K can occur between the pyrometer and thermocouples when identical operating parameters are used. In order to be able to predict the temperature distribution in the component with good accuracy, it is highly recommended to carry out an accompanying FEM modeling of the temperature distribution. The combination of experiment and modeling is the basis for reliably designing the tools and achieving high reproducibility of the FAST/SPS cycles. Another possibility for estimating the temperature distribution is the use of a "dummy" tool without powder cavity, which is equipped with thermocouples in as many places as possible. It should also be noted that the temperature gradients increase with tool size. In industrial production, temperature gradients of up to 80 K can occur in multi-component tools (up to 500 components per cycle), especially at the beginning of the cycle. When supporting tool design by FEM modeling, temperature deviations can be reduced to below 20 K.

== Applications of FAST/SPS ==

== Alternative operation modes of FAST/SPS devices ==

Field assisted sintering technology/spark plasma sintering

2021-08-05T06:48:11Z

M.bram: /* Tool design and tool materials */

== General principle of FAST/SPS ==
Field Assisted Sintering Technology/Spark Plasma Sintering (FAST/SPS) is a low-voltage, current-activated and pressure-supported sintering process that is based on Joule heating (= resistance heating) of the conductive tools ('''Figure 1''') and is characterized by high heating rates and short cycle times. If electrically conductive powders are applied, the powder itself is also heated directly via the Joule effect. The FAST/SPS process is established in the industry and particularly promising when powders are to be sintered, which have a low sintering activity or an unfavorable particle morphology and particle size distribution for conventional pressing and sintering. Furthermore, the method is well suited for the production of composite materials, especially when phases will be combined, which have very different physical properties. Some typical application examples of FAST/SPS technology are presented in Chapter 7. Due to the great flexibility, the short cycle times and the comparatively simple and cost-effective production of tools, research and development is another important field of application for FAST/SPS technology and is widespread there.

[[File:Wiki Keramik FAST SPS Abb 01.jpg|thumb|center]]
'''Figure 1:''' ''Heated graphite tool in a FAST / SPS device.''

In principle, a FAST/SPS device is a mechanical press, which at the same time also forms a high-energy current circuit. The FAST/SPS process is carried out in a conductive tool consisting of two punches and a die. Two additional cones establish the contact with the device's electrodes. The pressing force is also applied via these electrodes by means of a hydraulic pressure cylinder. '''Figure 2''' shows a schematic sketch of such a device. FAST/SPS processes are usually carried out in a vacuum or protective gas to protect the tool and the powder inside the tool from oxidation. Accordingly, the pressing device is located in a water-cooled chamber, in which a moderate vacuum (0.5 - 20 mbar) or a defined protective gas atmosphere (e.g. Ar or N2) can be set. The heating of the tool via the Joule effect requires the use of conductive materials for the punch and the die. The standard material for punch and die is graphite, alternatives to this are introduced in Chapter 4.

[[File:Wiki Keramik FAST SPS Abb 02 englisch.jpg|thumb|center]]
'''Figure 2:''' ''Schematic sketch of a FAST/SPS device.''

The tool is heated by a continuous or pulsed direct current with moderate voltages <10 V and high currents in the range from 1 to several 10 kA (depending on the size of the device). Non-conductive powders can also be sintered in good quality via FAST/SPS. Here, the direct contact between the tool and the powder leads to rapid heat transfer and relatively even heating over the entire cross-section of the sample. The heating takes place primarily via thermal conduction. In order to reduce the heat loss through thermal radiation, the die can optionally be thermally insulated, e.g. with a graphite felt. In the standard configuration, heating rates of up to approx. 300 K/min can be achieved in a FAST/SPS device. The high heating rates are one of the main reasons for the fast cycle times, as grain boundary and volume diffusion necessary for mass transport during sintering are activated directly. Due to the thermal mass of the tools, extremely high cooling rates cannot be achieved. Typical cooling rates are around 100 - 150 K/min. It should be noted here that the use of thermal insulation materials further reduces the cooling rates. In addition to the rapid heating, the sintering kinetics are also supported by the applied load. Depending on the type of system and sample size, compaction pressure in the range of 50 - 100 MPa can be achieved with the standard material graphite. Special grades of graphite allow maximum pressures of up to 200 MPa. When using graphite tools, temperatures of up to approx. 2,200 °C can be achieved in FAST/SPS devices. Alternative tools made of highly heat-resistant metals or electrically conductive ceramics enable pressures of up to 400 MPa, but the maximum permissible sintering temperatures are usually significantly lower in these cases. In order to improve the electrical contact between the punches, the die and the sample, a flexible, ideally electrically conductive foil is usually positioned between the punches and the sample. Graphite has also proven to be the standard material for this foil. FAST/SPS systems are usually controlled by programming the temperature-time curve. The measurement of the temperature as a major process parameter is carried out by axially or radially arranged pyrometers or by thermocouples. A direct measurement of the sample temperature is usually not possible. In order to measure the temperature as close as possible to the sample, holes are often drilled in the tools, at the bottom of which the temperature is measured. Furthermore, especially with increasing size of sintered parts and complexity of shape, it is recommended to predict the temperature distribution in the parts using suitable FEM modeling.

== Advantages and limitations of FAST/SPS ==
i.) '''Advantages:''' An essential feature of the FAST/SPS process is the rapid heating of the sample, which is based on the direct heating of the tool and the good heat transfer between the die and the powder. The superimposition of an uniaxial pressure during sintering further accelerates the sintering kinetics, so that the sintering temperature can often be significantly reduced compared to conventional sintering processes. Accordingly, the FAST/SPS process is a promising technology for

* '''Powder with low sintering activity:''' FAST/SPS enables the compaction of powders that have a low sintering activity (e.g. borides, carbides, nitrides and their mixtures).
* '''Powders with unfavorable powder properties:''' Powders can be sintered whose particle size distribution and morphology are unsuitable for conventional pressing and sintering.
* '''Nanoscale powders:''' The rapid processing in the case of FAST/SPS makes it possible to preserve the structure of nanoscale powders in the component.
* '''Materials with limited stability:''' FAST/SPS enables the sintering of materials that tend to decompose at high temperatures and long dwell times and to form undesirable secondary phases.
* '''Materials containing phases out of thermodynamic equilibrium:''' Phases out of thermodynamic equilibrium can be maintained in the sintered part (e.g. amorphous phases). Based on this, properties can be achieved that are not feasible with other sintering methods.
* '''Composite materials:''' FAST/SPS has great potential for sintering of composite materials that combine phases, which have large differences in their physical properties (e.g. very different melting points).
* '''Energy-efficient processing:''' In general, the FAST/SPS process is classified as an energy-efficient process due to the reduced sintering temperature and the short cycle times, but the degree of automation and the number of components per sintering cycle must also be taken carefully into account for an objective comparison with other sintering technologies.

ii.) '''Limitations:''' Despite the obvious advantages of FAST/SPS technology, there are also a number of process-related limitations.
* '''Risk of density and stress gradients in the component:''' If powders with a low thermal conductivity and high electrical resistance are sintered by FAST/SPS, there might arise an inhomogeneous temperature distribution in the component, which becomes more pronounced with increasing sample size. If exceeding a critical value, density and/or stress gradients in the sintered part result. There are also limitations with respect to the maximum height/diameter ratio. Similar to conventional pressing, wall friction can cause density gradients in the sintered part.
* '''Chemical and electrochemical interaction with the tool materials:''' The direct contact of the powder with the tools is advantageous with respect to heat transfer, but in the worst case it also leads to a chemical interaction with the tools or the inserted foils. When using graphite tools or foils, possible contamination of the component with carbon must be taken carefully into account. Therefore, adhering residues of the graphite foil and the reaction zone on the component surface must be removed mechanically, e.g. by grinding. In addition, it must be noted that the electrical field applied to the powder can trigger electrochemical reactions at the interfaces. A well-known effect is electrochemical blackening of oxide ceramics caused by the release of oxygen at low oxygen partial pressures. Furthermore, oxide ceramics that contain transition metals at the A or B position are sensitive to chemical expansion, which in the worst case leads to severe cracking in the component.
* '''Change of conductivity of semi-conductive and mixed-conductive materials:''' When sintering semi-conductive and mixed-conductive materials via FAST/SPS, it should be noted that the conductivity of the powder changes with increasing temperature and density during the FAST/SPS cycle. If the heating at the beginning of the sintering cycle is primarily based on heat conduction, this state might change suddenly if a current flow through the sample becomes possible when the temperature exceeds a specific value. The result is a complex sintering process that becomes difficult to control and which can impair reproducibility. This effect is used for specific kinds of field-assisted sintering, e.g. for flash sintering. For more details, see Chapter 8.
* '''Net-shaping:''' The FAST/SPS process reaches its limits when complex shapes are to be realized. In addition to the challenges of suitable tool design, increasing geometrical complexity might cause inhomogeneous temperature distribution and, in the case of conductive powders, inhomogeneous current flow over the entire sample cross-section. There are a number of approaches to manufacture complex shapes e.g. by using split tools or by sintering near net-shaped green parts in a powder bed directly via FAST/SPS. However, the possibilities for automating these technologies must be evaluated critical.
* '''Automation of the FAST/SPS process:''' At current state of development, cycle times in FAST/SPS systems cannot compete with conventional pressing and sintering, since a complete FAST/SPS cycle takes several minutes despite high heating rates and short dwell times. If insert foils are used to improve the electrical and thermal contact during tool assembly, this slows down the cycle time further. In order to operate FAST/SPS devices with higher productivity, partially automated, multiple tools (capacity up to several hundred components) are in use, which can optionally be filled with a robot system outside the device and then installed in the device via a manipulator. Another concept are FAST/SPS devices with a system of separate chambers in which the individual processing steps of tool assembly, powder filling, compression and cooling are carried out in a separate and sequential manner.

== How to conduct a standard FAST/SPS cycle ==
In this section, the processing steps for sintering a ceramic powder via FAST/SPS are explained in detail. For conducting FAST/SPS cycles, the following three devices are available at the institute IEK-1 ('''Figure 3''').

'''-> Figure 3''' 
'''Figure 3:''' ''FAST/SPS devices at the institute IEK-1 '''a.)''' Laboratory device HP-D 5 '''b.)''' Hybrid sintering system H-HP-D25 SD/FL/MoSi '''c.)''' Sintering press DSP515 on industrial scale.''

The '''HP-D 5 laboratory device''' is characterized by the following operating parameters:
* Type: HP-D 5
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 50 kN
* Maximum heating power: 37 kW
* Maximum sample diameter: 30 mm
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operating mode: FAST / SPS with pulsed direct current

The '''hybrid sintering device H-HP-D25 SD/FL/MoSi''' enables a number of different operating modes in addition to the conventional FAST/SPS mode through the optional application of additional heaters or operation with an external voltage source.
* Type: H-HP-D25 SD/FL/MoSi
* Manufacturer: FCT Systeme GmbH, Rauenstein, Germany
* Maximum pressing force: 250 kN
* Maximum sample diameter: 100 mm (FAST/SPS mode), 20 mm (Flash sintering mode)
* Maximum heating power (FAST / SPS): 60 kW
* Maximum heating power (Induction): 80 kW
* Maximum heating power (MoSi2): 10 kW
* Maximum heating power (Hybrid heating): 100 kW
* External voltage source: AC/DC, 1000 V, max. 25 A
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2, air
* Operation modes: i.) FAST / SPS with pulsed direct current ii.) Hybrid FAST/SPS with induction coil or MoSi2 furnace as additional heater iii.) Hot press with MoSi2 heater iv.) Flash SPS with defined heating power v.) Flash sintering with an external voltage source and MoSi2 heater.

The '''DSP515 sintering press''' is a device, which can be used for industrial production and enables the scaling up of promising results from experiments on lab-scale.
* Type: DSP515
* Manufacturer: Dr. Fritsch Sondermaschinen GmbH, Fellbach, Germany
* Maxiumum pressing force: 555 kN
* Electrode size: 180 x 180 mm2
* Maximum sample size: approx. 160 x 160 mm2
* Maximum heating power: 170 kW
* Possible sintering atmospheres: Vacuum, Ar, Ar / H2, N2
* Operating modes: i.) FAST/SPS with constant direct current ii.) Flash SPS with defined heating power.
* Debinding unit: The system is also equipped with a cooling trap for debinding of tape-cast parts.

Below, the steps of a standard FAST/SPS cycle using a graphite tool with a sample diameter of 20 mm are described. An additional graphite foil (thickness approx. 0.35 mm) is inserted into the graphite tool. The thickness of the foil must be taken into account when designing the tool. The inserted foil has two main functions. On the one hand, it improves the electrical and thermal contact between the punch and the die as well as between the powder, the face of the punch and the die. On the other hand, it avoids chemical interactions between powder and tool, so that the tool life is increased. The FAST/SPS cycle shown here was carried out in the HP-D 5 laboratory device.

i.) '''Sample preparation:''' '''Figure 4''' shows the parts of a lab-scale graphite tool (inner diameter 20 mm) as well as the graphite insert foils (thickness 0.35 mm), which are sized with respect to the tool dimensions. In a first step, the graphite foils are positioned on the inner wall of the die and on the faces of the punches. It is important that the foils has a tight contact to the tool components and that there are no kinks or gaps after positioning. For health protection, the graphite tool should be filled in a laboratory hood. Filling can be carried out on a balance. This increases the accuracy of the powder quantity weighed in.

'''-> Figure 4''' 
'''Figure 4:''' ''Preparation of the graphite tool and the insert foil for the FAST/SPS cycle. For accurate sample preparation, the powder should be directly balanced in the tool. Furthermore, it is recommended to handle the powder in a hood.''

After filling in the tool, the powder is covered with an additional graphite foil and pre-pressed in a manual laboratory press with 50 MPa (16 KN for diameter 20 mm tool) ('''Figure 5'''). In order to avoid sticking of powder particles on the face the upper punch, the upper punch is removed again and powder residues are manually removed. Afterwards, the upper punch is placed again in the tool.

'''-> Figure 5''' 
'''Figure 5:''' '''''a.)''' Filling the mold and positioning the graphite foil '''b.)''' Pre-pressing of the FAST/SPS sample in a manual hand press '''c.)''' Removal of the upper punch after the pressing process and removal of adhering powder particles.''

ii.) '''Mounting of the tool and programming the FAST/SPS device:''' At the laboratory system HP-D 5, the programming of the FAST/SPS parameters can be done via a process controller type Stange SE607 ('''Figure 6'''). The main operating parameters temperature, pressing force, pulse length of the current and moving speed of the lower electrode is programmed in individual program segments. During the FAST/SPS cycle, all process data are shown on the controller display as a numerical values and as a time-resolved graph. In parallel, all data are saved via a data logger integrated in the system. By default, the data are transferred to an external PC for data management and further evaluation. Individual parameter sets of the users are also stored on the PC and can be easily transferred to the controller if required.

'''-> Figure 6''' 
'''Figure 6:''' ''Display of the controller of the HP-D 5 device giving a compact overview of all process-relevant data.''

'''Figure 7''' shows the graphite tool mounted into the HP-D 5 devices as well as the CuBe electrodes. Optionally, the graphite tool can be thermally isolated with a jacket made of a graphite felt (not shown here). A graphite cord can be used to fix the graphite felt on the tool.

'''-> Figure 7''' 
'''Figure 7:''' ''View on the processing chamber of the HP-D 5 device with mounted graphite tool. When installing the tool and the two cones, it should be noted that graphite is a brittle and shock-sensitive material and therefore breaks very easily. For this reason, sudden contact of all graphite parts with the other system components (stamp, chamber walls) must be avoided.''

After the graphite tool has been inserted and fixed by lifting the lower punch, the container door is closed and the FAST/SPS cycle can be started.

iii.) '''Choice and regulation of the sintering atmosphere:''' A FAST/SPS cycle is usually carried out in vacuum or under protective gas atmosphere. Accordingly, the process chamber is evacuated by a vacuum pump at the beginning of the cycle. In the laboratory device HP-D 5, a vacuum of approx. 0.5 mbar is achieved; in larger systems, this value can also be higher (e.g. 20 mbar for the DSP515). The quality of the vacuum depends on the sealing of the process chamber and the power of the vacuum pump. If aiming on a high vacuum, cost of the FAST/SPS device significantly increases. After evacuation, the chamber can optionally be flooded with gases such as N2, Ar or Ar/H2 (static atmosphere control) or a continuous gas flow (dynamic atmosphere control). Figure 8 shows the valves for feeding the individual gases from the institute's gas store into the system. The evacuation of the process chamber and the optional supply of protective gases to the process chamber is regulated by the system control and takes place automated. The pressure in the process chamber is continuously recorded in the HP-D 5 device by two sensors with different measuring ranges (coarse sensor 1.0 - 1300 mbar, fine sensor 0.01 - 13 mbar), which are positioned at the gas outlet. For operation of the system under relative pressure (reduced pressure in relation to the ambient pressure), the system is also equipped with a relative pressure sensor, which enables to regulate the relative pressure in the range of 5 - 50 mbar. Static or dynamic operation is also possible in the relative pressure mode. A safety valve is used to protect the processing chamber against overpressure. The valve opens at an overpressure of 100 mbar above the ambient pressure. The pressure curve during the FAST/SPS cycle is recorded continuously. An analysis of the pressure curve can be helpful if components outgas from the sample or if the sample decomposes under the FAST/SPS conditions.

'''-> Figure 8''' 
'''Figure 8:''' ''Valves for flooding the processing chamber with the protective gases Ar, N2, Ar/H2.''

When sintering oxide ceramics via FAST/SPS, it should be noted that the sintering conditions have a reducing effect, i.e. there is a release oxygen atoms from the lattice, which increases with decreasing oxygen partial pressure. The effect is aggravated in the case of direct contact with the graphite tools or the graphite foils. The release of oxygen is visually noticeable in the darkening of the ceramic. This effect is superimposed by the uptake of carbon. If the release of oxygen exceeds a critical value, the sample can undergo chemical expansion, which can be up to several percent (as e.g. the case for gadolinium-doped cerium oxide or barium-strontium-cobalt oxides). Usually, this effect leads to severe cracking of the sample. Furthermore, the crystal lattice can become unstable if the oxygen release progresses further. In worst case, reduction of components down to the metallic phase might appear.

In principle, it is possible to operate a FAST/SPS device with technical air. Such operation must be done with special care, since most materials used for the tools are unstable in air and start to strongly oxidize if the temperature exceeds a critical value (usually around 400°C). It should also be noted that the powder in the tool is encapsulated in such a way that the access of oxygen to the powder is prevented to a large extent.

iv.) '''Performing of the FAST/SPS cycle:''' After the device has been prepared, the selected program is started and runs automatically. '''Figure 9''' shows the graphite die during the heating process. As already mentioned, the operation of FAST/SPS devices is usually temperature-controlled. This means that the controller defines the temperature and the system regulates the current and voltage in such a way that the temperature profile is adhered to the specification as precisely as possible. In order to keep the deviations from the programmed temperature curve as low as possible, the system is equipped with a PID control (PID = Proportional-Integral-Derivative). This control unit iteratively adapt the optimal current and voltage curves for heating the tool to the respective electrical resistance of the tool.

'''-> Figure 9''' 
'''Figure 9:''' ''View on the heated graphite tool (punch diameter 20 mm) in the laboratory device HP-D 5. When operating a FAST/SPS system, it should be noted that the high currents in the system cause strong electromagnetic fields, which can damage pacemakers and others sensitive electronic devices.''

== Tool design and tool materials ==
In most cases, graphite tools are used in FAST/SPS systems. '''Figure 10''' shows a selection of graphite tools for the laboratory system HP-D 5 with punch diameters of 12, 20 and 30 mm and for the hybrid sintering device H-HP-D25 with a punch diameter of 100 mm.

'''-> Figure 10'''
'''Figure 10:''' ''Graphite tools for performing FAST/SPS cycles '''a.)''' Overview: die, punch with hole for pyrometer, cone for adaptation to the geometry of the electrodes of the FAST/SPS device '''b.)''' Tools for the laboratory device HP-D 5 with a diameter of 12, 20 and 30 mm and '''c.)''' Tools for the hybrid sintering device H-HP-D25 with a diameter of 100 mm.''

The use of graphite has the advantage that it is easy to machine the tools. Furthermore, it has an electrical resistance that is favorable for Joule heating. Temperatures of up to around 2,200 °C can be achieved in graphite tools. The compressive strength of standard grades is approx. 50 - 100 MPa (e.g. Sigrafine R7710, SGL Carbon GmbH), special grades achieve compressive strengths of up to 230 MPa (e.g. Grade 2334, Mersen). It should be noted that the geometry of the tool also has an influence on the maximum permissible pressure, e.g. the notch effect of a hole drilled for temperature measurement can lead to failure of the tool even at low pressures. Above 450 °C, graphite tools can only be used in a vacuum or under protective gas (e.g. Ar). If a tool is used frequently, attention must also be paid to possible wear, which can reduce the dimensional accuracy of the sintered parts.

If pressures well above 100 MPa or long tool life are desired, the following materials can used as alternative to graphite. At temperatures up to 600 °C, the use of a high-speed steel (e.g. W360, Böhler) is recommended, which can resist pressures of up to 400 MPa. If higher temperatures are desired, Mo alloys (e.g. Ti-Zr-Mo TZM, Plansee) can be used, which enable maximum temperature of approx. 1100 ° C and maximum pressure of 350 MPa. The maximum operating temperature of metal tools is limited by the onset of creep processes and severe grain coarsening. Both effects can cause a macroscopic deformation of the tools, so that in the worst case the punch can become jammed in the die. '''Figure 11''' shows as an example tools made of W360 steel and TZM.

'''-> Figure 11'''
'''Figure 11:''' ''Metallic tools '''a.)''' Overview: Die, punch, and cone of a tool made of W360 steel '''b.)''' Same tool in the assembled state '''c.)''' Similar tool made of TZM.''

If even higher temperatures or pressures are desired, the literature reports on tools made of conductive ceramics. Suitable materials are tungsten carbide or silicon carbide, which are already used in the laboratory up to pressures of 1000 MPa. When using ceramic tools, the high effort in production and the inherent brittleness must be taken into account. Careful handling is strictly required in order to avoid breakage.

When using metallic and ceramic tools, it should be noted that these materials usually have a different electrical resistance than graphite. This has an influence on the system control and may require an adjustment of the PID parameters for precise temperature control (see Chapter 4).

== Measurement of temperature ==

== Applications of FAST/SPS ==

== Alternative operation modes of FAST/SPS devices ==

Field assisted sintering technology/spark plasma sintering

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M.bram: /* General principle of FAST/SPS */

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M.bram: /* How to conduct a standard FAST/SPS cycle */

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M.bram: /* How to conduct a standard FAST/SPS cycle */

File:Wiki Keramik FAST SPS Abb 03 new.png

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Figure 3: FAST/SPS devices at the institute IEK-1 a.) Laboratory device HP-D 5 b.) Hybrid sintering system H-HP-D25 SD/FL/MoSi c.) Sintering press DSP515 on industrial scale.

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M.bram: /* How to conduct a standard FAST/SPS cycle */

File:Wiki Keramik FAST SPS Abb 04 new.jpg

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Figure 4: Preparation of the graphite tool and the insert foil for the FAST/SPS cycle. For accurate sample preparation, the powder should be directly balanced in the tool. Furthermore, it is recommended to handle the powder in a hood.

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M.bram: /* How to conduct a standard FAST/SPS cycle */

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M.bram: /* How to conduct a standard FAST/SPS cycle */

File:Wiki Keramik FAST SPS Abb 03.jpg

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Figure 3: FAST/SPS devices at the institute IEK-1 a.) Laboratory device HP-D 5 b.) Hybrid sintering system H-HP-D25 SD/FL/MoSi c.) Sintering press DSP515 on industrial scale.

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M.bram: /* Advantages and limitations of FAST/SPS */

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M.bram: /* General principle of FAST/SPS */

File:Wiki Keramik FAST SPS Abb 02 englisch.jpg

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Figure 2: Schematic sketch of a FAST/SPS device.

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File:Wiki Keramik FAST SPS Abb 01.jpg

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Figure 1: Heated graphite tool in a FAST / SPS device.

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M.bram: /* General principle of FAST/SPS */

Field assisted sintering technology/spark plasma sintering

2021-08-04T11:52:20Z

M.bram: Created page with "== General principle of FAST/SPS == == Advantages and limitations of FAST/SPS == == How to conduct a standard FAST/SPS cycle == == Tool design and tool materials == == Mea..."

== General principle of FAST/SPS ==

== Advantages and limitations of FAST/SPS ==

== How to conduct a standard FAST/SPS cycle ==

== Tool design and tool materials ==

== Measurement of temperature ==

== Applications of FAST/SPS ==

== Alternative operation modes of FAST/SPS devices ==

Cold isostatic pressing

2021-08-04T11:45:43Z

M.bram: /* General principle of cold isostatic pressing (CIP) */

== General principle of cold isostatic pressing (CIP) ==

The cold isostatic pressing (CIP) is based on the effect that a pressure applied to a liquid spreads evenly in all directions (so-called Pascal's principle). Inside the liquid, this leads to a homogeneous pressure distribution, which can be used for shaping ceramic and metallic powders if the powder is encapsulated in an elastic die. Elastic polymers (elastomers) such as polyurethane (PU), polyvinyl chloride (PVC), synthetic or natural rubber have proven successful as materials for the elastic die. The main components of a cold isostatic press are the recipient filled with the pressure transmission medium, the high-pressure pump, the locking system, the overpressure protection and the system control. The recipient is a pressure cylinder, which consists of either a high-strength, thick-walled steel cylinder or a thin-walled steel vessel with a pre-tensioned wire winding. '''Figure 1''' shows a cold isostatic press in lab scale.

The pressure transmission media used are preferably water with the addition of an anti-corrosion agent, oil-water emulsions or glycerine. A hydraulic unit like an axial piston pump is used to build up pressure. This unit is connected to the recipient via a fluid transport system with appropriate valves and throttles. The pressure cylinder is sealed, for example, by a polymer O-ring that is integrated into the cover plate and is pressed into a groove when the pressure is built up. In order to absorb the large forces in the axial direction, the cover plate of the recipient is usually supported by a massive yoke. A rupture disc is used to protect against overpressure, which fails when the critical pressure is exceeded and thus enables a regulated pressure release before irreversible damage to the recipient occurs. Cold isostatic pressing is carried out in most cases at room temperature. In specially designed presses, moderate heating of the pressure medium up to a maximum temperature of 300 °C is possible.

In technical practice, a distinction is made between two basic principles of cold isostatic pressing, the wet bag process and the dry bag process. In addition, the wet bag process can also be used for the post-compaction of components uniaxial pre-pressed in a rigid form. The three variants are explained in more detail below:

i.) '''Wet bag process:''' In the wet bag process, the die is a self-supporting, elastic hollow mold that is filled with the powder outside the cold isostatic press. Optionally, a metallic mandrel can be integrated into the hollow mold for the production of pipes. After filling, the die is closed with an elastic cover plate. In order to protect the interior of the die against the ingress of liquid, the die can also be enveloped with an elastic foil, which is then evacuated and sealed in a liquid-tight manner. The wet bag process is often used in research and development due to its great flexibility with regard to the system parameters (including pressures up to approx. 400 MPa), the component geometries and the number of components per cycle. It is also used in industry for the production of large-volume components (e.g. filter candles) and semi-finished products (e.g. for manufacturing of ceramic insulators) with dimensions up to the meter range. Disadvantages of the wet bag process are the limited dimensional accuracy due to the elastic die and the comparatively long cycle times of several minutes.

ii.) '''Dry bag process:''' In dry bag pressing, the elastic die is firmly fixed to the recipient. Correspondingly, the mold filling takes place inside the cold isostatic press. The main advantages compared to wet bag pressing are the possibility of full automation, fast cycle times in the range of 10 s - 100 s depending on the component size (increase in cycle time with component size) and better dimensional accuracy. However, it should be noted that in the area of fixing the elastic die to the recipient there are restrictions with regard to the homogeneity of the pressure distribution, which, however, are less relevant for simpler geometries such as plates, cylinders or tubes. Dry die pressing is preferred in industrial production. The best-known application example are spark plug insulators, which are manufactured in a fully automated manner in quantities of millions.

iii.) '''Post-compaction of uniaxially pressed components:''' The shaping of ceramic and metallic powders via the uniaxial pressing in rigid molds is restricted by the wall friction, which leads to increasing density gradients in the component with increasing height/diameter ratio. The result is an inhomogeneous shrinkage during the subsequent sintering. In order to use the advantages of uniaxial pressing in terms of dimensional accuracy and at the same time to achieve a homogeneous density distribution in the component, it is possible to pre-press components uniaxially in a rigid die at moderate pressures, e.g. in the range of 50 - 100 MPa, and then post-compact them using cold isostatic pressing, which can be done e.g. at pressures in the range of 300 - 400 MPa. For the pressure transfer, the component must be liquid-tight welded into an elastic foil. When welding the foil, it must made sure that the foil is not damaged by sharp edges or particles.

[[File:Wiki Keramik KIP Abb 01.jpg|thumb|center]]
'''Figure 1:''' ''Cold isostatic press on a laboratory scale operated at the institute IEK-1, Forschungszentrum Jülich (manufacturer EPSI, type CIP 400-125 * 300Y). Usable volume: Diameter 125 mm, height = 300 mm.'' 

== Advantages and limitations of cold isostatic pressing ==

i.) '''Advantages:''' The main advantage of cold isostatic pressing is the elimination of friction-related variation in density, such as occurring in the case of uniaxial pressing in rigid molds. Therefore, higher green densities, higher green strengths and more homogeneous structures can be achieved with cold isostatic pressing. For example, press-related textures in the structure can be avoided to a large extent. Furthermore, components with a height / diameter ratio greater than 3: 1 (usually specified as limit for uniaxial pressing) can be produced relatively easily. Because there is no wall friction, it is possible to omit dispense with lubricants during pressing and the required proportion of other pressing additives can be significantly reduced. Furthermore, ceramic feedstocks can be compacted that contain abrasive solid particles that would lead to high tool wear in the case of uniaxial pressing.

ii.) '''Limits:''' Cold isostatic pressing is only suitable for relatively simple component geometries and is therefore restricted with respect to near-net-shape production. Due to the elastic properties of the die, there are limitations with regard to dimensional accuracy even with simpler geometries. Furthermore, the surface roughness is usually also relatively high, since the die wall yields elastically during pressing. Furthermore, sharp-edged particles can be pressed into the die wall, whereby the die is damaged in the worst case and demolding is aggravated. In order to increase the dimensional accuracy, mechanical post-processing of the cold isostatically pressed semi-finished products (so-called green machining) is often carried out. The relatively high green strength of cold isostatically pressed semi-finished products has a positive effect here.

== How to conduct a cold isostatic pressing cycle ==

In the following, it is explained in detail which processing steps are carried out in cold isostatic pressing and what must be considered in order to obtain crack-free samples and avoid damage to the system. The processing steps shown were carried out in a cold isostatic laboratory press of the following type:

Type: CIP 400-125*300Y 
Manufacturer: EPSI, Temse, Belgium 
Material of recipient: SA 723 Class 3 
Recipient inner diameter: 125 mm 
Recipient inner height: 300 mm 
Maximum sample size: Limited by recipient volume 
Maximum filling height: 295 mm 
Recipient volume: 3.7 Liter 
Nominal operating pressure: 4000 bar (400 MPa) 
Maximum operating pressure: 4400 bar (440 MPa) 
Safety factor: 1,1 (related to 4840 bar, 484 MPa) 

i.) '''Encapsulation of the samples:''' Even with cold isostatic pressing, a uniform filling of the mold and a high filling density are basic requirements for successful compaction of the powder. In order to estimate the flowability of the powder, it is recommended to measure the bulk and tap density in accordance with DIN ISO 3923 and DIN ISO 3953. The flowability of a powder can be improved by granulating in a fluidizing bed or by spray drying. During granulation, spherical, easily flowable agglomerates are formed, which have a relatively low stability and are destroyed during the cold isostatic pressing. Some powder manufacturers offer powder directly in a granulated state. In order to increase the bulk density in the mold, the elastic die can optionally be vibrated or subjected to ultrasonic treatment. As an example, '''Figure 2''' shows a simple elastic mold made of rubber for cold isostatic pressing of round bars.

[[File:Wiki Keramik KIP Abb 02.jpg|thumb|center]]
'''Figure 2:''' ''Elastic mold (rubber tube with cover plug) for cold isostatic pressing of round bars.
'' 

As mentioned above, there is also the possibility of post-compaction of uniaxially pressed semi-finished parts using cold isostatic pressing. '''Figure 3''' shows how the welding of a pre-pressed part into an elastic foil can be carried out. For this purpose, at the IEK-1 institute, a vacuum sealer is used, which is usually applied in the household for sealing and freezing food. Elastic foils, which are established for this purpose, are suitable for encapsulation of pre-pressed parts in cold isostatic pressing as well. The sample is placed in the prepared bag, then interior is evacuated and the bag is finally liquid-tight welded. A more primitive alternative is to put the sample in a latex glove, which is evacuated, for example, by a water jet pump and sealed with a string.

[[File:Wiki Keramik KIP Abb 03.jpg|thumb|center]]
'''Figure 3:''' ''Sealing of a uniaxially pre-pressed sample in an elastic foil using a household vacuum sealer a.) Insertion of the uniaxially pre-pressed sample b.) Evacuation c.) Liquid-tight sealed sample.''

ii.) '''Opening the recipient:''' '''Figure 4''' shows the individual steps for opening the recipient of the cold isostatic press of the type CIP 400-125 * 300Y (EPSI, Belgium). The press is equipped with a hydraulic lifting device. A screw is attached to this, via which the cover plate is connected to the hydraulic lifting device. The screw is protected from damage by a cage. After the screw has been attached, the cover is lifted using the lifting device. The sealing ring can be seen on the lower edge of the cover plate. This ring is pressed into the groove when the pressure is built up.

iii.) '''Introducing the sample into the recipient:''' For safety reasons it is important that the welded sample is not positioned directly in the oil-water emulsion. In the worst case, the sample or parts of the elastic foil can get into the liquid transport system of the cold isostatic press and block it, so that a pressure reduction is no longer possible and a service technician has to be called in. To safely avoid this risk, the sample must be placed in the oil-water emulsion in a specifically designed metal cage shown in Figure 4f. Spacers are welded onto the underpart of the metal cage, which prevent the metal mesh from resting directly on the bottom of the recipient. In this way, an unhindered pressure build-up and release is ensured. The metal cage also makes it easier to remove the sample after the cycle from the oil-water emulsion.

[[File:Wiki Keramik CIP Fig 04 english.jpg|thumb|center]]
'''Figure 4:''' ''Preparation of the system for the CIP cycle a.) Closed system b.) Attaching the screw to the cover plate c.) Starting the opening process d.) Open system e.) View on the oil-water emulsion f.) Metal cage for placing the encapsulated sample in the CIP device.''

iv.) '''Closing the recipient:''' After installing the metal cage including the sample in the recipient, the cover plate is closed via the hydraulic lifting system and the screw for fixing the cover plate is removed. The yoke, which absorbs the pressure in the axial direction, is then positioned over the cover plate. A specially designed locking system guarantees the exact position of the yoke in relation to the recipient. The locking bar is manually locked in the pressing position with a lever. '''Figure 5''' shows the individual steps for closing the recipient.

[[File:Wiki Keramik KIP Abb 05.jpg|thumb|center]]
'''Figure 5:''' ''a., b.) Closing the recipient using the hydraulic lifting device c.) Locking the yoke before starting the pressing cycle.''

v.) '''Pressure build-up and dwell time, protection against overpressure:''' As mentioned at the beginning, the pressure build-up takes place by a high-pressure pump which is connected to the interior of the recipient via the liquid transport system. '''Figure 6''' shows the system components relevant for pressure build-up. The desired pressure and the dwell time at this pressure are programmed via the system control display. The pressure is applied at the speed as defined in the program. The run of the pressure curve and the actual pressure can be read directly on the display and on an analog manometer. The cold isostatic press operated on the IEK-1 is designed for a maximum pressure of 4400 bar (440 MPa). To be on the safe side, the pressure in standard operation of the system should not exceed 4000 bar (400 MPa). The system is equipped with a rupture disc as overpressure protection. The rupture disc protects the system from uncontrolled failure and is designed with a safety factor of 1.1 based on the maximum pressure.

[[File:Wiki Keramik KIP Abb 06.jpg|thumb|center]]
'''Figure 6:''' ''a.) Programming of the pressing process via the display b.) Indication of the pressure via the manometer c.) Rupture disc as protection against overpressure.''

vi.) '''Decompression:''' Decompression is the most critical step in cold isostatic pressing. If there is still air in the sample after the sample preparation, it is strongly compressed during the CIP cycle. The high compression of the powder compact is associated with a strong reduction in the residual porosity. Accordingly, after pressing, there is a high flow resistance for the compressed air to escape and the pressure release takes a certain amount of time (up to a few minutes, depending on the pressing density achieved). If the pressure is released suddenly, this can lead to failure of the compact by severe cracking. It should be noted that a powder compact is also deformed elastically in addition to plastic deformation. When the pressure is released, there is therefore an elastic rebound of the pressed part ("spring-back" effect), which can be between 0.5 - 2%. Since the compression takes place in an elastic mold, the spring-back is viewed as less critical, but in the worst case it can also lead to damage to the pressed part, e.g. if it sticks to the die wall.

The decompression at the laboratory facility of the IEK-1 institute (type CIP 400-125 * 300Y, EPSI, Belgium) is initiated by opening a pneumatic high-pressure valve. The pressure release can then be regulated either manually via a valve or via an adjustable throttle valve. The throttle valve consists of a high pressure tube in which a needle is inserted. The decompression speed is controlled by the inner diameter of the tube and the position and thickness of the needle. '''Figure 7''' shows the display for initiating decompression and the throttle valve, which is located on the rear of the cold isostatic press.

[[File:Wiki Keramik KIP Abb 07 englisch.jpg|thumb|center]]
'''Figure 7:''' ''a.) Display for selecting the decompression mode b.) Throttle valve.''

After the pressure has been completely released, the system can be opened as already described under i.). Afterwards, the metal cage together with the sample can be removed. After removing the elastic foil, the sample is ready for use.

== Applications of cold isostatic pressing ==

Cold isostatic pressing is widely used in industry as well as in research and development. One advantage is the great flexibility of the method and the comparatively low costs for the die production. Cold isostatic pressing can be used universally for the compression of oxides, nitrides, borides, graphite, hard metals and other composite materials, as well as for metallic powders. The starting powder should have good compressibility, since the use of high proportions of binder is rather unusual with this method. In general, this method is used to manufacture semi-finished products as well as structural and functional components with moderate geometrical complexity. Specific application examples are spark plug insulators made of alumina, cap insulators, components for lambda sensors, semi-finished products for ceramic insulators and semi-finished products for ceramic balls. Metallic filter cartridges with a length of up to 1.8 m and a diameter of up to 300 mm are also manufactured using this process.

Cold isostatic pressing

2021-08-04T11:44:18Z

M.bram: /* How to conduct a cold isostatic pressing cycle */

== General principle of cold isostatic pressing (CIP) ==

The cold isostatic pressing CIP is based on the effect that a pressure applied to a liquid spreads evenly in all directions (so-called Pascal's principle). Inside the liquid, this leads to a homogeneous pressure distribution, which can be used for shaping ceramic and metallic powders if the powder is encapsulated in an elastic die. Elastic polymers (elastomers) such as polyurethane (PU), polyvinyl chloride (PVC), synthetic or natural rubber have proven successful as materials for the elastic die. The main components of a cold isostatic press are the recipient filled with the pressure transmission medium, the high-pressure pump, the locking system, the overpressure protection and the system control. The recipient is a pressure cylinder, which consists of either a high-strength, thick-walled steel cylinder or a thin-walled steel vessel with a pre-tensioned wire winding. '''Figure 1''' shows a cold isostatic press in lab scale.

The pressure transmission media used are preferably water with the addition of an anti-corrosion agent, oil-water emulsions or glycerine. A hydraulic unit like an axial piston pump is used to build up pressure. This unit is connected to the recipient via a fluid transport system with appropriate valves and throttles. The pressure cylinder is sealed, for example, by a polymer O-ring that is integrated into the cover plate and is pressed into a groove when the pressure is built up. In order to absorb the large forces in the axial direction, the cover plate of the recipient is usually supported by a massive yoke. A rupture disc is used to protect against overpressure, which fails when the critical pressure is exceeded and thus enables a regulated pressure release before irreversible damage to the recipient occurs. Cold isostatic pressing is carried out in most cases at room temperature. In specially designed presses, moderate heating of the pressure medium up to a maximum temperature of 300 °C is possible.

In technical practice, a distinction is made between two basic principles of cold isostatic pressing, the wet bag process and the dry bag process. In addition, the wet bag process can also be used for the post-compaction of components uniaxial pre-pressed in a rigid form. The three variants are explained in more detail below:

i.) '''Wet bag process:''' In the wet bag process, the die is a self-supporting, elastic hollow mold that is filled with the powder outside the cold isostatic press. Optionally, a metallic mandrel can be integrated into the hollow mold for the production of pipes. After filling, the die is closed with an elastic cover plate. In order to protect the interior of the die against the ingress of liquid, the die can also be enveloped with an elastic foil, which is then evacuated and sealed in a liquid-tight manner. The wet bag process is often used in research and development due to its great flexibility with regard to the system parameters (including pressures up to approx. 400 MPa), the component geometries and the number of components per cycle. It is also used in industry for the production of large-volume components (e.g. filter candles) and semi-finished products (e.g. for manufacturing of ceramic insulators) with dimensions up to the meter range. Disadvantages of the wet bag process are the limited dimensional accuracy due to the elastic die and the comparatively long cycle times of several minutes.

ii.) '''Dry bag process:''' In dry bag pressing, the elastic die is firmly fixed to the recipient. Correspondingly, the mold filling takes place inside the cold isostatic press. The main advantages compared to wet bag pressing are the possibility of full automation, fast cycle times in the range of 10 s - 100 s depending on the component size (increase in cycle time with component size) and better dimensional accuracy. However, it should be noted that in the area of fixing the elastic die to the recipient there are restrictions with regard to the homogeneity of the pressure distribution, which, however, are less relevant for simpler geometries such as plates, cylinders or tubes. Dry die pressing is preferred in industrial production. The best-known application example are spark plug insulators, which are manufactured in a fully automated manner in quantities of millions.

iii.) '''Post-compaction of uniaxially pressed components:''' The shaping of ceramic and metallic powders via the uniaxial pressing in rigid molds is restricted by the wall friction, which leads to increasing density gradients in the component with increasing height/diameter ratio. The result is an inhomogeneous shrinkage during the subsequent sintering. In order to use the advantages of uniaxial pressing in terms of dimensional accuracy and at the same time to achieve a homogeneous density distribution in the component, it is possible to pre-press components uniaxially in a rigid die at moderate pressures, e.g. in the range of 50 - 100 MPa, and then post-compact them using cold isostatic pressing, which can be done e.g. at pressures in the range of 300 - 400 MPa. For the pressure transfer, the component must be liquid-tight welded into an elastic foil. When welding the foil, it must made sure that the foil is not damaged by sharp edges or particles.

[[File:Wiki Keramik KIP Abb 01.jpg|thumb|center]]
'''Figure 1:''' ''Cold isostatic press on a laboratory scale operated at the institute IEK-1, Forschungszentrum Jülich (manufacturer EPSI, type CIP 400-125 * 300Y). Usable volume: Diameter 125 mm, height = 300 mm.'' 

== Advantages and limitations of cold isostatic pressing ==

i.) '''Advantages:''' The main advantage of cold isostatic pressing is the elimination of friction-related variation in density, such as occurring in the case of uniaxial pressing in rigid molds. Therefore, higher green densities, higher green strengths and more homogeneous structures can be achieved with cold isostatic pressing. For example, press-related textures in the structure can be avoided to a large extent. Furthermore, components with a height / diameter ratio greater than 3: 1 (usually specified as limit for uniaxial pressing) can be produced relatively easily. Because there is no wall friction, it is possible to omit dispense with lubricants during pressing and the required proportion of other pressing additives can be significantly reduced. Furthermore, ceramic feedstocks can be compacted that contain abrasive solid particles that would lead to high tool wear in the case of uniaxial pressing.

ii.) '''Limits:''' Cold isostatic pressing is only suitable for relatively simple component geometries and is therefore restricted with respect to near-net-shape production. Due to the elastic properties of the die, there are limitations with regard to dimensional accuracy even with simpler geometries. Furthermore, the surface roughness is usually also relatively high, since the die wall yields elastically during pressing. Furthermore, sharp-edged particles can be pressed into the die wall, whereby the die is damaged in the worst case and demolding is aggravated. In order to increase the dimensional accuracy, mechanical post-processing of the cold isostatically pressed semi-finished products (so-called green machining) is often carried out. The relatively high green strength of cold isostatically pressed semi-finished products has a positive effect here.

== How to conduct a cold isostatic pressing cycle ==

In the following, it is explained in detail which processing steps are carried out in cold isostatic pressing and what must be considered in order to obtain crack-free samples and avoid damage to the system. The processing steps shown were carried out in a cold isostatic laboratory press of the following type:

Type: CIP 400-125*300Y 
Manufacturer: EPSI, Temse, Belgium 
Material of recipient: SA 723 Class 3 
Recipient inner diameter: 125 mm 
Recipient inner height: 300 mm 
Maximum sample size: Limited by recipient volume 
Maximum filling height: 295 mm 
Recipient volume: 3.7 Liter 
Nominal operating pressure: 4000 bar (400 MPa) 
Maximum operating pressure: 4400 bar (440 MPa) 
Safety factor: 1,1 (related to 4840 bar, 484 MPa) 

i.) '''Encapsulation of the samples:''' Even with cold isostatic pressing, a uniform filling of the mold and a high filling density are basic requirements for successful compaction of the powder. In order to estimate the flowability of the powder, it is recommended to measure the bulk and tap density in accordance with DIN ISO 3923 and DIN ISO 3953. The flowability of a powder can be improved by granulating in a fluidizing bed or by spray drying. During granulation, spherical, easily flowable agglomerates are formed, which have a relatively low stability and are destroyed during the cold isostatic pressing. Some powder manufacturers offer powder directly in a granulated state. In order to increase the bulk density in the mold, the elastic die can optionally be vibrated or subjected to ultrasonic treatment. As an example, '''Figure 2''' shows a simple elastic mold made of rubber for cold isostatic pressing of round bars.

[[File:Wiki Keramik KIP Abb 02.jpg|thumb|center]]
'''Figure 2:''' ''Elastic mold (rubber tube with cover plug) for cold isostatic pressing of round bars.
'' 

As mentioned above, there is also the possibility of post-compaction of uniaxially pressed semi-finished parts using cold isostatic pressing. '''Figure 3''' shows how the welding of a pre-pressed part into an elastic foil can be carried out. For this purpose, at the IEK-1 institute, a vacuum sealer is used, which is usually applied in the household for sealing and freezing food. Elastic foils, which are established for this purpose, are suitable for encapsulation of pre-pressed parts in cold isostatic pressing as well. The sample is placed in the prepared bag, then interior is evacuated and the bag is finally liquid-tight welded. A more primitive alternative is to put the sample in a latex glove, which is evacuated, for example, by a water jet pump and sealed with a string.

[[File:Wiki Keramik KIP Abb 03.jpg|thumb|center]]
'''Figure 3:''' ''Sealing of a uniaxially pre-pressed sample in an elastic foil using a household vacuum sealer a.) Insertion of the uniaxially pre-pressed sample b.) Evacuation c.) Liquid-tight sealed sample.''

ii.) '''Opening the recipient:''' '''Figure 4''' shows the individual steps for opening the recipient of the cold isostatic press of the type CIP 400-125 * 300Y (EPSI, Belgium). The press is equipped with a hydraulic lifting device. A screw is attached to this, via which the cover plate is connected to the hydraulic lifting device. The screw is protected from damage by a cage. After the screw has been attached, the cover is lifted using the lifting device. The sealing ring can be seen on the lower edge of the cover plate. This ring is pressed into the groove when the pressure is built up.

iii.) '''Introducing the sample into the recipient:''' For safety reasons it is important that the welded sample is not positioned directly in the oil-water emulsion. In the worst case, the sample or parts of the elastic foil can get into the liquid transport system of the cold isostatic press and block it, so that a pressure reduction is no longer possible and a service technician has to be called in. To safely avoid this risk, the sample must be placed in the oil-water emulsion in a specifically designed metal cage shown in Figure 4f. Spacers are welded onto the underpart of the metal cage, which prevent the metal mesh from resting directly on the bottom of the recipient. In this way, an unhindered pressure build-up and release is ensured. The metal cage also makes it easier to remove the sample after the cycle from the oil-water emulsion.

[[File:Wiki Keramik CIP Fig 04 english.jpg|thumb|center]]
'''Figure 4:''' ''Preparation of the system for the CIP cycle a.) Closed system b.) Attaching the screw to the cover plate c.) Starting the opening process d.) Open system e.) View on the oil-water emulsion f.) Metal cage for placing the encapsulated sample in the CIP device.''

iv.) '''Closing the recipient:''' After installing the metal cage including the sample in the recipient, the cover plate is closed via the hydraulic lifting system and the screw for fixing the cover plate is removed. The yoke, which absorbs the pressure in the axial direction, is then positioned over the cover plate. A specially designed locking system guarantees the exact position of the yoke in relation to the recipient. The locking bar is manually locked in the pressing position with a lever. '''Figure 5''' shows the individual steps for closing the recipient.

[[File:Wiki Keramik KIP Abb 05.jpg|thumb|center]]
'''Figure 5:''' ''a., b.) Closing the recipient using the hydraulic lifting device c.) Locking the yoke before starting the pressing cycle.''

v.) '''Pressure build-up and dwell time, protection against overpressure:''' As mentioned at the beginning, the pressure build-up takes place by a high-pressure pump which is connected to the interior of the recipient via the liquid transport system. '''Figure 6''' shows the system components relevant for pressure build-up. The desired pressure and the dwell time at this pressure are programmed via the system control display. The pressure is applied at the speed as defined in the program. The run of the pressure curve and the actual pressure can be read directly on the display and on an analog manometer. The cold isostatic press operated on the IEK-1 is designed for a maximum pressure of 4400 bar (440 MPa). To be on the safe side, the pressure in standard operation of the system should not exceed 4000 bar (400 MPa). The system is equipped with a rupture disc as overpressure protection. The rupture disc protects the system from uncontrolled failure and is designed with a safety factor of 1.1 based on the maximum pressure.

[[File:Wiki Keramik KIP Abb 06.jpg|thumb|center]]
'''Figure 6:''' ''a.) Programming of the pressing process via the display b.) Indication of the pressure via the manometer c.) Rupture disc as protection against overpressure.''

vi.) '''Decompression:''' Decompression is the most critical step in cold isostatic pressing. If there is still air in the sample after the sample preparation, it is strongly compressed during the CIP cycle. The high compression of the powder compact is associated with a strong reduction in the residual porosity. Accordingly, after pressing, there is a high flow resistance for the compressed air to escape and the pressure release takes a certain amount of time (up to a few minutes, depending on the pressing density achieved). If the pressure is released suddenly, this can lead to failure of the compact by severe cracking. It should be noted that a powder compact is also deformed elastically in addition to plastic deformation. When the pressure is released, there is therefore an elastic rebound of the pressed part ("spring-back" effect), which can be between 0.5 - 2%. Since the compression takes place in an elastic mold, the spring-back is viewed as less critical, but in the worst case it can also lead to damage to the pressed part, e.g. if it sticks to the die wall.

The decompression at the laboratory facility of the IEK-1 institute (type CIP 400-125 * 300Y, EPSI, Belgium) is initiated by opening a pneumatic high-pressure valve. The pressure release can then be regulated either manually via a valve or via an adjustable throttle valve. The throttle valve consists of a high pressure tube in which a needle is inserted. The decompression speed is controlled by the inner diameter of the tube and the position and thickness of the needle. '''Figure 7''' shows the display for initiating decompression and the throttle valve, which is located on the rear of the cold isostatic press.

[[File:Wiki Keramik KIP Abb 07 englisch.jpg|thumb|center]]
'''Figure 7:''' ''a.) Display for selecting the decompression mode b.) Throttle valve.''

After the pressure has been completely released, the system can be opened as already described under i.). Afterwards, the metal cage together with the sample can be removed. After removing the elastic foil, the sample is ready for use.

== Applications of cold isostatic pressing ==

Cold isostatic pressing is widely used in industry as well as in research and development. One advantage is the great flexibility of the method and the comparatively low costs for the die production. Cold isostatic pressing can be used universally for the compression of oxides, nitrides, borides, graphite, hard metals and other composite materials, as well as for metallic powders. The starting powder should have good compressibility, since the use of high proportions of binder is rather unusual with this method. In general, this method is used to manufacture semi-finished products as well as structural and functional components with moderate geometrical complexity. Specific application examples are spark plug insulators made of alumina, cap insulators, components for lambda sensors, semi-finished products for ceramic insulators and semi-finished products for ceramic balls. Metallic filter cartridges with a length of up to 1.8 m and a diameter of up to 300 mm are also manufactured using this process.

File:Wiki Keramik KIP Abb 07 englisch.jpg

2021-08-04T11:43:59Z

M.bram:

Figure 7: a.) Display for selecting the decompression mode b.) Throttle valve.

Cold isostatic pressing

2021-08-04T11:30:50Z

M.bram: /* General principle of cold isostatic pressing (CIP) */

== General principle of cold isostatic pressing (CIP) ==

The cold isostatic pressing CIP is based on the effect that a pressure applied to a liquid spreads evenly in all directions (so-called Pascal's principle). Inside the liquid, this leads to a homogeneous pressure distribution, which can be used for shaping ceramic and metallic powders if the powder is encapsulated in an elastic die. Elastic polymers (elastomers) such as polyurethane (PU), polyvinyl chloride (PVC), synthetic or natural rubber have proven successful as materials for the elastic die. The main components of a cold isostatic press are the recipient filled with the pressure transmission medium, the high-pressure pump, the locking system, the overpressure protection and the system control. The recipient is a pressure cylinder, which consists of either a high-strength, thick-walled steel cylinder or a thin-walled steel vessel with a pre-tensioned wire winding. '''Figure 1''' shows a cold isostatic press in lab scale.

The pressure transmission media used are preferably water with the addition of an anti-corrosion agent, oil-water emulsions or glycerine. A hydraulic unit like an axial piston pump is used to build up pressure. This unit is connected to the recipient via a fluid transport system with appropriate valves and throttles. The pressure cylinder is sealed, for example, by a polymer O-ring that is integrated into the cover plate and is pressed into a groove when the pressure is built up. In order to absorb the large forces in the axial direction, the cover plate of the recipient is usually supported by a massive yoke. A rupture disc is used to protect against overpressure, which fails when the critical pressure is exceeded and thus enables a regulated pressure release before irreversible damage to the recipient occurs. Cold isostatic pressing is carried out in most cases at room temperature. In specially designed presses, moderate heating of the pressure medium up to a maximum temperature of 300 °C is possible.

In technical practice, a distinction is made between two basic principles of cold isostatic pressing, the wet bag process and the dry bag process. In addition, the wet bag process can also be used for the post-compaction of components uniaxial pre-pressed in a rigid form. The three variants are explained in more detail below:

i.) '''Wet bag process:''' In the wet bag process, the die is a self-supporting, elastic hollow mold that is filled with the powder outside the cold isostatic press. Optionally, a metallic mandrel can be integrated into the hollow mold for the production of pipes. After filling, the die is closed with an elastic cover plate. In order to protect the interior of the die against the ingress of liquid, the die can also be enveloped with an elastic foil, which is then evacuated and sealed in a liquid-tight manner. The wet bag process is often used in research and development due to its great flexibility with regard to the system parameters (including pressures up to approx. 400 MPa), the component geometries and the number of components per cycle. It is also used in industry for the production of large-volume components (e.g. filter candles) and semi-finished products (e.g. for manufacturing of ceramic insulators) with dimensions up to the meter range. Disadvantages of the wet bag process are the limited dimensional accuracy due to the elastic die and the comparatively long cycle times of several minutes.

ii.) '''Dry bag process:''' In dry bag pressing, the elastic die is firmly fixed to the recipient. Correspondingly, the mold filling takes place inside the cold isostatic press. The main advantages compared to wet bag pressing are the possibility of full automation, fast cycle times in the range of 10 s - 100 s depending on the component size (increase in cycle time with component size) and better dimensional accuracy. However, it should be noted that in the area of fixing the elastic die to the recipient there are restrictions with regard to the homogeneity of the pressure distribution, which, however, are less relevant for simpler geometries such as plates, cylinders or tubes. Dry die pressing is preferred in industrial production. The best-known application example are spark plug insulators, which are manufactured in a fully automated manner in quantities of millions.

iii.) '''Post-compaction of uniaxially pressed components:''' The shaping of ceramic and metallic powders via the uniaxial pressing in rigid molds is restricted by the wall friction, which leads to increasing density gradients in the component with increasing height/diameter ratio. The result is an inhomogeneous shrinkage during the subsequent sintering. In order to use the advantages of uniaxial pressing in terms of dimensional accuracy and at the same time to achieve a homogeneous density distribution in the component, it is possible to pre-press components uniaxially in a rigid die at moderate pressures, e.g. in the range of 50 - 100 MPa, and then post-compact them using cold isostatic pressing, which can be done e.g. at pressures in the range of 300 - 400 MPa. For the pressure transfer, the component must be liquid-tight welded into an elastic foil. When welding the foil, it must made sure that the foil is not damaged by sharp edges or particles.

[[File:Wiki Keramik KIP Abb 01.jpg|thumb|center]]
'''Figure 1:''' ''Cold isostatic press on a laboratory scale operated at the institute IEK-1, Forschungszentrum Jülich (manufacturer EPSI, type CIP 400-125 * 300Y). Usable volume: Diameter 125 mm, height = 300 mm.'' 

== Advantages and limitations of cold isostatic pressing ==

i.) '''Advantages:''' The main advantage of cold isostatic pressing is the elimination of friction-related variation in density, such as occurring in the case of uniaxial pressing in rigid molds. Therefore, higher green densities, higher green strengths and more homogeneous structures can be achieved with cold isostatic pressing. For example, press-related textures in the structure can be avoided to a large extent. Furthermore, components with a height / diameter ratio greater than 3: 1 (usually specified as limit for uniaxial pressing) can be produced relatively easily. Because there is no wall friction, it is possible to omit dispense with lubricants during pressing and the required proportion of other pressing additives can be significantly reduced. Furthermore, ceramic feedstocks can be compacted that contain abrasive solid particles that would lead to high tool wear in the case of uniaxial pressing.

ii.) '''Limits:''' Cold isostatic pressing is only suitable for relatively simple component geometries and is therefore restricted with respect to near-net-shape production. Due to the elastic properties of the die, there are limitations with regard to dimensional accuracy even with simpler geometries. Furthermore, the surface roughness is usually also relatively high, since the die wall yields elastically during pressing. Furthermore, sharp-edged particles can be pressed into the die wall, whereby the die is damaged in the worst case and demolding is aggravated. In order to increase the dimensional accuracy, mechanical post-processing of the cold isostatically pressed semi-finished products (so-called green machining) is often carried out. The relatively high green strength of cold isostatically pressed semi-finished products has a positive effect here.

== How to conduct a cold isostatic pressing cycle ==

In the following, it is explained in detail which processing steps are carried out in cold isostatic pressing and what must be considered in order to obtain crack-free samples and avoid damage to the system. The processing steps shown were carried out in a cold isostatic laboratory press of the following type:

Type: CIP 400-125*300Y 
Manufacturer: EPSI, Temse, Belgium 
Material of recipient: SA 723 Class 3 
Recipient inner diameter: 125 mm 
Recipient inner height: 300 mm 
Maximum sample size: Limited by recipient volume 
Maximum filling height: 295 mm 
Recipient volume: 3.7 Liter 
Nominal operating pressure: 4000 bar (400 MPa) 
Maximum operating pressure: 4400 bar (440 MPa) 
Safety factor: 1,1 (related to 4840 bar, 484 MPa) 

i.) '''Encapsulation of the samples:''' Even with cold isostatic pressing, a uniform filling of the mold and a high filling density are basic requirements for successful compaction of the powder. In order to estimate the flowability of the powder, it is recommended to measure the bulk and tap density in accordance with DIN ISO 3923 and DIN ISO 3953. The flowability of a powder can be improved by granulating in a fluidizing bed or by spray drying. During granulation, spherical, easily flowable agglomerates are formed, which have a relatively low stability and are destroyed during the cold isostatic pressing. Some powder manufacturers offer powder directly in a granulated state. In order to increase the bulk density in the mold, the elastic die can optionally be vibrated or subjected to ultrasonic treatment. As an example, '''Figure 2''' shows a simple elastic mold made of rubber for cold isostatic pressing of round bars.

[[File:Wiki Keramik KIP Abb 02.jpg|thumb|center]]
'''Figure 2:''' ''Elastic mold (rubber tube with cover plug) for cold isostatic pressing of round bars.
'' 

As mentioned above, there is also the possibility of post-compaction of uniaxially pressed semi-finished parts using cold isostatic pressing. '''Figure 3''' shows how the welding of a pre-pressed part into an elastic foil can be carried out. For this purpose, at the IEK-1 institute, a vacuum sealer is used, which is usually applied in the household for sealing and freezing food. Elastic foils, which are established for this purpose, are suitable for encapsulation of pre-pressed parts in cold isostatic pressing as well. The sample is placed in the prepared bag, then interior is evacuated and the bag is finally liquid-tight welded. A more primitive alternative is to put the sample in a latex glove, which is evacuated, for example, by a water jet pump and sealed with a string.

[[File:Wiki Keramik KIP Abb 03.jpg|thumb|center]]
'''Figure 3:''' ''Sealing of a uniaxially pre-pressed sample in an elastic foil using a household vacuum sealer a.) Insertion of the uniaxially pre-pressed sample b.) Evacuation c.) Liquid-tight sealed sample.''

ii.) '''Opening the recipient:''' '''Figure 4''' shows the individual steps for opening the recipient of the cold isostatic press of the type CIP 400-125 * 300Y (EPSI, Belgium). The press is equipped with a hydraulic lifting device. A screw is attached to this, via which the cover plate is connected to the hydraulic lifting device. The screw is protected from damage by a cage. After the screw has been attached, the cover is lifted using the lifting device. The sealing ring can be seen on the lower edge of the cover plate. This ring is pressed into the groove when the pressure is built up.

iii.) '''Introducing the sample into the recipient:''' For safety reasons it is important that the welded sample is not positioned directly in the oil-water emulsion. In the worst case, the sample or parts of the elastic foil can get into the liquid transport system of the cold isostatic press and block it, so that a pressure reduction is no longer possible and a service technician has to be called in. To safely avoid this risk, the sample must be placed in the oil-water emulsion in a specifically designed metal cage shown in Figure 4f. Spacers are welded onto the underpart of the metal cage, which prevent the metal mesh from resting directly on the bottom of the recipient. In this way, an unhindered pressure build-up and release is ensured. The metal cage also makes it easier to remove the sample after the cycle from the oil-water emulsion.

[[File:Wiki Keramik CIP Fig 04 english.jpg|thumb|center]]
'''Figure 4:''' ''Preparation of the system for the CIP cycle a.) Closed system b.) Attaching the screw to the cover plate c.) Starting the opening process d.) Open system e.) View on the oil-water emulsion f.) Metal cage for placing the encapsulated sample in the CIP device.''

iv.) '''Closing the recipient:''' After installing the metal cage including the sample in the recipient, the cover plate is closed via the hydraulic lifting system and the screw for fixing the cover plate is removed. The yoke, which absorbs the pressure in the axial direction, is then positioned over the cover plate. A specially designed locking system guarantees the exact position of the yoke in relation to the recipient. The locking bar is manually locked in the pressing position with a lever. '''Figure 5''' shows the individual steps for closing the recipient.

[[File:Wiki Keramik KIP Abb 05.jpg|thumb|center]]
'''Figure 5:''' ''a., b.) Closing the recipient using the hydraulic lifting device c.) Locking the yoke before starting the pressing cycle.''

v.) '''Pressure build-up and dwell time, protection against overpressure:''' As mentioned at the beginning, the pressure build-up takes place by a high-pressure pump which is connected to the interior of the recipient via the liquid transport system. '''Figure 6''' shows the system components relevant for pressure build-up. The desired pressure and the dwell time at this pressure are programmed via the system control display. The pressure is applied at the speed as defined in the program. The run of the pressure curve and the actual pressure can be read directly on the display and on an analog manometer. The cold isostatic press operated on the IEK-1 is designed for a maximum pressure of 4400 bar (440 MPa). To be on the safe side, the pressure in standard operation of the system should not exceed 4000 bar (400 MPa). The system is equipped with a rupture disc as overpressure protection. The rupture disc protects the system from uncontrolled failure and is designed with a safety factor of 1.1 based on the maximum pressure.

[[File:Wiki Keramik KIP Abb 06.jpg|thumb|center]]
'''Figure 6:''' ''a.) Programming of the pressing process via the display b.) Indication of the pressure via the manometer c.) Rupture disc as protection against overpressure.''

vi.) '''Decompression:''' Decompression is the most critical step in cold isostatic pressing. If there is still air in the sample after the sample preparation, it is strongly compressed during the CIP cycle. The high compression of the powder compact is associated with a strong reduction in the residual porosity. Accordingly, after pressing, there is a high flow resistance for the compressed air to escape and the pressure release takes a certain amount of time (up to a few minutes, depending on the pressing density achieved). If the pressure is released suddenly, this can lead to failure of the compact by severe cracking. It should be noted that a powder compact is also deformed elastically in addition to plastic deformation. When the pressure is released, there is therefore an elastic rebound of the pressed part ("spring-back" effect), which can be between 0.5 - 2%. Since the compression takes place in an elastic mold, the spring-back is viewed as less critical, but in the worst case it can also lead to damage to the pressed part, e.g. if it sticks to the die wall.

The decompression at the laboratory facility of the IEK-1 institute (type CIP 400-125 * 300Y, EPSI, Belgium) is initiated by opening a pneumatic high-pressure valve. The pressure release can then be regulated either manually via a valve or via an adjustable throttle valve. The throttle valve consists of a high pressure tube in which a needle is inserted. The decompression speed is controlled by the inner diameter of the tube and the position and thickness of the needle. '''Figure 7''' shows the display for initiating decompression and the throttle valve, which is located on the rear of the cold isostatic press.

[[File:Wiki Keramik KIP Abb 07.jpg|thumb|center]]
'''Figure 7:''' ''a.) Display for selecting the decompression mode b.) Throttle valve.''

After the pressure has been completely released, the system can be opened as already described under i.). Afterwards, the metal cage together with the sample can be removed. After removing the elastic foil, the sample is ready for use.

== Applications of cold isostatic pressing ==

Cold isostatic pressing is widely used in industry as well as in research and development. One advantage is the great flexibility of the method and the comparatively low costs for the die production. Cold isostatic pressing can be used universally for the compression of oxides, nitrides, borides, graphite, hard metals and other composite materials, as well as for metallic powders. The starting powder should have good compressibility, since the use of high proportions of binder is rather unusual with this method. In general, this method is used to manufacture semi-finished products as well as structural and functional components with moderate geometrical complexity. Specific application examples are spark plug insulators made of alumina, cap insulators, components for lambda sensors, semi-finished products for ceramic insulators and semi-finished products for ceramic balls. Metallic filter cartridges with a length of up to 1.8 m and a diameter of up to 300 mm are also manufactured using this process.

Cold isostatic pressing

2021-08-04T11:30:10Z

M.bram: /* How to conduct a cold isostatic pressing cycle */

== General principle of cold isostatic pressing (CIP) ==

The cold isostatic pressing CIP is based on the effect that a pressure applied to a liquid spreads evenly in all directions (so-called Pascal's principle). Inside the liquid, this leads to a homogeneous pressure distribution, which can be used for shaping ceramic and metallic powders if the powder is encapsulated in an elastic die. Elastic polymers (elastomers) such as polyurethane (PU), polyvinyl chloride (PVC), synthetic or natural rubber have proven successful as materials for the elastic die. The main components of a cold isostatic press are the recipient filled with the pressure transmission medium, the high-pressure pump, the locking system, the overpressure protection and the system control. The recipient is a pressure cylinder, which consists of either a high-strength, thick-walled steel cylinder or a thin-walled steel vessel with a pre-tensioned wire winding. '''Figure 1''' shows a cold isostatic press in lab scale.

The pressure transmission media used are preferably water with the addition of an anti-corrosion agent, oil-water emulsions or glycerine. A hydraulic unit like an axial piston pump is used to build up pressure. This unit is connected to the recipient via a fluid transport system with appropriate valves and throttles. The pressure cylinder is sealed, for example, by a polymer O-ring that is integrated into the cover plate and is pressed into a groove when the pressure is built up. In order to absorb the large forces in the axial direction, the cover plate of the recipient is usually supported by a massive yoke. A rupture disc is used to protect against overpressure, which fails when the critical pressure is exceeded and thus enables a regulated pressure release before irreversible damage to the recipient occurs. Cold isostatic pressing is carried out in most cases at room temperature. In specially designed presses, moderate heating of the pressure medium up to a maximum temperature of 300 °C is possible.

In technical practice, a distinction is made between two basic principles of cold isostatic pressing, the wet bag process and the dry bag process. In addition, the wet bag process can also be used for the post-compaction of components uniaxial pre-pressed in a rigid form. The three variants are explained in more detail below:

i.) '''Wet bag process:''' In the wet bag process, the die is a self-supporting, elastic hollow mold that is filled with the powder outside the cold isostatic press. Optionally, a metallic mandrel can be integrated into the hollow mold for the production of pipes. After filling, the die is closed with an elastic cover plate. In order to protect the interior of the die against the ingress of liquid, the die can also be enveloped with an elastic foil, which is then evacuated and sealed in a liquid-tight manner. The wet bag process is often used in research and development due to its great flexibility with regard to the system parameters (including pressures up to approx. 400 MPa), the component geometries and the number of components per cycle. It is also used in industry for the production of large-volume components (e.g. filter candles) and semi-finished products (e.g. for manufacturing of ceramic insulators) with dimensions up to the meter range. Disadvantages of the wet bag process are the limited dimensional accuracy due to the elastic die and the comparatively long cycle times of several minutes.

ii.) '''Dry bag process:''' In dry bag pressing, the elastic die is firmly fixed to the recipient. Correspondingly, the mold filling takes place inside the cold isostatic press. The main advantages compared to wet bag pressing are the possibility of full automation, fast cycle times in the range of 10 s - 100 s depending on the component size (increase in cycle time with component size) and better dimensional accuracy. However, it should be noted that in the area of fixing the elastic die to the recipient there are restrictions with regard to the homogeneity of the pressure distribution, which, however, are less relevant for simpler geometries such as plates, cylinders or tubes. Dry die pressing is preferred in industrial production. The best-known application example are spark plug insulators, which are manufactured in a fully automated manner in quantities of millions.

iii.) '''Post-compaction of uniaxially pressed components:''' The shaping of ceramic and metallic powders via the uniaxial pressing in rigid molds is restricted by the wall friction, which leads to increasing density gradients in the component with increasing height/diameter ratio. The result is an inhomogeneous shrinkage during the subsequent sintering. In order to use the advantages of uniaxial pressing in terms of dimensional accuracy and at the same time to achieve a homogeneous density distribution in the component, it is possible to pre-press components uniaxially in a rigid die at moderate pressures, e.g. in the range of 50 - 100 MPa, and then post-compact them using cold isostatic pressing, which can be done e.g. at pressures in the range of 300 - 400 MPa. For the pressure transfer, the component must be liquid-tight welded into an elastic foil. When welding the foil, it must made sure that the foil is not damaged by sharp edges or particles.

[[File:Wiki Keramik KIP Abb 01.jpg|thumb|center]]
'''Figure 1:''' Cold isostatic press on a laboratory scale operated at the institute IEK-1, Forschungszentrum Jülich (manufacturer EPSI, type CIP 400-125 * 300Y). Usable volume: Diameter 125 mm, height = 300 mm. 

== Advantages and limitations of cold isostatic pressing ==

i.) '''Advantages:''' The main advantage of cold isostatic pressing is the elimination of friction-related variation in density, such as occurring in the case of uniaxial pressing in rigid molds. Therefore, higher green densities, higher green strengths and more homogeneous structures can be achieved with cold isostatic pressing. For example, press-related textures in the structure can be avoided to a large extent. Furthermore, components with a height / diameter ratio greater than 3: 1 (usually specified as limit for uniaxial pressing) can be produced relatively easily. Because there is no wall friction, it is possible to omit dispense with lubricants during pressing and the required proportion of other pressing additives can be significantly reduced. Furthermore, ceramic feedstocks can be compacted that contain abrasive solid particles that would lead to high tool wear in the case of uniaxial pressing.

ii.) '''Limits:''' Cold isostatic pressing is only suitable for relatively simple component geometries and is therefore restricted with respect to near-net-shape production. Due to the elastic properties of the die, there are limitations with regard to dimensional accuracy even with simpler geometries. Furthermore, the surface roughness is usually also relatively high, since the die wall yields elastically during pressing. Furthermore, sharp-edged particles can be pressed into the die wall, whereby the die is damaged in the worst case and demolding is aggravated. In order to increase the dimensional accuracy, mechanical post-processing of the cold isostatically pressed semi-finished products (so-called green machining) is often carried out. The relatively high green strength of cold isostatically pressed semi-finished products has a positive effect here.

== How to conduct a cold isostatic pressing cycle ==

In the following, it is explained in detail which processing steps are carried out in cold isostatic pressing and what must be considered in order to obtain crack-free samples and avoid damage to the system. The processing steps shown were carried out in a cold isostatic laboratory press of the following type:

Type: CIP 400-125*300Y 
Manufacturer: EPSI, Temse, Belgium 
Material of recipient: SA 723 Class 3 
Recipient inner diameter: 125 mm 
Recipient inner height: 300 mm 
Maximum sample size: Limited by recipient volume 
Maximum filling height: 295 mm 
Recipient volume: 3.7 Liter 
Nominal operating pressure: 4000 bar (400 MPa) 
Maximum operating pressure: 4400 bar (440 MPa) 
Safety factor: 1,1 (related to 4840 bar, 484 MPa) 

i.) '''Encapsulation of the samples:''' Even with cold isostatic pressing, a uniform filling of the mold and a high filling density are basic requirements for successful compaction of the powder. In order to estimate the flowability of the powder, it is recommended to measure the bulk and tap density in accordance with DIN ISO 3923 and DIN ISO 3953. The flowability of a powder can be improved by granulating in a fluidizing bed or by spray drying. During granulation, spherical, easily flowable agglomerates are formed, which have a relatively low stability and are destroyed during the cold isostatic pressing. Some powder manufacturers offer powder directly in a granulated state. In order to increase the bulk density in the mold, the elastic die can optionally be vibrated or subjected to ultrasonic treatment. As an example, '''Figure 2''' shows a simple elastic mold made of rubber for cold isostatic pressing of round bars.

[[File:Wiki Keramik KIP Abb 02.jpg|thumb|center]]
'''Figure 2:''' ''Elastic mold (rubber tube with cover plug) for cold isostatic pressing of round bars.
'' 

As mentioned above, there is also the possibility of post-compaction of uniaxially pressed semi-finished parts using cold isostatic pressing. '''Figure 3''' shows how the welding of a pre-pressed part into an elastic foil can be carried out. For this purpose, at the IEK-1 institute, a vacuum sealer is used, which is usually applied in the household for sealing and freezing food. Elastic foils, which are established for this purpose, are suitable for encapsulation of pre-pressed parts in cold isostatic pressing as well. The sample is placed in the prepared bag, then interior is evacuated and the bag is finally liquid-tight welded. A more primitive alternative is to put the sample in a latex glove, which is evacuated, for example, by a water jet pump and sealed with a string.

[[File:Wiki Keramik KIP Abb 03.jpg|thumb|center]]
'''Figure 3:''' ''Sealing of a uniaxially pre-pressed sample in an elastic foil using a household vacuum sealer a.) Insertion of the uniaxially pre-pressed sample b.) Evacuation c.) Liquid-tight sealed sample.''

ii.) '''Opening the recipient:''' '''Figure 4''' shows the individual steps for opening the recipient of the cold isostatic press of the type CIP 400-125 * 300Y (EPSI, Belgium). The press is equipped with a hydraulic lifting device. A screw is attached to this, via which the cover plate is connected to the hydraulic lifting device. The screw is protected from damage by a cage. After the screw has been attached, the cover is lifted using the lifting device. The sealing ring can be seen on the lower edge of the cover plate. This ring is pressed into the groove when the pressure is built up.

iii.) '''Introducing the sample into the recipient:''' For safety reasons it is important that the welded sample is not positioned directly in the oil-water emulsion. In the worst case, the sample or parts of the elastic foil can get into the liquid transport system of the cold isostatic press and block it, so that a pressure reduction is no longer possible and a service technician has to be called in. To safely avoid this risk, the sample must be placed in the oil-water emulsion in a specifically designed metal cage shown in Figure 4f. Spacers are welded onto the underpart of the metal cage, which prevent the metal mesh from resting directly on the bottom of the recipient. In this way, an unhindered pressure build-up and release is ensured. The metal cage also makes it easier to remove the sample after the cycle from the oil-water emulsion.

[[File:Wiki Keramik CIP Fig 04 english.jpg|thumb|center]]
'''Figure 4:''' ''Preparation of the system for the CIP cycle a.) Closed system b.) Attaching the screw to the cover plate c.) Starting the opening process d.) Open system e.) View on the oil-water emulsion f.) Metal cage for placing the encapsulated sample in the CIP device.''

iv.) '''Closing the recipient:''' After installing the metal cage including the sample in the recipient, the cover plate is closed via the hydraulic lifting system and the screw for fixing the cover plate is removed. The yoke, which absorbs the pressure in the axial direction, is then positioned over the cover plate. A specially designed locking system guarantees the exact position of the yoke in relation to the recipient. The locking bar is manually locked in the pressing position with a lever. '''Figure 5''' shows the individual steps for closing the recipient.

[[File:Wiki Keramik KIP Abb 05.jpg|thumb|center]]
'''Figure 5:''' ''a., b.) Closing the recipient using the hydraulic lifting device c.) Locking the yoke before starting the pressing cycle.''

v.) '''Pressure build-up and dwell time, protection against overpressure:''' As mentioned at the beginning, the pressure build-up takes place by a high-pressure pump which is connected to the interior of the recipient via the liquid transport system. '''Figure 6''' shows the system components relevant for pressure build-up. The desired pressure and the dwell time at this pressure are programmed via the system control display. The pressure is applied at the speed as defined in the program. The run of the pressure curve and the actual pressure can be read directly on the display and on an analog manometer. The cold isostatic press operated on the IEK-1 is designed for a maximum pressure of 4400 bar (440 MPa). To be on the safe side, the pressure in standard operation of the system should not exceed 4000 bar (400 MPa). The system is equipped with a rupture disc as overpressure protection. The rupture disc protects the system from uncontrolled failure and is designed with a safety factor of 1.1 based on the maximum pressure.

[[File:Wiki Keramik KIP Abb 06.jpg|thumb|center]]
'''Figure 6:''' ''a.) Programming of the pressing process via the display b.) Indication of the pressure via the manometer c.) Rupture disc as protection against overpressure.''

vi.) '''Decompression:''' Decompression is the most critical step in cold isostatic pressing. If there is still air in the sample after the sample preparation, it is strongly compressed during the CIP cycle. The high compression of the powder compact is associated with a strong reduction in the residual porosity. Accordingly, after pressing, there is a high flow resistance for the compressed air to escape and the pressure release takes a certain amount of time (up to a few minutes, depending on the pressing density achieved). If the pressure is released suddenly, this can lead to failure of the compact by severe cracking. It should be noted that a powder compact is also deformed elastically in addition to plastic deformation. When the pressure is released, there is therefore an elastic rebound of the pressed part ("spring-back" effect), which can be between 0.5 - 2%. Since the compression takes place in an elastic mold, the spring-back is viewed as less critical, but in the worst case it can also lead to damage to the pressed part, e.g. if it sticks to the die wall.

The decompression at the laboratory facility of the IEK-1 institute (type CIP 400-125 * 300Y, EPSI, Belgium) is initiated by opening a pneumatic high-pressure valve. The pressure release can then be regulated either manually via a valve or via an adjustable throttle valve. The throttle valve consists of a high pressure tube in which a needle is inserted. The decompression speed is controlled by the inner diameter of the tube and the position and thickness of the needle. '''Figure 7''' shows the display for initiating decompression and the throttle valve, which is located on the rear of the cold isostatic press.

[[File:Wiki Keramik KIP Abb 07.jpg|thumb|center]]
'''Figure 7:''' ''a.) Display for selecting the decompression mode b.) Throttle valve.''

After the pressure has been completely released, the system can be opened as already described under i.). Afterwards, the metal cage together with the sample can be removed. After removing the elastic foil, the sample is ready for use.

== Applications of cold isostatic pressing ==

Cold isostatic pressing is widely used in industry as well as in research and development. One advantage is the great flexibility of the method and the comparatively low costs for the die production. Cold isostatic pressing can be used universally for the compression of oxides, nitrides, borides, graphite, hard metals and other composite materials, as well as for metallic powders. The starting powder should have good compressibility, since the use of high proportions of binder is rather unusual with this method. In general, this method is used to manufacture semi-finished products as well as structural and functional components with moderate geometrical complexity. Specific application examples are spark plug insulators made of alumina, cap insulators, components for lambda sensors, semi-finished products for ceramic insulators and semi-finished products for ceramic balls. Metallic filter cartridges with a length of up to 1.8 m and a diameter of up to 300 mm are also manufactured using this process.

Cold isostatic pressing

2021-08-04T11:29:08Z

M.bram: /* How to conduct a cold isostatic pressing cycle */

== General principle of cold isostatic pressing (CIP) ==

The cold isostatic pressing CIP is based on the effect that a pressure applied to a liquid spreads evenly in all directions (so-called Pascal's principle). Inside the liquid, this leads to a homogeneous pressure distribution, which can be used for shaping ceramic and metallic powders if the powder is encapsulated in an elastic die. Elastic polymers (elastomers) such as polyurethane (PU), polyvinyl chloride (PVC), synthetic or natural rubber have proven successful as materials for the elastic die. The main components of a cold isostatic press are the recipient filled with the pressure transmission medium, the high-pressure pump, the locking system, the overpressure protection and the system control. The recipient is a pressure cylinder, which consists of either a high-strength, thick-walled steel cylinder or a thin-walled steel vessel with a pre-tensioned wire winding. '''Figure 1''' shows a cold isostatic press in lab scale.

The pressure transmission media used are preferably water with the addition of an anti-corrosion agent, oil-water emulsions or glycerine. A hydraulic unit like an axial piston pump is used to build up pressure. This unit is connected to the recipient via a fluid transport system with appropriate valves and throttles. The pressure cylinder is sealed, for example, by a polymer O-ring that is integrated into the cover plate and is pressed into a groove when the pressure is built up. In order to absorb the large forces in the axial direction, the cover plate of the recipient is usually supported by a massive yoke. A rupture disc is used to protect against overpressure, which fails when the critical pressure is exceeded and thus enables a regulated pressure release before irreversible damage to the recipient occurs. Cold isostatic pressing is carried out in most cases at room temperature. In specially designed presses, moderate heating of the pressure medium up to a maximum temperature of 300 °C is possible.

In technical practice, a distinction is made between two basic principles of cold isostatic pressing, the wet bag process and the dry bag process. In addition, the wet bag process can also be used for the post-compaction of components uniaxial pre-pressed in a rigid form. The three variants are explained in more detail below:

i.) '''Wet bag process:''' In the wet bag process, the die is a self-supporting, elastic hollow mold that is filled with the powder outside the cold isostatic press. Optionally, a metallic mandrel can be integrated into the hollow mold for the production of pipes. After filling, the die is closed with an elastic cover plate. In order to protect the interior of the die against the ingress of liquid, the die can also be enveloped with an elastic foil, which is then evacuated and sealed in a liquid-tight manner. The wet bag process is often used in research and development due to its great flexibility with regard to the system parameters (including pressures up to approx. 400 MPa), the component geometries and the number of components per cycle. It is also used in industry for the production of large-volume components (e.g. filter candles) and semi-finished products (e.g. for manufacturing of ceramic insulators) with dimensions up to the meter range. Disadvantages of the wet bag process are the limited dimensional accuracy due to the elastic die and the comparatively long cycle times of several minutes.

ii.) '''Dry bag process:''' In dry bag pressing, the elastic die is firmly fixed to the recipient. Correspondingly, the mold filling takes place inside the cold isostatic press. The main advantages compared to wet bag pressing are the possibility of full automation, fast cycle times in the range of 10 s - 100 s depending on the component size (increase in cycle time with component size) and better dimensional accuracy. However, it should be noted that in the area of fixing the elastic die to the recipient there are restrictions with regard to the homogeneity of the pressure distribution, which, however, are less relevant for simpler geometries such as plates, cylinders or tubes. Dry die pressing is preferred in industrial production. The best-known application example are spark plug insulators, which are manufactured in a fully automated manner in quantities of millions.

iii.) '''Post-compaction of uniaxially pressed components:''' The shaping of ceramic and metallic powders via the uniaxial pressing in rigid molds is restricted by the wall friction, which leads to increasing density gradients in the component with increasing height/diameter ratio. The result is an inhomogeneous shrinkage during the subsequent sintering. In order to use the advantages of uniaxial pressing in terms of dimensional accuracy and at the same time to achieve a homogeneous density distribution in the component, it is possible to pre-press components uniaxially in a rigid die at moderate pressures, e.g. in the range of 50 - 100 MPa, and then post-compact them using cold isostatic pressing, which can be done e.g. at pressures in the range of 300 - 400 MPa. For the pressure transfer, the component must be liquid-tight welded into an elastic foil. When welding the foil, it must made sure that the foil is not damaged by sharp edges or particles.

[[File:Wiki Keramik KIP Abb 01.jpg|thumb|center]]
'''Figure 1:''' Cold isostatic press on a laboratory scale operated at the institute IEK-1, Forschungszentrum Jülich (manufacturer EPSI, type CIP 400-125 * 300Y). Usable volume: Diameter 125 mm, height = 300 mm. 

== Advantages and limitations of cold isostatic pressing ==

i.) '''Advantages:''' The main advantage of cold isostatic pressing is the elimination of friction-related variation in density, such as occurring in the case of uniaxial pressing in rigid molds. Therefore, higher green densities, higher green strengths and more homogeneous structures can be achieved with cold isostatic pressing. For example, press-related textures in the structure can be avoided to a large extent. Furthermore, components with a height / diameter ratio greater than 3: 1 (usually specified as limit for uniaxial pressing) can be produced relatively easily. Because there is no wall friction, it is possible to omit dispense with lubricants during pressing and the required proportion of other pressing additives can be significantly reduced. Furthermore, ceramic feedstocks can be compacted that contain abrasive solid particles that would lead to high tool wear in the case of uniaxial pressing.

ii.) '''Limits:''' Cold isostatic pressing is only suitable for relatively simple component geometries and is therefore restricted with respect to near-net-shape production. Due to the elastic properties of the die, there are limitations with regard to dimensional accuracy even with simpler geometries. Furthermore, the surface roughness is usually also relatively high, since the die wall yields elastically during pressing. Furthermore, sharp-edged particles can be pressed into the die wall, whereby the die is damaged in the worst case and demolding is aggravated. In order to increase the dimensional accuracy, mechanical post-processing of the cold isostatically pressed semi-finished products (so-called green machining) is often carried out. The relatively high green strength of cold isostatically pressed semi-finished products has a positive effect here.

== How to conduct a cold isostatic pressing cycle ==

In the following, it is explained in detail which processing steps are carried out in cold isostatic pressing and what must be considered in order to obtain crack-free samples and avoid damage to the system. The processing steps shown were carried out in a cold isostatic laboratory press of the following type:

Type: CIP 400-125*300Y 
Manufacturer: EPSI, Temse, Belgien 
Material of recipient: SA 723 Class 3 
Recipient inner diameter: 125 mm 
Recipient inner height: 300 mm 
Maximum sample size: limited by recipient volume 
Maximum filling height: 295 mm 
Recipient volume: 3.7 Liter 
Nominal operating pressure: 4000 bar (400 MPa) 
Maximum operating pressure: 4400 bar (440 MPa) 
Safety factor: 1,1 (related to 4840 bar, 484 MPa) 

i.) '''Encapsulation of the samples:''' Even with cold isostatic pressing, a uniform filling of the mold and a high filling density are basic requirements for successful compaction of the powder. In order to estimate the flowability of the powder, it is recommended to measure the bulk and tap density in accordance with DIN ISO 3923 and DIN ISO 3953. The flowability of a powder can be improved by granulating in a fluidizing bed or by spray drying. During granulation, spherical, easily flowable agglomerates are formed, which have a relatively low stability and are destroyed during the cold isostatic pressing. Some powder manufacturers offer powder directly in a granulated state. In order to increase the bulk density in the mold, the elastic die can optionally be vibrated or subjected to ultrasonic treatment. As an example, '''Figure 2''' shows a simple elastic mold made of rubber for cold isostatic pressing of round bars.

[[File:Wiki Keramik KIP Abb 02.jpg|thumb|center]]
'''Figure 2:''' ''Elastic mold (rubber tube with cover plug) for cold isostatic pressing of round bars.
'' 

As mentioned above, there is also the possibility of post-compaction of uniaxially pressed semi-finished parts using cold isostatic pressing. '''Figure 3''' shows how the welding of a pre-pressed part into an elastic foil can be carried out. For this purpose, at the IEK-1 institute, a vacuum sealer is used, which is usually applied in the household for sealing and freezing food. Elastic foils, which are established for this purpose, are suitable for encapsulation of pre-pressed parts in cold isostatic pressing as well. The sample is placed in the prepared bag, then interior is evacuated and the bag is finally liquid-tight welded. A more primitive alternative is to put the sample in a latex glove, which is evacuated, for example, by a water jet pump and sealed with a string.

[[File:Wiki Keramik KIP Abb 03.jpg|thumb|center]]
'''Figure 3:''' ''Sealing of a uniaxially pre-pressed sample in an elastic foil using a household vacuum sealer a.) Insertion of the uniaxially pre-pressed sample b.) Evacuation c.) Liquid-tight sealed sample.''

ii.) '''Opening the recipient:''' '''Figure 4''' shows the individual steps for opening the recipient of the cold isostatic press of the type CIP 400-125 * 300Y (EPSI, Belgium). The press is equipped with a hydraulic lifting device. A screw is attached to this, via which the cover plate is connected to the hydraulic lifting device. The screw is protected from damage by a cage. After the screw has been attached, the cover is lifted using the lifting device. The sealing ring can be seen on the lower edge of the cover plate. This ring is pressed into the groove when the pressure is built up.

iii.) '''Introducing the sample into the recipient:''' For safety reasons it is important that the welded sample is not positioned directly in the oil-water emulsion. In the worst case, the sample or parts of the elastic foil can get into the liquid transport system of the cold isostatic press and block it, so that a pressure reduction is no longer possible and a service technician has to be called in. To safely avoid this risk, the sample must be placed in the oil-water emulsion in a specifically designed metal cage shown in Figure 4f. Spacers are welded onto the underpart of the metal cage, which prevent the metal mesh from resting directly on the bottom of the recipient. In this way, an unhindered pressure build-up and release is ensured. The metal cage also makes it easier to remove the sample after the cycle from the oil-water emulsion.

[[File:Wiki Keramik CIP Fig 04 english.jpg|thumb|center]]
'''Figure 4:''' ''Preparation of the system for the CIP cycle a.) Closed system b.) Attaching the screw to the cover plate c.) Starting the opening process d.) Open system e.) View on the oil-water emulsion f.) Metal cage for placing the encapsulated sample in the CIP device.''

iv.) '''Closing the recipient:''' After installing the metal cage including the sample in the recipient, the cover plate is closed via the hydraulic lifting system and the screw for fixing the cover plate is removed. The yoke, which absorbs the pressure in the axial direction, is then positioned over the cover plate. A specially designed locking system guarantees the exact position of the yoke in relation to the recipient. The locking bar is manually locked in the pressing position with a lever. '''Figure 5''' shows the individual steps for closing the recipient.

[[File:Wiki Keramik KIP Abb 05.jpg|thumb|center]]
'''Figure 5:''' ''a., b.) Closing the recipient using the hydraulic lifting device c.) Locking the yoke before starting the pressing cycle.''

v.) '''Pressure build-up and dwell time, protection against overpressure:''' As mentioned at the beginning, the pressure build-up takes place by a high-pressure pump which is connected to the interior of the recipient via the liquid transport system. '''Figure 6''' shows the system components relevant for pressure build-up. The desired pressure and the dwell time at this pressure are programmed via the system control display. The pressure is applied at the speed as defined in the program. The run of the pressure curve and the actual pressure can be read directly on the display and on an analog manometer. The cold isostatic press operated on the IEK-1 is designed for a maximum pressure of 4400 bar (440 MPa). To be on the safe side, the pressure in standard operation of the system should not exceed 4000 bar (400 MPa). The system is equipped with a rupture disc as overpressure protection. The rupture disc protects the system from uncontrolled failure and is designed with a safety factor of 1.1 based on the maximum pressure.

[[File:Wiki Keramik KIP Abb 06.jpg|thumb|center]]
'''Figure 6:''' ''a.) Programming of the pressing process via the display b.) Indication of the pressure via the manometer c.) Rupture disc as protection against overpressure.''

vi.) '''Decompression:''' Decompression is the most critical step in cold isostatic pressing. If there is still air in the sample after the sample preparation, it is strongly compressed during the CIP cycle. The high compression of the powder compact is associated with a strong reduction in the residual porosity. Accordingly, after pressing, there is a high flow resistance for the compressed air to escape and the pressure release takes a certain amount of time (up to a few minutes, depending on the pressing density achieved). If the pressure is released suddenly, this can lead to failure of the compact by severe cracking. It should be noted that a powder compact is also deformed elastically in addition to plastic deformation. When the pressure is released, there is therefore an elastic rebound of the pressed part ("spring-back" effect), which can be between 0.5 - 2%. Since the compression takes place in an elastic mold, the spring-back is viewed as less critical, but in the worst case it can also lead to damage to the pressed part, e.g. if it sticks to the die wall.

The decompression at the laboratory facility of the IEK-1 institute (type CIP 400-125 * 300Y, EPSI, Belgium) is initiated by opening a pneumatic high-pressure valve. The pressure release can then be regulated either manually via a valve or via an adjustable throttle valve. The throttle valve consists of a high pressure tube in which a needle is inserted. The decompression speed is controlled by the inner diameter of the tube and the position and thickness of the needle. '''Figure 7''' shows the display for initiating decompression and the throttle valve, which is located on the rear of the cold isostatic press.

[[File:Wiki Keramik KIP Abb 07.jpg|thumb|center]]
'''Figure 7:''' ''a.) Display for selecting the decompression mode b.) Throttle valve.''

After the pressure has been completely released, the system can be opened as already described under i.). Afterwards, the metal cage together with the sample can be removed. After removing the elastic foil, the sample is ready for use.

== Applications of cold isostatic pressing ==

Cold isostatic pressing is widely used in industry as well as in research and development. One advantage is the great flexibility of the method and the comparatively low costs for the die production. Cold isostatic pressing can be used universally for the compression of oxides, nitrides, borides, graphite, hard metals and other composite materials, as well as for metallic powders. The starting powder should have good compressibility, since the use of high proportions of binder is rather unusual with this method. In general, this method is used to manufacture semi-finished products as well as structural and functional components with moderate geometrical complexity. Specific application examples are spark plug insulators made of alumina, cap insulators, components for lambda sensors, semi-finished products for ceramic insulators and semi-finished products for ceramic balls. Metallic filter cartridges with a length of up to 1.8 m and a diameter of up to 300 mm are also manufactured using this process.

Cold isostatic pressing

2021-08-04T11:25:41Z

M.bram: /* General principle of cold isostatic pressing (CIP) */

== General principle of cold isostatic pressing (CIP) ==

The cold isostatic pressing CIP is based on the effect that a pressure applied to a liquid spreads evenly in all directions (so-called Pascal's principle). Inside the liquid, this leads to a homogeneous pressure distribution, which can be used for shaping ceramic and metallic powders if the powder is encapsulated in an elastic die. Elastic polymers (elastomers) such as polyurethane (PU), polyvinyl chloride (PVC), synthetic or natural rubber have proven successful as materials for the elastic die. The main components of a cold isostatic press are the recipient filled with the pressure transmission medium, the high-pressure pump, the locking system, the overpressure protection and the system control. The recipient is a pressure cylinder, which consists of either a high-strength, thick-walled steel cylinder or a thin-walled steel vessel with a pre-tensioned wire winding. '''Figure 1''' shows a cold isostatic press in lab scale.

The pressure transmission media used are preferably water with the addition of an anti-corrosion agent, oil-water emulsions or glycerine. A hydraulic unit like an axial piston pump is used to build up pressure. This unit is connected to the recipient via a fluid transport system with appropriate valves and throttles. The pressure cylinder is sealed, for example, by a polymer O-ring that is integrated into the cover plate and is pressed into a groove when the pressure is built up. In order to absorb the large forces in the axial direction, the cover plate of the recipient is usually supported by a massive yoke. A rupture disc is used to protect against overpressure, which fails when the critical pressure is exceeded and thus enables a regulated pressure release before irreversible damage to the recipient occurs. Cold isostatic pressing is carried out in most cases at room temperature. In specially designed presses, moderate heating of the pressure medium up to a maximum temperature of 300 °C is possible.

In technical practice, a distinction is made between two basic principles of cold isostatic pressing, the wet bag process and the dry bag process. In addition, the wet bag process can also be used for the post-compaction of components uniaxial pre-pressed in a rigid form. The three variants are explained in more detail below:

i.) '''Wet bag process:''' In the wet bag process, the die is a self-supporting, elastic hollow mold that is filled with the powder outside the cold isostatic press. Optionally, a metallic mandrel can be integrated into the hollow mold for the production of pipes. After filling, the die is closed with an elastic cover plate. In order to protect the interior of the die against the ingress of liquid, the die can also be enveloped with an elastic foil, which is then evacuated and sealed in a liquid-tight manner. The wet bag process is often used in research and development due to its great flexibility with regard to the system parameters (including pressures up to approx. 400 MPa), the component geometries and the number of components per cycle. It is also used in industry for the production of large-volume components (e.g. filter candles) and semi-finished products (e.g. for manufacturing of ceramic insulators) with dimensions up to the meter range. Disadvantages of the wet bag process are the limited dimensional accuracy due to the elastic die and the comparatively long cycle times of several minutes.

ii.) '''Dry bag process:''' In dry bag pressing, the elastic die is firmly fixed to the recipient. Correspondingly, the mold filling takes place inside the cold isostatic press. The main advantages compared to wet bag pressing are the possibility of full automation, fast cycle times in the range of 10 s - 100 s depending on the component size (increase in cycle time with component size) and better dimensional accuracy. However, it should be noted that in the area of fixing the elastic die to the recipient there are restrictions with regard to the homogeneity of the pressure distribution, which, however, are less relevant for simpler geometries such as plates, cylinders or tubes. Dry die pressing is preferred in industrial production. The best-known application example are spark plug insulators, which are manufactured in a fully automated manner in quantities of millions.

iii.) '''Post-compaction of uniaxially pressed components:''' The shaping of ceramic and metallic powders via the uniaxial pressing in rigid molds is restricted by the wall friction, which leads to increasing density gradients in the component with increasing height/diameter ratio. The result is an inhomogeneous shrinkage during the subsequent sintering. In order to use the advantages of uniaxial pressing in terms of dimensional accuracy and at the same time to achieve a homogeneous density distribution in the component, it is possible to pre-press components uniaxially in a rigid die at moderate pressures, e.g. in the range of 50 - 100 MPa, and then post-compact them using cold isostatic pressing, which can be done e.g. at pressures in the range of 300 - 400 MPa. For the pressure transfer, the component must be liquid-tight welded into an elastic foil. When welding the foil, it must made sure that the foil is not damaged by sharp edges or particles.

[[File:Wiki Keramik KIP Abb 01.jpg|thumb|center]]
'''Figure 1:''' Cold isostatic press on a laboratory scale operated at the institute IEK-1, Forschungszentrum Jülich (manufacturer EPSI, type CIP 400-125 * 300Y). Usable volume: Diameter 125 mm, height = 300 mm. 

== Advantages and limitations of cold isostatic pressing ==

i.) '''Advantages:''' The main advantage of cold isostatic pressing is the elimination of friction-related variation in density, such as occurring in the case of uniaxial pressing in rigid molds. Therefore, higher green densities, higher green strengths and more homogeneous structures can be achieved with cold isostatic pressing. For example, press-related textures in the structure can be avoided to a large extent. Furthermore, components with a height / diameter ratio greater than 3: 1 (usually specified as limit for uniaxial pressing) can be produced relatively easily. Because there is no wall friction, it is possible to omit dispense with lubricants during pressing and the required proportion of other pressing additives can be significantly reduced. Furthermore, ceramic feedstocks can be compacted that contain abrasive solid particles that would lead to high tool wear in the case of uniaxial pressing.

ii.) '''Limits:''' Cold isostatic pressing is only suitable for relatively simple component geometries and is therefore restricted with respect to near-net-shape production. Due to the elastic properties of the die, there are limitations with regard to dimensional accuracy even with simpler geometries. Furthermore, the surface roughness is usually also relatively high, since the die wall yields elastically during pressing. Furthermore, sharp-edged particles can be pressed into the die wall, whereby the die is damaged in the worst case and demolding is aggravated. In order to increase the dimensional accuracy, mechanical post-processing of the cold isostatically pressed semi-finished products (so-called green machining) is often carried out. The relatively high green strength of cold isostatically pressed semi-finished products has a positive effect here.

== How to conduct a cold isostatic pressing cycle ==

In the following, it is explained in detail which processing steps are carried out in cold isostatic pressing and what must be considered in order to obtain crack-free samples and avoid damage to the system. The processing steps shown were carried out in a cold isostatic laboratory press of the following type:

Type: CIP 400-125*300Y
Manufacturer: EPSI, Temse, Belgien
Material of recipient SA 723 Class 3
Recipient inner diameter: 125 mm
Recipient inner height: 300 mm
Maximum sample size: limited by recipient volume
Maximum filling height: 295 mm
Recipient volume: 3.7 Liter
Nominal operating pressure: 4000 bar (400 MPa)
Maximum operating pressure: 4400 bar (440 MPa)
Safety factor: 1,1 (related to 4840 bar, 484 MPa)

i.) '''Encapsulation of the samples:''' Even with cold isostatic pressing, a uniform filling of the mold and a high filling density are basic requirements for successful compaction of the powder. In order to estimate the flowability of the powder, it is recommended to measure the bulk and tap density in accordance with DIN ISO 3923 and DIN ISO 3953. The flowability of a powder can be improved by granulating in a fluidizing bed or by spray drying. During granulation, spherical, easily flowable agglomerates are formed, which have a relatively low stability and are destroyed during the cold isostatic pressing. Some powder manufacturers offer powder directly in a granulated state. In order to increase the bulk density in the mold, the elastic die can optionally be vibrated or subjected to ultrasonic treatment. As an example, Figure 2 shows a simple elastic mold made of rubber for cold isostatic pressing of round bars.

[[File:Wiki Keramik KIP Abb 02.jpg|thumb|center]]
'''Figure 2:''' ''Elastic mold (rubber tube with cover plug) for cold isostatic pressing of round bars.
'' 

As mentioned above, there is also the possibility of post-compaction of uniaxially pressed semi-finished parts using cold isostatic pressing. Figure 3 shows how the welding of a pre-pressed part into an elastic foil can be carried out. For this purpose, at the IEK-1 institute, a vacuum sealer is used, which is usually applied in the household for sealing and freezing food. Elastic foils, which are established for this purpose, are suitable for encapsulation of pre-pressed parts in cold isostatic pressing as well. The sample is placed in the prepared bag, then interior is evacuated and the bag is finally liquid-tight welded. A more primitive alternative is to put the sample in a latex glove, which is evacuated, for example, by a water jet pump and sealed with a string.

[[File:Wiki Keramik KIP Abb 03.jpg|thumb|center]]
'''Figure 3:''' ''Sealing of a uniaxially pre-pressed sample in an elastic foil using a household vacuum sealer a.) Insertion of the uniaxially pre-pressed sample b.) Evacuation c.) Liquid-tight sealed sample.''

ii.) '''Opening the recipient:''' Figure 4 shows the individual steps for opening the recipient of the cold isostatic press of the type CIP 400-125 * 300Y (EPSI, Belgium). The press is equipped with a hydraulic lifting device. A screw is attached to this, via which the cover plate is connected to the hydraulic lifting device. The screw is protected from damage by a cage. After the screw has been attached, the cover is lifted using the lifting device. The sealing ring can be seen on the lower edge of the cover plate. This ring is pressed into the groove when the pressure is built up.

iii.) '''Introducing the sample into the recipient:''' For safety reasons it is important that the welded sample is not positioned directly in the oil-water emulsion. In the worst case, the sample or parts of the elastic foil can get into the liquid transport system of the cold isostatic press and block it, so that a pressure reduction is no longer possible and a service technician has to be called in. To safely avoid this risk, the sample must be placed in the oil-water emulsion in a specifically designed metal cage shown in Figure 4f. Spacers are welded onto the underpart of the metal cage, which prevent the metal mesh from resting directly on the bottom of the recipient. In this way, an unhindered pressure build-up and release is ensured. The metal cage also makes it easier to remove the sample after the cycle from the oil-water emulsion.

[[File:Wiki Keramik CIP Fig 04 english.jpg|thumb|center]]
'''Figure 4:''' ''Preparation of the system for the CIP cycle a.) Closed system b.) Attaching the screw to the cover plate c.) Starting the opening process d.) Open system e.) View on the oil-water emulsion f.) Metal cage for placing the encapsulated sample in the CIP device.''

iv.) '''Closing the recipient:''' After installing the metal cage including the sample in the recipient, the cover plate is closed via the hydraulic lifting system and the screw for fixing the cover plate is removed. The yoke, which absorbs the pressure in the axial direction, is then positioned over the cover plate. A specially designed locking system guarantees the exact position of the yoke in relation to the recipient. The locking bar is manually locked in the pressing position with a lever. Figure 5 shows the individual steps for closing the recipient.

[[File:Wiki Keramik KIP Abb 05.jpg|thumb|center]]
'''Figure 5:''' ''a., b.) Closing the recipient using the hydraulic lifting device c.) Locking the yoke before starting the pressing cycle.''

v.) '''Pressure build-up and dwell time, protection against overpressure:''' As mentioned at the beginning, the pressure build-up takes place by a high-pressure pump which is connected to the interior of the recipient via the liquid transport system. Figure 6 shows the system components relevant for pressure build-up. The desired pressure and the dwell time at this pressure are programmed via the system control display. The pressure is applied at the speed as defined in the program. The run of the pressure curve and the actual pressure can be read directly on the display and on an analog manometer. The cold isostatic press operated on the IEK-1 is designed for a maximum pressure of 4400 bar (440 MPa). To be on the safe side, the pressure in standard operation of the system should not exceed 4000 bar (400 MPa). The system is equipped with a rupture disc as overpressure protection. The rupture disc protects the system from uncontrolled failure and is designed with a safety factor of 1.1 based on the maximum pressure.

[[File:Wiki Keramik KIP Abb 06.jpg|thumb|center]]
'''Figure 6:''' ''a.) Programming of the pressing process via the display b.) Indication of the pressure via the manometer c.) Rupture disc as protection against overpressure.''

vi.) '''Decompression:''' Decompression is the most critical step in cold isostatic pressing. If there is still air in the sample after the sample preparation, it is strongly compressed during the CIP cycle. The high compression of the powder compact is associated with a strong reduction in the residual porosity. Accordingly, after pressing, there is a high flow resistance for the compressed air to escape and the pressure release takes a certain amount of time (up to a few minutes, depending on the pressing density achieved). If the pressure is released suddenly, this can lead to failure of the compact by severe cracking. It should be noted that a powder compact is also deformed elastically in addition to plastic deformation. When the pressure is released, there is therefore an elastic rebound of the pressed part ("spring-back" effect), which can be between 0.5 - 2%. Since the compression takes place in an elastic mold, the spring-back is viewed as less critical, but in the worst case it can also lead to damage to the pressed part, e.g. if it sticks to the die wall.

The decompression at the laboratory facility of the IEK-1 institute (type CIP 400-125 * 300Y, EPSI, Belgium) is initiated by opening a pneumatic high-pressure valve. The pressure release can then be regulated either manually via a valve or via an adjustable throttle valve. The throttle valve consists of a high pressure tube in which a needle is inserted. The decompression speed is controlled by the inner diameter of the tube and the position and thickness of the needle. Figure 7 shows the display for initiating decompression and the throttle valve, which is located on the rear of the cold isostatic press.

[[File:Wiki Keramik KIP Abb 07.jpg|thumb|center]]
'''Figure 7:''' ''a.) Display for selecting the decompression mode b.) Throttle valve.''

After the pressure has been completely released, the system can be opened as already described under i.). Afterwards, the metal cage together with the sample can be removed. After removing the elastic foil, the sample is ready for use.

== Applications of cold isostatic pressing ==

Cold isostatic pressing is widely used in industry as well as in research and development. One advantage is the great flexibility of the method and the comparatively low costs for the die production. Cold isostatic pressing can be used universally for the compression of oxides, nitrides, borides, graphite, hard metals and other composite materials, as well as for metallic powders. The starting powder should have good compressibility, since the use of high proportions of binder is rather unusual with this method. In general, this method is used to manufacture semi-finished products as well as structural and functional components with moderate geometrical complexity. Specific application examples are spark plug insulators made of alumina, cap insulators, components for lambda sensors, semi-finished products for ceramic insulators and semi-finished products for ceramic balls. Metallic filter cartridges with a length of up to 1.8 m and a diameter of up to 300 mm are also manufactured using this process.

Cold isostatic pressing

2021-08-04T11:24:17Z

M.bram: /* Applications of cold isostatic pressing */

== General principle of cold isostatic pressing (CIP) ==

The cold isostatic pressing CIP is based on the effect that a pressure applied to a liquid spreads evenly in all directions (so-called Pascal's principle). Inside the liquid, this leads to a homogeneous pressure distribution, which can be used for shaping ceramic and metallic powders if the powder is encapsulated in an elastic die. Elastic polymers (elastomers) such as polyurethane (PU), polyvinyl chloride (PVC), synthetic or natural rubber have proven successful as materials for the elastic die. The main components of a cold isostatic press are the recipient filled with the pressure transmission medium, the high-pressure pump, the locking system, the overpressure protection and the system control. The recipient is a pressure cylinder, which consists of either a high-strength, thick-walled steel cylinder or a thin-walled steel vessel with a pre-tensioned wire winding.

The pressure transmission media used are preferably water with the addition of an anti-corrosion agent, oil-water emulsions or glycerine. A hydraulic unit like an axial piston pump is used to build up pressure. This unit is connected to the recipient via a fluid transport system with appropriate valves and throttles. The pressure cylinder is sealed, for example, by a polymer O-ring that is integrated into the cover plate and is pressed into a groove when the pressure is built up. In order to absorb the large forces in the axial direction, the cover plate of the recipient is usually supported by a massive yoke. A rupture disc is used to protect against overpressure, which fails when the critical pressure is exceeded and thus enables a regulated pressure release before irreversible damage to the recipient occurs. Cold isostatic pressing is carried out in most cases at room temperature. In specially designed presses, moderate heating of the pressure medium up to a maximum temperature of 300 °C is possible.

In technical practice, a distinction is made between two basic principles of cold isostatic pressing, the wet bag process and the dry bag process. In addition, the wet bag process can also be used for the post-compaction of components uniaxial pre-pressed in a rigid form. The three variants are explained in more detail below:

i.) '''Wet bag process:''' In the wet bag process, the die is a self-supporting, elastic hollow mold that is filled with the powder outside the cold isostatic press. Optionally, a metallic mandrel can be integrated into the hollow mold for the production of pipes. After filling, the die is closed with an elastic cover plate. In order to protect the interior of the die against the ingress of liquid, the die can also be enveloped with an elastic foil, which is then evacuated and sealed in a liquid-tight manner. The wet bag process is often used in research and development due to its great flexibility with regard to the system parameters (including pressures up to approx. 400 MPa), the component geometries and the number of components per cycle. It is also used in industry for the production of large-volume components (e.g. filter candles) and semi-finished products (e.g. for manufacturing of ceramic insulators) with dimensions up to the meter range. Disadvantages of the wet bag process are the limited dimensional accuracy due to the elastic die and the comparatively long cycle times of several minutes.

ii.) '''Dry bag process:''' In dry bag pressing, the elastic die is firmly fixed to the recipient. Correspondingly, the mold filling takes place inside the cold isostatic press. The main advantages compared to wet bag pressing are the possibility of full automation, fast cycle times in the range of 10 s - 100 s depending on the component size (increase in cycle time with component size) and better dimensional accuracy. However, it should be noted that in the area of fixing the elastic die to the recipient there are restrictions with regard to the homogeneity of the pressure distribution, which, however, are less relevant for simpler geometries such as plates, cylinders or tubes. Dry die pressing is preferred in industrial production. The best-known application example are spark plug insulators, which are manufactured in a fully automated manner in quantities of millions.

iii.) '''Post-compaction of uniaxially pressed components:''' The shaping of ceramic and metallic powders via the uniaxial pressing in rigid molds is restricted by the wall friction, which leads to increasing density gradients in the component with increasing height/diameter ratio. The result is an inhomogeneous shrinkage during the subsequent sintering. In order to use the advantages of uniaxial pressing in terms of dimensional accuracy and at the same time to achieve a homogeneous density distribution in the component, it is possible to pre-press components uniaxially in a rigid die at moderate pressures, e.g. in the range of 50 - 100 MPa, and then post-compact them using cold isostatic pressing, which can be done e.g. at pressures in the range of 300 - 400 MPa. For the pressure transfer, the component must be liquid-tight welded into an elastic foil. When welding the foil, it must made sure that the foil is not damaged by sharp edges or particles.

[[File:Wiki Keramik KIP Abb 01.jpg|thumb|center]]
'''Figure 1:''' Cold isostatic press on a laboratory scale operated at the institute IEK-1, Forschungszentrum Jülich (manufacturer EPSI, type CIP 400-125 * 300Y). Usable volume: Diameter 125 mm, height = 300 mm. 

== Advantages and limitations of cold isostatic pressing ==

i.) '''Advantages:''' The main advantage of cold isostatic pressing is the elimination of friction-related variation in density, such as occurring in the case of uniaxial pressing in rigid molds. Therefore, higher green densities, higher green strengths and more homogeneous structures can be achieved with cold isostatic pressing. For example, press-related textures in the structure can be avoided to a large extent. Furthermore, components with a height / diameter ratio greater than 3: 1 (usually specified as limit for uniaxial pressing) can be produced relatively easily. Because there is no wall friction, it is possible to omit dispense with lubricants during pressing and the required proportion of other pressing additives can be significantly reduced. Furthermore, ceramic feedstocks can be compacted that contain abrasive solid particles that would lead to high tool wear in the case of uniaxial pressing.

ii.) '''Limits:''' Cold isostatic pressing is only suitable for relatively simple component geometries and is therefore restricted with respect to near-net-shape production. Due to the elastic properties of the die, there are limitations with regard to dimensional accuracy even with simpler geometries. Furthermore, the surface roughness is usually also relatively high, since the die wall yields elastically during pressing. Furthermore, sharp-edged particles can be pressed into the die wall, whereby the die is damaged in the worst case and demolding is aggravated. In order to increase the dimensional accuracy, mechanical post-processing of the cold isostatically pressed semi-finished products (so-called green machining) is often carried out. The relatively high green strength of cold isostatically pressed semi-finished products has a positive effect here.

== How to conduct a cold isostatic pressing cycle ==

In the following, it is explained in detail which processing steps are carried out in cold isostatic pressing and what must be considered in order to obtain crack-free samples and avoid damage to the system. The processing steps shown were carried out in a cold isostatic laboratory press of the following type:

Type: CIP 400-125*300Y
Manufacturer: EPSI, Temse, Belgien
Material of recipient SA 723 Class 3
Recipient inner diameter: 125 mm
Recipient inner height: 300 mm
Maximum sample size: limited by recipient volume
Maximum filling height: 295 mm
Recipient volume: 3.7 Liter
Nominal operating pressure: 4000 bar (400 MPa)
Maximum operating pressure: 4400 bar (440 MPa)
Safety factor: 1,1 (related to 4840 bar, 484 MPa)

i.) '''Encapsulation of the samples:''' Even with cold isostatic pressing, a uniform filling of the mold and a high filling density are basic requirements for successful compaction of the powder. In order to estimate the flowability of the powder, it is recommended to measure the bulk and tap density in accordance with DIN ISO 3923 and DIN ISO 3953. The flowability of a powder can be improved by granulating in a fluidizing bed or by spray drying. During granulation, spherical, easily flowable agglomerates are formed, which have a relatively low stability and are destroyed during the cold isostatic pressing. Some powder manufacturers offer powder directly in a granulated state. In order to increase the bulk density in the mold, the elastic die can optionally be vibrated or subjected to ultrasonic treatment. As an example, Figure 2 shows a simple elastic mold made of rubber for cold isostatic pressing of round bars.

[[File:Wiki Keramik KIP Abb 02.jpg|thumb|center]]
'''Figure 2:''' ''Elastic mold (rubber tube with cover plug) for cold isostatic pressing of round bars.
'' 

As mentioned above, there is also the possibility of post-compaction of uniaxially pressed semi-finished parts using cold isostatic pressing. Figure 3 shows how the welding of a pre-pressed part into an elastic foil can be carried out. For this purpose, at the IEK-1 institute, a vacuum sealer is used, which is usually applied in the household for sealing and freezing food. Elastic foils, which are established for this purpose, are suitable for encapsulation of pre-pressed parts in cold isostatic pressing as well. The sample is placed in the prepared bag, then interior is evacuated and the bag is finally liquid-tight welded. A more primitive alternative is to put the sample in a latex glove, which is evacuated, for example, by a water jet pump and sealed with a string.

[[File:Wiki Keramik KIP Abb 03.jpg|thumb|center]]
'''Figure 3:''' ''Sealing of a uniaxially pre-pressed sample in an elastic foil using a household vacuum sealer a.) Insertion of the uniaxially pre-pressed sample b.) Evacuation c.) Liquid-tight sealed sample.''

ii.) '''Opening the recipient:''' Figure 4 shows the individual steps for opening the recipient of the cold isostatic press of the type CIP 400-125 * 300Y (EPSI, Belgium). The press is equipped with a hydraulic lifting device. A screw is attached to this, via which the cover plate is connected to the hydraulic lifting device. The screw is protected from damage by a cage. After the screw has been attached, the cover is lifted using the lifting device. The sealing ring can be seen on the lower edge of the cover plate. This ring is pressed into the groove when the pressure is built up.

iii.) '''Introducing the sample into the recipient:''' For safety reasons it is important that the welded sample is not positioned directly in the oil-water emulsion. In the worst case, the sample or parts of the elastic foil can get into the liquid transport system of the cold isostatic press and block it, so that a pressure reduction is no longer possible and a service technician has to be called in. To safely avoid this risk, the sample must be placed in the oil-water emulsion in a specifically designed metal cage shown in Figure 4f. Spacers are welded onto the underpart of the metal cage, which prevent the metal mesh from resting directly on the bottom of the recipient. In this way, an unhindered pressure build-up and release is ensured. The metal cage also makes it easier to remove the sample after the cycle from the oil-water emulsion.

[[File:Wiki Keramik CIP Fig 04 english.jpg|thumb|center]]
'''Figure 4:''' ''Preparation of the system for the CIP cycle a.) Closed system b.) Attaching the screw to the cover plate c.) Starting the opening process d.) Open system e.) View on the oil-water emulsion f.) Metal cage for placing the encapsulated sample in the CIP device.''

iv.) '''Closing the recipient:''' After installing the metal cage including the sample in the recipient, the cover plate is closed via the hydraulic lifting system and the screw for fixing the cover plate is removed. The yoke, which absorbs the pressure in the axial direction, is then positioned over the cover plate. A specially designed locking system guarantees the exact position of the yoke in relation to the recipient. The locking bar is manually locked in the pressing position with a lever. Figure 5 shows the individual steps for closing the recipient.

[[File:Wiki Keramik KIP Abb 05.jpg|thumb|center]]
'''Figure 5:''' ''a., b.) Closing the recipient using the hydraulic lifting device c.) Locking the yoke before starting the pressing cycle.''

v.) '''Pressure build-up and dwell time, protection against overpressure:''' As mentioned at the beginning, the pressure build-up takes place by a high-pressure pump which is connected to the interior of the recipient via the liquid transport system. Figure 6 shows the system components relevant for pressure build-up. The desired pressure and the dwell time at this pressure are programmed via the system control display. The pressure is applied at the speed as defined in the program. The run of the pressure curve and the actual pressure can be read directly on the display and on an analog manometer. The cold isostatic press operated on the IEK-1 is designed for a maximum pressure of 4400 bar (440 MPa). To be on the safe side, the pressure in standard operation of the system should not exceed 4000 bar (400 MPa). The system is equipped with a rupture disc as overpressure protection. The rupture disc protects the system from uncontrolled failure and is designed with a safety factor of 1.1 based on the maximum pressure.

[[File:Wiki Keramik KIP Abb 06.jpg|thumb|center]]
'''Figure 6:''' ''a.) Programming of the pressing process via the display b.) Indication of the pressure via the manometer c.) Rupture disc as protection against overpressure.''

vi.) '''Decompression:''' Decompression is the most critical step in cold isostatic pressing. If there is still air in the sample after the sample preparation, it is strongly compressed during the CIP cycle. The high compression of the powder compact is associated with a strong reduction in the residual porosity. Accordingly, after pressing, there is a high flow resistance for the compressed air to escape and the pressure release takes a certain amount of time (up to a few minutes, depending on the pressing density achieved). If the pressure is released suddenly, this can lead to failure of the compact by severe cracking. It should be noted that a powder compact is also deformed elastically in addition to plastic deformation. When the pressure is released, there is therefore an elastic rebound of the pressed part ("spring-back" effect), which can be between 0.5 - 2%. Since the compression takes place in an elastic mold, the spring-back is viewed as less critical, but in the worst case it can also lead to damage to the pressed part, e.g. if it sticks to the die wall.

The decompression at the laboratory facility of the IEK-1 institute (type CIP 400-125 * 300Y, EPSI, Belgium) is initiated by opening a pneumatic high-pressure valve. The pressure release can then be regulated either manually via a valve or via an adjustable throttle valve. The throttle valve consists of a high pressure tube in which a needle is inserted. The decompression speed is controlled by the inner diameter of the tube and the position and thickness of the needle. Figure 7 shows the display for initiating decompression and the throttle valve, which is located on the rear of the cold isostatic press.

[[File:Wiki Keramik KIP Abb 07.jpg|thumb|center]]
'''Figure 7:''' ''a.) Display for selecting the decompression mode b.) Throttle valve.''

After the pressure has been completely released, the system can be opened as already described under i.). Afterwards, the metal cage together with the sample can be removed. After removing the elastic foil, the sample is ready for use.

== Applications of cold isostatic pressing ==

Cold isostatic pressing is widely used in industry as well as in research and development. One advantage is the great flexibility of the method and the comparatively low costs for the die production. Cold isostatic pressing can be used universally for the compression of oxides, nitrides, borides, graphite, hard metals and other composite materials, as well as for metallic powders. The starting powder should have good compressibility, since the use of high proportions of binder is rather unusual with this method. In general, this method is used to manufacture semi-finished products as well as structural and functional components with moderate geometrical complexity. Specific application examples are spark plug insulators made of alumina, cap insulators, components for lambda sensors, semi-finished products for ceramic insulators and semi-finished products for ceramic balls. Metallic filter cartridges with a length of up to 1.8 m and a diameter of up to 300 mm are also manufactured using this process.

Cold isostatic pressing

2021-08-04T11:23:09Z

M.bram:

== General principle of cold isostatic pressing (CIP) ==

The cold isostatic pressing CIP is based on the effect that a pressure applied to a liquid spreads evenly in all directions (so-called Pascal's principle). Inside the liquid, this leads to a homogeneous pressure distribution, which can be used for shaping ceramic and metallic powders if the powder is encapsulated in an elastic die. Elastic polymers (elastomers) such as polyurethane (PU), polyvinyl chloride (PVC), synthetic or natural rubber have proven successful as materials for the elastic die. The main components of a cold isostatic press are the recipient filled with the pressure transmission medium, the high-pressure pump, the locking system, the overpressure protection and the system control. The recipient is a pressure cylinder, which consists of either a high-strength, thick-walled steel cylinder or a thin-walled steel vessel with a pre-tensioned wire winding.

The pressure transmission media used are preferably water with the addition of an anti-corrosion agent, oil-water emulsions or glycerine. A hydraulic unit like an axial piston pump is used to build up pressure. This unit is connected to the recipient via a fluid transport system with appropriate valves and throttles. The pressure cylinder is sealed, for example, by a polymer O-ring that is integrated into the cover plate and is pressed into a groove when the pressure is built up. In order to absorb the large forces in the axial direction, the cover plate of the recipient is usually supported by a massive yoke. A rupture disc is used to protect against overpressure, which fails when the critical pressure is exceeded and thus enables a regulated pressure release before irreversible damage to the recipient occurs. Cold isostatic pressing is carried out in most cases at room temperature. In specially designed presses, moderate heating of the pressure medium up to a maximum temperature of 300 °C is possible.

In technical practice, a distinction is made between two basic principles of cold isostatic pressing, the wet bag process and the dry bag process. In addition, the wet bag process can also be used for the post-compaction of components uniaxial pre-pressed in a rigid form. The three variants are explained in more detail below:

i.) '''Wet bag process:''' In the wet bag process, the die is a self-supporting, elastic hollow mold that is filled with the powder outside the cold isostatic press. Optionally, a metallic mandrel can be integrated into the hollow mold for the production of pipes. After filling, the die is closed with an elastic cover plate. In order to protect the interior of the die against the ingress of liquid, the die can also be enveloped with an elastic foil, which is then evacuated and sealed in a liquid-tight manner. The wet bag process is often used in research and development due to its great flexibility with regard to the system parameters (including pressures up to approx. 400 MPa), the component geometries and the number of components per cycle. It is also used in industry for the production of large-volume components (e.g. filter candles) and semi-finished products (e.g. for manufacturing of ceramic insulators) with dimensions up to the meter range. Disadvantages of the wet bag process are the limited dimensional accuracy due to the elastic die and the comparatively long cycle times of several minutes.

ii.) '''Dry bag process:''' In dry bag pressing, the elastic die is firmly fixed to the recipient. Correspondingly, the mold filling takes place inside the cold isostatic press. The main advantages compared to wet bag pressing are the possibility of full automation, fast cycle times in the range of 10 s - 100 s depending on the component size (increase in cycle time with component size) and better dimensional accuracy. However, it should be noted that in the area of fixing the elastic die to the recipient there are restrictions with regard to the homogeneity of the pressure distribution, which, however, are less relevant for simpler geometries such as plates, cylinders or tubes. Dry die pressing is preferred in industrial production. The best-known application example are spark plug insulators, which are manufactured in a fully automated manner in quantities of millions.

iii.) '''Post-compaction of uniaxially pressed components:''' The shaping of ceramic and metallic powders via the uniaxial pressing in rigid molds is restricted by the wall friction, which leads to increasing density gradients in the component with increasing height/diameter ratio. The result is an inhomogeneous shrinkage during the subsequent sintering. In order to use the advantages of uniaxial pressing in terms of dimensional accuracy and at the same time to achieve a homogeneous density distribution in the component, it is possible to pre-press components uniaxially in a rigid die at moderate pressures, e.g. in the range of 50 - 100 MPa, and then post-compact them using cold isostatic pressing, which can be done e.g. at pressures in the range of 300 - 400 MPa. For the pressure transfer, the component must be liquid-tight welded into an elastic foil. When welding the foil, it must made sure that the foil is not damaged by sharp edges or particles.

[[File:Wiki Keramik KIP Abb 01.jpg|thumb|center]]
'''Figure 1:''' Cold isostatic press on a laboratory scale operated at the institute IEK-1, Forschungszentrum Jülich (manufacturer EPSI, type CIP 400-125 * 300Y). Usable volume: Diameter 125 mm, height = 300 mm. 

== Advantages and limitations of cold isostatic pressing ==

i.) '''Advantages:''' The main advantage of cold isostatic pressing is the elimination of friction-related variation in density, such as occurring in the case of uniaxial pressing in rigid molds. Therefore, higher green densities, higher green strengths and more homogeneous structures can be achieved with cold isostatic pressing. For example, press-related textures in the structure can be avoided to a large extent. Furthermore, components with a height / diameter ratio greater than 3: 1 (usually specified as limit for uniaxial pressing) can be produced relatively easily. Because there is no wall friction, it is possible to omit dispense with lubricants during pressing and the required proportion of other pressing additives can be significantly reduced. Furthermore, ceramic feedstocks can be compacted that contain abrasive solid particles that would lead to high tool wear in the case of uniaxial pressing.

ii.) '''Limits:''' Cold isostatic pressing is only suitable for relatively simple component geometries and is therefore restricted with respect to near-net-shape production. Due to the elastic properties of the die, there are limitations with regard to dimensional accuracy even with simpler geometries. Furthermore, the surface roughness is usually also relatively high, since the die wall yields elastically during pressing. Furthermore, sharp-edged particles can be pressed into the die wall, whereby the die is damaged in the worst case and demolding is aggravated. In order to increase the dimensional accuracy, mechanical post-processing of the cold isostatically pressed semi-finished products (so-called green machining) is often carried out. The relatively high green strength of cold isostatically pressed semi-finished products has a positive effect here.

== How to conduct a cold isostatic pressing cycle ==

In the following, it is explained in detail which processing steps are carried out in cold isostatic pressing and what must be considered in order to obtain crack-free samples and avoid damage to the system. The processing steps shown were carried out in a cold isostatic laboratory press of the following type:

Type: CIP 400-125*300Y
Manufacturer: EPSI, Temse, Belgien
Material of recipient SA 723 Class 3
Recipient inner diameter: 125 mm
Recipient inner height: 300 mm
Maximum sample size: limited by recipient volume
Maximum filling height: 295 mm
Recipient volume: 3.7 Liter
Nominal operating pressure: 4000 bar (400 MPa)
Maximum operating pressure: 4400 bar (440 MPa)
Safety factor: 1,1 (related to 4840 bar, 484 MPa)

i.) '''Encapsulation of the samples:''' Even with cold isostatic pressing, a uniform filling of the mold and a high filling density are basic requirements for successful compaction of the powder. In order to estimate the flowability of the powder, it is recommended to measure the bulk and tap density in accordance with DIN ISO 3923 and DIN ISO 3953. The flowability of a powder can be improved by granulating in a fluidizing bed or by spray drying. During granulation, spherical, easily flowable agglomerates are formed, which have a relatively low stability and are destroyed during the cold isostatic pressing. Some powder manufacturers offer powder directly in a granulated state. In order to increase the bulk density in the mold, the elastic die can optionally be vibrated or subjected to ultrasonic treatment. As an example, Figure 2 shows a simple elastic mold made of rubber for cold isostatic pressing of round bars.

[[File:Wiki Keramik KIP Abb 02.jpg|thumb|center]]
'''Figure 2:''' ''Elastic mold (rubber tube with cover plug) for cold isostatic pressing of round bars.
'' 

As mentioned above, there is also the possibility of post-compaction of uniaxially pressed semi-finished parts using cold isostatic pressing. Figure 3 shows how the welding of a pre-pressed part into an elastic foil can be carried out. For this purpose, at the IEK-1 institute, a vacuum sealer is used, which is usually applied in the household for sealing and freezing food. Elastic foils, which are established for this purpose, are suitable for encapsulation of pre-pressed parts in cold isostatic pressing as well. The sample is placed in the prepared bag, then interior is evacuated and the bag is finally liquid-tight welded. A more primitive alternative is to put the sample in a latex glove, which is evacuated, for example, by a water jet pump and sealed with a string.

[[File:Wiki Keramik KIP Abb 03.jpg|thumb|center]]
'''Figure 3:''' ''Sealing of a uniaxially pre-pressed sample in an elastic foil using a household vacuum sealer a.) Insertion of the uniaxially pre-pressed sample b.) Evacuation c.) Liquid-tight sealed sample.''

ii.) '''Opening the recipient:''' Figure 4 shows the individual steps for opening the recipient of the cold isostatic press of the type CIP 400-125 * 300Y (EPSI, Belgium). The press is equipped with a hydraulic lifting device. A screw is attached to this, via which the cover plate is connected to the hydraulic lifting device. The screw is protected from damage by a cage. After the screw has been attached, the cover is lifted using the lifting device. The sealing ring can be seen on the lower edge of the cover plate. This ring is pressed into the groove when the pressure is built up.

iii.) '''Introducing the sample into the recipient:''' For safety reasons it is important that the welded sample is not positioned directly in the oil-water emulsion. In the worst case, the sample or parts of the elastic foil can get into the liquid transport system of the cold isostatic press and block it, so that a pressure reduction is no longer possible and a service technician has to be called in. To safely avoid this risk, the sample must be placed in the oil-water emulsion in a specifically designed metal cage shown in Figure 4f. Spacers are welded onto the underpart of the metal cage, which prevent the metal mesh from resting directly on the bottom of the recipient. In this way, an unhindered pressure build-up and release is ensured. The metal cage also makes it easier to remove the sample after the cycle from the oil-water emulsion.

[[File:Wiki Keramik CIP Fig 04 english.jpg|thumb|center]]
'''Figure 4:''' ''Preparation of the system for the CIP cycle a.) Closed system b.) Attaching the screw to the cover plate c.) Starting the opening process d.) Open system e.) View on the oil-water emulsion f.) Metal cage for placing the encapsulated sample in the CIP device.''

iv.) '''Closing the recipient:''' After installing the metal cage including the sample in the recipient, the cover plate is closed via the hydraulic lifting system and the screw for fixing the cover plate is removed. The yoke, which absorbs the pressure in the axial direction, is then positioned over the cover plate. A specially designed locking system guarantees the exact position of the yoke in relation to the recipient. The locking bar is manually locked in the pressing position with a lever. Figure 5 shows the individual steps for closing the recipient.

[[File:Wiki Keramik KIP Abb 05.jpg|thumb|center]]
'''Figure 5:''' ''a., b.) Closing the recipient using the hydraulic lifting device c.) Locking the yoke before starting the pressing cycle.''

v.) '''Pressure build-up and dwell time, protection against overpressure:''' As mentioned at the beginning, the pressure build-up takes place by a high-pressure pump which is connected to the interior of the recipient via the liquid transport system. Figure 6 shows the system components relevant for pressure build-up. The desired pressure and the dwell time at this pressure are programmed via the system control display. The pressure is applied at the speed as defined in the program. The run of the pressure curve and the actual pressure can be read directly on the display and on an analog manometer. The cold isostatic press operated on the IEK-1 is designed for a maximum pressure of 4400 bar (440 MPa). To be on the safe side, the pressure in standard operation of the system should not exceed 4000 bar (400 MPa). The system is equipped with a rupture disc as overpressure protection. The rupture disc protects the system from uncontrolled failure and is designed with a safety factor of 1.1 based on the maximum pressure.

[[File:Wiki Keramik KIP Abb 06.jpg|thumb|center]]
'''Figure 6:''' ''a.) Programming of the pressing process via the display b.) Indication of the pressure via the manometer c.) Rupture disc as protection against overpressure.''

vi.) '''Decompression:''' Decompression is the most critical step in cold isostatic pressing. If there is still air in the sample after the sample preparation, it is strongly compressed during the CIP cycle. The high compression of the powder compact is associated with a strong reduction in the residual porosity. Accordingly, after pressing, there is a high flow resistance for the compressed air to escape and the pressure release takes a certain amount of time (up to a few minutes, depending on the pressing density achieved). If the pressure is released suddenly, this can lead to failure of the compact by severe cracking. It should be noted that a powder compact is also deformed elastically in addition to plastic deformation. When the pressure is released, there is therefore an elastic rebound of the pressed part ("spring-back" effect), which can be between 0.5 - 2%. Since the compression takes place in an elastic mold, the spring-back is viewed as less critical, but in the worst case it can also lead to damage to the pressed part, e.g. if it sticks to the die wall.

The decompression at the laboratory facility of the IEK-1 institute (type CIP 400-125 * 300Y, EPSI, Belgium) is initiated by opening a pneumatic high-pressure valve. The pressure release can then be regulated either manually via a valve or via an adjustable throttle valve. The throttle valve consists of a high pressure tube in which a needle is inserted. The decompression speed is controlled by the inner diameter of the tube and the position and thickness of the needle. Figure 7 shows the display for initiating decompression and the throttle valve, which is located on the rear of the cold isostatic press.

[[File:Wiki Keramik KIP Abb 07.jpg|thumb|center]]
'''Figure 7:''' ''a.) Display for selecting the decompression mode b.) Throttle valve.''

After the pressure has been completely released, the system can be opened as already described under i.). Afterwards, the metal cage together with the sample can be removed. After removing the elastic foil, the sample is ready for use.

== Applications of cold isostatic pressing ==

Cold isostatic pressing

2021-08-04T08:34:24Z

M.bram: /* How to conduct a cold isostatic pressing cycle */

== General principle of cold isostatic pressing (CIP) ==

The cold isostatic pressing CIP is based on the effect that a pressure applied to a liquid spreads evenly in all directions (so-called Pascal's principle). Inside the liquid, this leads to a homogeneous pressure distribution, which can be used for shaping ceramic and metallic powders if the powder is encapsulated in an elastic die. Elastic polymers (elastomers) such as polyurethane (PU), polyvinyl chloride (PVC), synthetic or natural rubber have proven successful as materials for the elastic die. The main components of a cold isostatic press are the recipient filled with the pressure transmission medium, the high-pressure pump, the locking system, the overpressure protection and the system control. The recipient is a pressure cylinder, which consists of either a high-strength, thick-walled steel cylinder or a thin-walled steel vessel with a pre-tensioned wire winding.

The pressure transmission media used are preferably water with the addition of an anti-corrosion agent, oil-water emulsions or glycerine. A hydraulic unit like an axial piston pump is used to build up pressure. This unit is connected to the recipient via a fluid transport system with appropriate valves and throttles. The pressure cylinder is sealed, for example, by a polymer O-ring that is integrated into the cover plate and is pressed into a groove when the pressure is built up. In order to absorb the large forces in the axial direction, the cover plate of the recipient is usually supported by a massive yoke. A rupture disc is used to protect against overpressure, which fails when the critical pressure is exceeded and thus enables a regulated pressure release before irreversible damage to the recipient occurs. Cold isostatic pressing is carried out in most cases at room temperature. In specially designed presses, moderate heating of the pressure medium up to a maximum temperature of 300 °C is possible.

In technical practice, a distinction is made between two basic principles of cold isostatic pressing, the wet bag process and the dry bag process. In addition, the wet bag process can also be used for the post-compaction of components uniaxial pre-pressed in a rigid form. The three variants are explained in more detail below:

i.) '''Wet bag process:''' In the wet bag process, the die is a self-supporting, elastic hollow mold that is filled with the powder outside the cold isostatic press. Optionally, a metallic mandrel can be integrated into the hollow mold for the production of pipes. After filling, the die is closed with an elastic cover plate. In order to protect the interior of the die against the ingress of liquid, the die can also be enveloped with an elastic foil, which is then evacuated and sealed in a liquid-tight manner. The wet bag process is often used in research and development due to its great flexibility with regard to the system parameters (including pressures up to approx. 400 MPa), the component geometries and the number of components per cycle. It is also used in industry for the production of large-volume components (e.g. filter candles) and semi-finished products (e.g. for manufacturing of ceramic insulators) with dimensions up to the meter range. Disadvantages of the wet bag process are the limited dimensional accuracy due to the elastic die and the comparatively long cycle times of several minutes.

ii.) '''Dry bag process:''' In dry bag pressing, the elastic die is firmly fixed to the recipient. Correspondingly, the mold filling takes place inside the cold isostatic press. The main advantages compared to wet bag pressing are the possibility of full automation, fast cycle times in the range of 10 s - 100 s depending on the component size (increase in cycle time with component size) and better dimensional accuracy. However, it should be noted that in the area of fixing the elastic die to the recipient there are restrictions with regard to the homogeneity of the pressure distribution, which, however, are less relevant for simpler geometries such as plates, cylinders or tubes. Dry die pressing is preferred in industrial production. The best-known application example are spark plug insulators, which are manufactured in a fully automated manner in quantities of millions.

iii.) '''Post-compaction of uniaxially pressed components:''' The shaping of ceramic and metallic powders via the uniaxial pressing in rigid molds is restricted by the wall friction, which leads to increasing density gradients in the component with increasing height/diameter ratio. The result is an inhomogeneous shrinkage during the subsequent sintering. In order to use the advantages of uniaxial pressing in terms of dimensional accuracy and at the same time to achieve a homogeneous density distribution in the component, it is possible to pre-press components uniaxially in a rigid die at moderate pressures, e.g. in the range of 50 - 100 MPa, and then post-compact them using cold isostatic pressing, which can be done e.g. at pressures in the range of 300 - 400 MPa. For the pressure transfer, the component must be liquid-tight welded into an elastic foil. When welding the foil, it must made sure that the foil is not damaged by sharp edges or particles.

[[File:Wiki Keramik KIP Abb 01.jpg|thumb|center]]
'''Figure 1:''' Cold isostatic press on a laboratory scale operated at the institute IEK-1, Forschungszentrum Jülich (manufacturer EPSI, type CIP 400-125 * 300Y). Usable volume: Diameter 125 mm, height = 300 mm. 

== Advantages and limitations of cold isostatic pressing ==

i.) '''Advantages:''' The main advantage of cold isostatic pressing is the elimination of friction-related variation in density, such as occurring in the case of uniaxial pressing in rigid molds. Therefore, higher green densities, higher green strengths and more homogeneous structures can be achieved with cold isostatic pressing. For example, press-related textures in the structure can be avoided to a large extent. Furthermore, components with a height / diameter ratio greater than 3: 1 (usually specified as limit for uniaxial pressing) can be produced relatively easily. Because there is no wall friction, it is possible to omit dispense with lubricants during pressing and the required proportion of other pressing additives can be significantly reduced. Furthermore, ceramic feedstocks can be compacted that contain abrasive solid particles that would lead to high tool wear in the case of uniaxial pressing.

ii.) '''Limits:''' Cold isostatic pressing is only suitable for relatively simple component geometries and is therefore restricted with respect to near-net-shape production. Due to the elastic properties of the die, there are limitations with regard to dimensional accuracy even with simpler geometries. Furthermore, the surface roughness is usually also relatively high, since the die wall yields elastically during pressing. Furthermore, sharp-edged particles can be pressed into the die wall, whereby the die is damaged in the worst case and demolding is aggravated. In order to increase the dimensional accuracy, mechanical post-processing of the cold isostatically pressed semi-finished products (so-called green machining) is often carried out. The relatively high green strength of cold isostatically pressed semi-finished products has a positive effect here.

== How to conduct a cold isostatic pressing cycle ==

In the following, it is explained in detail which processing steps are carried out in cold isostatic pressing and what must be considered in order to obtain crack-free samples and avoid damage to the system. The processing steps shown were carried out in a cold isostatic laboratory press of the following type:

Type: CIP 400-125*300Y
Manufacturer: EPSI, Temse, Belgien
Material of recipient SA 723 Class 3
Recipient inner diameter: 125 mm
Recipient inner height: 300 mm
Maximum sample size: limited by recipient volume
Maximum filling height: 295 mm
Recipient volume: 3.7 Liter
Nominal operating pressure: 4000 bar (400 MPa)
Maximum operating pressure: 4400 bar (440 MPa)
Safety factor: 1,1 (related to 4840 bar, 484 MPa)

i.) '''Encapsulation of the samples:''' Even with cold isostatic pressing, a uniform filling of the mold and a high filling density are basic requirements for successful compaction of the powder. In order to estimate the flowability of the powder, it is recommended to measure the bulk and tap density in accordance with DIN ISO 3923 and DIN ISO 3953. The flowability of a powder can be improved by granulating in a fluidizing bed or by spray drying. During granulation, spherical, easily flowable agglomerates are formed, which have a relatively low stability and are destroyed during the cold isostatic pressing. Some powder manufacturers offer powder directly in a granulated state. In order to increase the bulk density in the mold, the elastic die can optionally be vibrated or subjected to ultrasonic treatment. As an example, Figure 2 shows a simple elastic mold made of rubber for cold isostatic pressing of round bars.

[[File:Wiki Keramik KIP Abb 02.jpg|thumb|center]]
'''Figure 2:''' ''Elastic mold (rubber tube with cover plug) for cold isostatic pressing of round bars.
''
As mentioned above, there is also the possibility of post-compaction of uniaxially pressed semi-finished parts using cold isostatic pressing. Figure 3 shows how the welding of a pre-pressed part into an elastic foil can be carried out. For this purpose, at the IEK-1 institute, a vacuum sealer is used, which is usually applied in the household for sealing and freezing food. Elastic foils, which are established for this purpose, are suitable for encapsulation of pre-pressed parts in cold isostatic pressing as well. The sample is placed in the prepared bag, then interior is evacuated and the bag is finally liquid-tight welded. A more primitive alternative is to put the sample in a latex glove, which is evacuated, for example, by a water jet pump and sealed with a string.

[[File:Wiki Keramik KIP Abb 03.jpg|thumb|center]]
'''Figure 3:''' ''Sealing of a uniaxially pre-pressed sample in an elastic foil using a household vacuum sealer a.) Insertion of the uniaxially pre-pressed sample b.) Evacuation c.) Liquid-tight sealed sample.''

ii.) '''Opening the recipient:''' Figure 4 shows the individual steps for opening the recipient of the cold isostatic press of the type CIP 400-125 * 300Y (EPSI, Belgium). The press is equipped with a hydraulic lifting device. A screw is attached to this, via which the cover plate is connected to the hydraulic lifting device. The screw is protected from damage by a cage. After the screw has been attached, the cover is lifted using the lifting device. The sealing ring can be seen on the lower edge of the cover plate. This ring is pressed into the groove when the pressure is built up.

iii.) '''Introducing the sample into the recipient:''' For safety reasons it is important that the welded sample is not positioned directly in the oil-water emulsion. In the worst case, the sample or parts of the elastic foil can get into the liquid transport system of the cold isostatic press and block it, so that a pressure reduction is no longer possible and a service technician has to be called in. To safely avoid this risk, the sample must be placed in the oil-water emulsion in a specifically designed metal cage shown in Figure 4f. Spacers are welded onto the underpart of the metal cage, which prevent the metal mesh from resting directly on the bottom of the recipient. In this way, an unhindered pressure build-up and release is ensured. The metal cage also makes it easier to remove the sample after the cycle from the oil-water emulsion.

[[File:Wiki Keramik CIP Fig 04 english.jpg|thumb|center]]
'''Figure 4:''' ''Preparation of the system for the CIP cycle a.) Closed system b.) Attaching the screw to the cover plate c.) Starting the opening process d.) Open system e.) View on the oil-water emulsion f.) Metal cage for placing the encapsulated sample in the CIP device.''

iv.) '''Closing the recipient:''' After installing the metal cage including the sample in the recipient, the cover plate is closed via the hydraulic lifting system and the screw for fixing the cover plate is removed. The yoke, which absorbs the pressure in the axial direction, is then positioned over the cover plate. A specially designed locking system guarantees the exact position of the yoke in relation to the recipient. The locking bar is manually locked in the pressing position with a lever. Figure 5 shows the individual steps for closing the recipient.

[[File:Wiki Keramik KIP Abb 05.jpg|thumb|center]]
'''Figure 5:''' ''a., b.) Closing the recipient using the hydraulic lifting device c.) Locking the yoke before starting the pressing cycle.''

v.) '''Pressure build-up and dwell time, protection against overpressure:''' As mentioned at the beginning, the pressure build-up takes place by a high-pressure pump which is connected to the interior of the recipient via the liquid transport system. Figure 6 shows the system components relevant for pressure build-up. The desired pressure and the dwell time at this pressure are programmed via the system control display. The pressure is applied at the speed as defined in the program. The run of the pressure curve and the actual pressure can be read directly on the display and on an analog manometer. The cold isostatic press operated on the IEK-1 is designed for a maximum pressure of 4400 bar (440 MPa). To be on the safe side, the pressure in standard operation of the system should not exceed 4000 bar (400 MPa). The system is equipped with a rupture disc as overpressure protection. The rupture disc protects the system from uncontrolled failure and is designed with a safety factor of 1.1 based on the maximum pressure.

[[File:Wiki Keramik KIP Abb 06.jpg|thumb|center]]
'''Figure 6:''' ''a.) Programming of the pressing process via the display b.) Indication of the pressure via the manometer c.) Rupture disc as protection against overpressure.''

vi.) '''Decompression:''' Decompression is the most critical step in cold isostatic pressing. If there is still air in the sample after the sample preparation, it is strongly compressed during the CIP cycle. The high compression of the powder compact is associated with a strong reduction in the residual porosity. Accordingly, after pressing, there is a high flow resistance for the compressed air to escape and the pressure release takes a certain amount of time (up to a few minutes, depending on the pressing density achieved). If the pressure is released suddenly, this can lead to failure of the compact by severe cracking. It should be noted that a powder compact is also deformed elastically in addition to plastic deformation. When the pressure is released, there is therefore an elastic rebound of the pressed part ("spring-back" effect), which can be between 0.5 - 2%. Since the compression takes place in an elastic mold, the spring-back is viewed as less critical, but in the worst case it can also lead to damage to the pressed part, e.g. if it sticks to the die wall.

The decompression at the laboratory facility of the IEK-1 institute (type CIP 400-125 * 300Y, EPSI, Belgium) is initiated by opening a pneumatic high-pressure valve. The pressure release can then be regulated either manually via a valve or via an adjustable throttle valve. The throttle valve consists of a high pressure tube in which a needle is inserted. The decompression speed is controlled by the inner diameter of the tube and the position and thickness of the needle. Figure 7 shows the display for initiating decompression and the throttle valve, which is located on the rear of the cold isostatic press.

[[File:Wiki Keramik KIP Abb 07.jpg|thumb|center]]
'''Figure 7:''' ''a.) Display for selecting the decompression mode b.) Throttle valve.''

After the pressure has been completely released, the system can be opened as already described under i.). Afterwards, the metal cage together with the sample can be removed. After removing the elastic foil, the sample is ready for use.

== Applications of cold isostatic pressing ==

Cold isostatic pressing

2021-08-04T08:32:02Z

M.bram: /* How to conduct a cold isostatic pressing cycle */

== General principle of cold isostatic pressing (CIP) ==

The cold isostatic pressing CIP is based on the effect that a pressure applied to a liquid spreads evenly in all directions (so-called Pascal's principle). Inside the liquid, this leads to a homogeneous pressure distribution, which can be used for shaping ceramic and metallic powders if the powder is encapsulated in an elastic die. Elastic polymers (elastomers) such as polyurethane (PU), polyvinyl chloride (PVC), synthetic or natural rubber have proven successful as materials for the elastic die. The main components of a cold isostatic press are the recipient filled with the pressure transmission medium, the high-pressure pump, the locking system, the overpressure protection and the system control. The recipient is a pressure cylinder, which consists of either a high-strength, thick-walled steel cylinder or a thin-walled steel vessel with a pre-tensioned wire winding.

The pressure transmission media used are preferably water with the addition of an anti-corrosion agent, oil-water emulsions or glycerine. A hydraulic unit like an axial piston pump is used to build up pressure. This unit is connected to the recipient via a fluid transport system with appropriate valves and throttles. The pressure cylinder is sealed, for example, by a polymer O-ring that is integrated into the cover plate and is pressed into a groove when the pressure is built up. In order to absorb the large forces in the axial direction, the cover plate of the recipient is usually supported by a massive yoke. A rupture disc is used to protect against overpressure, which fails when the critical pressure is exceeded and thus enables a regulated pressure release before irreversible damage to the recipient occurs. Cold isostatic pressing is carried out in most cases at room temperature. In specially designed presses, moderate heating of the pressure medium up to a maximum temperature of 300 °C is possible.

In technical practice, a distinction is made between two basic principles of cold isostatic pressing, the wet bag process and the dry bag process. In addition, the wet bag process can also be used for the post-compaction of components uniaxial pre-pressed in a rigid form. The three variants are explained in more detail below:

i.) '''Wet bag process:''' In the wet bag process, the die is a self-supporting, elastic hollow mold that is filled with the powder outside the cold isostatic press. Optionally, a metallic mandrel can be integrated into the hollow mold for the production of pipes. After filling, the die is closed with an elastic cover plate. In order to protect the interior of the die against the ingress of liquid, the die can also be enveloped with an elastic foil, which is then evacuated and sealed in a liquid-tight manner. The wet bag process is often used in research and development due to its great flexibility with regard to the system parameters (including pressures up to approx. 400 MPa), the component geometries and the number of components per cycle. It is also used in industry for the production of large-volume components (e.g. filter candles) and semi-finished products (e.g. for manufacturing of ceramic insulators) with dimensions up to the meter range. Disadvantages of the wet bag process are the limited dimensional accuracy due to the elastic die and the comparatively long cycle times of several minutes.

ii.) '''Dry bag process:''' In dry bag pressing, the elastic die is firmly fixed to the recipient. Correspondingly, the mold filling takes place inside the cold isostatic press. The main advantages compared to wet bag pressing are the possibility of full automation, fast cycle times in the range of 10 s - 100 s depending on the component size (increase in cycle time with component size) and better dimensional accuracy. However, it should be noted that in the area of fixing the elastic die to the recipient there are restrictions with regard to the homogeneity of the pressure distribution, which, however, are less relevant for simpler geometries such as plates, cylinders or tubes. Dry die pressing is preferred in industrial production. The best-known application example are spark plug insulators, which are manufactured in a fully automated manner in quantities of millions.

iii.) '''Post-compaction of uniaxially pressed components:''' The shaping of ceramic and metallic powders via the uniaxial pressing in rigid molds is restricted by the wall friction, which leads to increasing density gradients in the component with increasing height/diameter ratio. The result is an inhomogeneous shrinkage during the subsequent sintering. In order to use the advantages of uniaxial pressing in terms of dimensional accuracy and at the same time to achieve a homogeneous density distribution in the component, it is possible to pre-press components uniaxially in a rigid die at moderate pressures, e.g. in the range of 50 - 100 MPa, and then post-compact them using cold isostatic pressing, which can be done e.g. at pressures in the range of 300 - 400 MPa. For the pressure transfer, the component must be liquid-tight welded into an elastic foil. When welding the foil, it must made sure that the foil is not damaged by sharp edges or particles.

[[File:Wiki Keramik KIP Abb 01.jpg|thumb|center]]
'''Figure 1:''' Cold isostatic press on a laboratory scale operated at the institute IEK-1, Forschungszentrum Jülich (manufacturer EPSI, type CIP 400-125 * 300Y). Usable volume: Diameter 125 mm, height = 300 mm. 

== Advantages and limitations of cold isostatic pressing ==

i.) '''Advantages:''' The main advantage of cold isostatic pressing is the elimination of friction-related variation in density, such as occurring in the case of uniaxial pressing in rigid molds. Therefore, higher green densities, higher green strengths and more homogeneous structures can be achieved with cold isostatic pressing. For example, press-related textures in the structure can be avoided to a large extent. Furthermore, components with a height / diameter ratio greater than 3: 1 (usually specified as limit for uniaxial pressing) can be produced relatively easily. Because there is no wall friction, it is possible to omit dispense with lubricants during pressing and the required proportion of other pressing additives can be significantly reduced. Furthermore, ceramic feedstocks can be compacted that contain abrasive solid particles that would lead to high tool wear in the case of uniaxial pressing.

ii.) '''Limits:''' Cold isostatic pressing is only suitable for relatively simple component geometries and is therefore restricted with respect to near-net-shape production. Due to the elastic properties of the die, there are limitations with regard to dimensional accuracy even with simpler geometries. Furthermore, the surface roughness is usually also relatively high, since the die wall yields elastically during pressing. Furthermore, sharp-edged particles can be pressed into the die wall, whereby the die is damaged in the worst case and demolding is aggravated. In order to increase the dimensional accuracy, mechanical post-processing of the cold isostatically pressed semi-finished products (so-called green machining) is often carried out. The relatively high green strength of cold isostatically pressed semi-finished products has a positive effect here.

== How to conduct a cold isostatic pressing cycle ==

In the following, it is explained in detail which processing steps are carried out in cold isostatic pressing and what must be considered in order to obtain crack-free samples and avoid damage to the system. The processing steps shown were carried out in a cold isostatic laboratory press of the following type:

Type: CIP 400-125*300Y
Manufacturer: EPSI, Temse, Belgien
Material of recipient SA 723 Class 3
Recipient inner diameter: 125 mm
Recipient inner height: 300 mm
Maximum sample size: limited by recipient volume
Maximum filling height: 295 mm
Recipient volume: 3.7 Liter
Nominal operating pressure: 4000 bar (400 MPa)
Maximum operating pressure: 4400 bar (440 MPa)
Safety factor: 1,1 (related to 4840 bar, 484 MPa)

i.) '''Encapsulation of the samples:''' Even with cold isostatic pressing, a uniform filling of the mold and a high filling density are basic requirements for successful compaction of the powder. In order to estimate the flowability of the powder, it is recommended to measure the bulk and tap density in accordance with DIN ISO 3923 and DIN ISO 3953. The flowability of a powder can be improved by granulating in a fluidizing bed or by spray drying. During granulation, spherical, easily flowable agglomerates are formed, which have a relatively low stability and are destroyed during the cold isostatic pressing. Some powder manufacturers offer powder directly in a granulated state. In order to increase the bulk density in the mold, the elastic die can optionally be vibrated or subjected to ultrasonic treatment. As an example, Figure 2 shows a simple elastic mold made of rubber for cold isostatic pressing of round bars.

[[File:Wiki Keramik KIP Abb 02.jpg|thumb|center]]
'''Figure 2:''' Elastic mold (rubber tube with cover plug) for cold isostatic pressing of round bars.

As mentioned above, there is also the possibility of post-compaction of uniaxially pressed semi-finished parts using cold isostatic pressing. Figure 3 shows how the welding of a pre-pressed part into an elastic foil can be carried out. For this purpose, at the IEK-1 institute, a vacuum sealer is used, which is usually applied in the household for sealing and freezing food. Elastic foils, which are established for this purpose, are suitable for encapsulation of pre-pressed parts in cold isostatic pressing as well. The sample is placed in the prepared bag, then interior is evacuated and the bag is finally liquid-tight welded. A more primitive alternative is to put the sample in a latex glove, which is evacuated, for example, by a water jet pump and sealed with a string.

[[File:Wiki Keramik KIP Abb 03.jpg|thumb|center]]
'''Figure 3:''' Sealing of a uniaxially pre-pressed sample in an elastic foil using a household vacuum sealer a.) Insertion of the uniaxially pre-pressed sample b.) Evacuation c.) Liquid-tight sealed sample.

ii.) '''Opening the recipient:''' Figure 4 shows the individual steps for opening the recipient of the cold isostatic press of the type CIP 400-125 * 300Y (EPSI, Belgium). The press is equipped with a hydraulic lifting device. A screw is attached to this, via which the cover plate is connected to the hydraulic lifting device. The screw is protected from damage by a cage. After the screw has been attached, the cover is lifted using the lifting device. The sealing ring can be seen on the lower edge of the cover plate. This ring is pressed into the groove when the pressure is built up.

iii.) '''Introducing the sample into the recipient:''' For safety reasons it is important that the welded sample is not positioned directly in the oil-water emulsion. In the worst case, the sample or parts of the elastic foil can get into the liquid transport system of the cold isostatic press and block it, so that a pressure reduction is no longer possible and a service technician has to be called in. To safely avoid this risk, the sample must be placed in the oil-water emulsion in a specifically designed metal cage shown in Figure 4f. Spacers are welded onto the underpart of the metal cage, which prevent the metal mesh from resting directly on the bottom of the recipient. In this way, an unhindered pressure build-up and release is ensured. The metal cage also makes it easier to remove the sample after the cycle from the oil-water emulsion.

[[File:Wiki Keramik CIP Fig 04 english.jpg|thumb|center]]
'''Figure 4:''' Preparation of the system for the CIP cycle a.) Closed system b.) Attaching the screw to the cover plate c.) Starting the opening process d.) Open system e.) View on the oil-water emulsion f.) Metal cage for placing the encapsulated sample in the CIP device.

iv.) '''Closing the recipient:''' After installing the metal cage including the sample in the recipient, the cover plate is closed via the hydraulic lifting system and the screw for fixing the cover plate is removed. The yoke, which absorbs the pressure in the axial direction, is then positioned over the cover plate. A specially designed locking system guarantees the exact position of the yoke in relation to the recipient. The locking bar is manually locked in the pressing position with a lever. Figure 5 shows the individual steps for closing the recipient.

[[File:Wiki Keramik KIP Abb 05.jpg|thumb|center]]
'''Figure 5:''' a., b.) Closing the recipient using the hydraulic lifting device c.) Locking the yoke before starting the pressing cycle.

v.) '''Pressure build-up and dwell time, protection against overpressure:''' As mentioned at the beginning, the pressure build-up takes place by a high-pressure pump which is connected to the interior of the recipient via the liquid transport system. Figure 6 shows the system components relevant for pressure build-up. The desired pressure and the dwell time at this pressure are programmed via the system control display. The pressure is applied at the speed as defined in the program. The run of the pressure curve and the actual pressure can be read directly on the display and on an analog manometer. The cold isostatic press operated on the IEK-1 is designed for a maximum pressure of 4400 bar (440 MPa). To be on the safe side, the pressure in standard operation of the system should not exceed 4000 bar (400 MPa). The system is equipped with a rupture disc as overpressure protection. The rupture disc protects the system from uncontrolled failure and is designed with a safety factor of 1.1 based on the maximum pressure.

[[File:Wiki Keramik KIP Abb 06.jpg|thumb|center]]
'''Figure 6:''' a.) Programming of the pressing process via the display b.) Indication of the pressure via the manometer c.) Rupture disc as protection against overpressure.

vi.) '''Decompression:''' Decompression is the most critical step in cold isostatic pressing. If there is still air in the sample after the sample preparation, it is strongly compressed during the CIP cycle. The high compression of the powder compact is associated with a strong reduction in the residual porosity. Accordingly, after pressing, there is a high flow resistance for the compressed air to escape and the pressure release takes a certain amount of time (up to a few minutes, depending on the pressing density achieved). If the pressure is released suddenly, this can lead to failure of the compact by severe cracking. It should be noted that a powder compact is also deformed elastically in addition to plastic deformation. When the pressure is released, there is therefore an elastic rebound of the pressed part ("spring-back" effect), which can be between 0.5 - 2%. Since the compression takes place in an elastic mold, the spring-back is viewed as less critical, but in the worst case it can also lead to damage to the pressed part, e.g. if it sticks to the die wall.

The decompression at the laboratory facility of the IEK-1 institute (type CIP 400-125 * 300Y, EPSI, Belgium) is initiated by opening a pneumatic high-pressure valve. The pressure release can then be regulated either manually via a valve or via an adjustable throttle valve. The throttle valve consists of a high pressure tube in which a needle is inserted. The decompression speed is controlled by the inner diameter of the tube and the position and thickness of the needle. Figure 7 shows the display for initiating decompression and the throttle valve, which is located on the rear of the cold isostatic press.

[[File:Wiki Keramik KIP Abb 07.jpg|thumb]]
Figure 7: a.) Display for selecting the decompression mode b.) Throttle valve.

After the pressure has been completely released, the system can be opened as already described under i.). Afterwards, the metal cage together with the sample can be removed. After removing the elastic foil, the sample is ready for use.

== Applications of cold isostatic pressing ==

File:Wiki Keramik KIP Abb 07.jpg

2021-08-04T08:31:13Z

M.bram:

Figure 7: a.) Display for selecting the decompression mode b.) Throttle valve.