The invention relates to an apparatus for pressing and heating multiple material samples in parallel and a method for same.
Material pellets are used for research in a wide range of technologies. For example, in semiconductor and thermoelectrics technologies, knowledge of the transport characteristics of a material, including its electrical resistivity (DC and AC), Hall coefficient, thermal conductivity and thermopower is required. In addition, in the area of structural materials, accurate information regarding a sample's toughness, yield strength, and hardness is often required. In the powder metallurgy field, reliable information on material properties can be obtained from a highly dense pellet (e.g., a pellet having greater than 99% density and less than 1% air pockets). Furthermore, pellets of materials are often used to obtain greater understanding of a material through optical measurements such as ultraviolet-visible (UV-Vis), infrared (IR) or magnetization measurements. Pellets are used in a wide variety of applications. In any given application, there may be many different material types to be researched, each of which has a myriad of chemical and processing variations.
Powdered material is often used as a starting form for making components of complex shapes. Powdered material is transformed into a dense, solid body through the application of pressure and/or heat. The general method for creating a dense body begins with loading loose powder into a die. The powder can be a metal, a ceramic, a plastic or any other material that is to be compressed. Pressure is applied to the powder through loading of an upper and lower punch. This pressure is high enough to cause the powdered material to fuse and take the shape of the interior of the die. If the load is taken off, the part can be removed from the die as a solid body. In this green state, the powder is usually not fully dense, the part lacks cohesion and is either very brittle or remains powdery. A green body is converted into a dense body by consolidation, a process that removes voids from the pellet, thus increasing the density. Consolidation requires mass transport within the green body, a process that can be activated by heat (sintering), ultra-high pressure, and/or the application of a voltage between the punches (e.g., Spark Plasma Sintering).
Spark Plasma Sintering (SPS) achieves consolidation through the application of a potential difference between the upper and lower punches. Advantages to this process include the reduction of sintering time and, as a consequence, the ability to retain the nanostructured grain structure necessary in many applications. The process of SPS is achieved by application of a potential difference (˜5 Volts, for example) between the punches and the generation of very high currents (>1000 Amps, for example). These currents are thought to induce consolidation by generation of heat via Joule heating and through the generation of plasma within the powder material.
Uniaxial hot pressing is used to densify a loose powder into a solid body, such as a pellet, that will be tested to determine different properties of the densified material. A load is applied to a powder (held in a die) in one direction, thus compacting the powder. At the same time, heat is applied to the powder in order to sinter it and bring the bulk component close to 100% material density. Traditional uniaxial hot pressing methods process one material sample at a time. In a lab where a large number of material samples are required for testing, this is too slow and expensive.
Access to a high-throughput pellet press would greatly increase the rate of production of material sample pellets and subsequent material research. An apparatus is provided that performs uniaxial hot pressing to multiple powder material samples in parallel. As used herein, “in parallel” means that load and/or heat is applied to the multiple powder material samples simultaneously. In some embodiments, the apparatus applies independent levels of loading and/or heat to the multiple powder samples. Parallel uniaxial hot pressing by the apparatus allows many samples to be densified in a high throughput manner.
Specifically, the apparatus includes a die assembly that defines multiple pockets, as well as a load transferring mechanism selectively providing a respective uniaxial compressive load at each of the pockets. Multiple heating mechanisms are arranged so that each of the pockets is aligned with a different respective one of the heating mechanisms. The load transferring mechanism and the heating mechanisms provide both compressive loading and heating of multiple material samples in parallel when material samples are placed in the pockets. The heating mechanisms may include inductive heating coils. Alternatively, the heating mechanisms may include lead wires, a power source and a power circuit configured to create a potential voltage difference between the upper and lower punches.
A method of hot pressing material includes dispensing powder material samples into spaced pockets at least partially defined by a die assembly and applying uniaxial pressure to each of the powder material samples in the spaced pockets with a load transferring mechanism to compact the powder material samples in parallel. Heating mechanisms are activated to heat the powder material samples in parallel while the uniaxial pressure is applied by the load transferring mechanism.
The above features and advantages and other features and advantages of the present invention are readily apparent from the following detailed description of the best modes for carrying out the invention when taken in connection with the accompanying drawings.
Referring to the drawings, wherein like reference numbers refer to like components throughout the views,
The apparatus includes a parallel die assembly 60 that is shown in more detail in
Four additional pockets 135 are formed by the parallel die 70 above the other four lower punches 110, and may be filled with the same or with different powder material samples. The pockets 135 shown in this embodiment have a circular cross-section. However, the pockets 135 could have any cross-sectional shape resulting from the lower punches 110 and die 70, with the lower punch 110 configured to fit into the opening 140 (that is, the lower punch 110 and the opening 140 having complementary shapes). In this embodiment, each lower punch 110 has a flat surface 142 on which the respective material sample 150A-150D rests. Alternatively, the surface 142 could have other topography as required by the part to be pressed. For example, the surface of a pocket 135 on which the powder material sample rests could instead be a three-dimensional shape in order to impart a corresponding three-dimensional shape to an outer surface of the processed material sample.
In step 304 of the method 300 of
Once the parallel die assembly 60 is loaded on the nest plate 160, the powder material samples 150A, 150B, 150C, 150D can be compacted. In step 306, uniaxial pressure is applied to each of the powder material samples 150A, 150B, 150C, 150D by pressurizing the hydraulic cylinder 30. That is, a hydraulic fluid is directed from a hydraulic fluid supply to the cylinder 30. The cylinder 30 has telescoping portions that expand the cylinder 30 when pressurized with the fluid. This causes the upper die plate 50 to move toward the powder material samples 150A, 150B, 150C, 150D (i.e., down in
The hydraulic cylinder 30 travels until the stacks of wave springs 210 are compressed a desired amount. Once the upper punches 180 contact the material samples 150A, 150B, 150C, 150D, the compressive load is transferred from the cylinder 30 through the upper die plate 50, the backing plate 215, and the stacks of wave springs 210 to the upper punches 180 and the powder material samples 150A, 150B, 150C, 150D along the respective centerlines 114A, 114B, 114C, 114D of the upper punches 180.
Each upper punch 180 is thus loaded by an individual stack of wave springs 210. This allows each upper punch 180 to move axially, independently of the other upper punches 180. Independent loading of the upper punches 180 allows each powder material sample 150A, 150B, 150C, 150D to be compressed a different desired amount. If the upper punches 180 were not independent, the loading of each powder material sample 150A, 150B, 150C, 150D would vary depending on the amount of material sample in each pocket 135. For example, if one pocket 135 contained a material sample of much less volume than the others, the upper punch 180 corresponding with that pocket 135 would not come into contact with the material sample. By enabling the upper punches 180 to move independently of one another, a desired load can be transferred to each powder material sample 150A, 150B, 150C, 150D.
The load transferring mechanism 15 shown uses similar stacks of wave springs 210 for each upper punch 180, thus providing the same loading on each powder material sample 150A, 150B, 150C, 150D. Different loads at one or more of the powder material samples 150A, 150B, 150C, 150D can be achieved by using different stiffness springs for each stack of wave springs 210 at each upper punch 180. In this way, different pressures can be applied in parallel to the different powder material samples 150A, 150B, 150C, 150D. A first powder material sample, such as material sample 150A in a first pocket 135 can be subjected to a different compressive load than a second powder material sample 150B in a second of the pockets 135.
An alternate embodiment of a uniaxial parallel hot pressing apparatus 10A is shown in
Referring to
In contrast, if the powder material samples 150A, 150B, 150C or 150D to be pressed are nonconductive, then the components that come into contact with the powder material sample 150A, 150B, 150C or 150D (parallel die 70, lower punch 110, and upper punch 180) must be made of a conductive material such as steel. Because nonconductive powder material samples 150A, 150B, 150C or 150D cannot be inductively heated directly, the die components in direct contact with the powder material sample 150A, 150B, 150C or 150D are heated inductively. Heat is transferred from the die components (parallel die 70, lower punch 110, and upper punch 180) to the material sample 150A, 150B, 150C or 150D as it is being compressed. The thermal breaks 202 would be used in such an embodiment.
The powder material samples 150A, 150B, 150C and 150D are thus held under pressure and heated simultaneously. This has been found to improve the densification process. The load (and corresponding pressure) and temperature can be adjusted depending on the requirements of the material sample. For example, to achieve 99% density of a 50 μm tool steel powder in one hour, a pressure of approximately 50 MPa and a first temperature of approximately 1200° C. are required. These parameters may be applied to a first material sample 150A using a first induction heating mechanism (coil 220), while a second powder material sample 150B can be heated to a second temperature of 800° C., for example, using a second induction heating mechanism (coil 220 aligned with powder material sample 150B). The controller 201 receives temperature data from temperature sensors (not shown) positioned in thermal communication with the pockets 135 of
As the powder material sample 150A, 150B, 150C or 150D is densified, the sample 150A, 150B, 150C or 150D will take up less volume. The independent spring loading of each upper punch 180 by a corresponding aligned one of the stacks of wave springs 210 allows each powder material sample 150A-150D to stay under a relatively constant pressure (determined by the spring rate of the corresponding stack of wave springs 210).
After densification is complete, hydraulic pressure applied to the hydraulic cylinder 30 is relieved so that the hydraulic cylinder 30 is retracted and the apparatus 10 for parallel uniaxial hot pressing returns to the open position of
The heating mechanism 220A includes a power source 204A and positive leads 206A, 206B, 206C, 206D operatively connected to the different upper punches 180, as well as negative leads 208A, 208B, 208C, 208D operatively connected to the different lower punches 110. A power circuit 209A is configured to enable different potential voltage differences to be established at the different pairs of upper punches 180 and lower punches 110 so that the currents and ultimately the heating of each of the material samples 150A, 150B, 150C, 150D is independent of the heating of the other material samples 150A, 150B, 150C, 150D. Alternatively, the power circuit 209A could be controlled to provide the same potential voltage difference to each of the material samples 150A-150D.
The apparatus 10B is operable according to the same method 300 of
While the best modes for carrying out the invention have been described in detail, those familiar with the art to which this invention relates will recognize various alternative designs and embodiments for practicing the invention within the scope of the appended claims.
U.S. Provisional Application No. 61/566,037 filed on Dec. 2, 2011 is hereby incorporated by reference in its entirety.
Number | Date | Country | |
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61566037 | Dec 2011 | US |