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Thermal Properties Laboratory

The Thermal Properties Laboratory is located within the Material Sciences Laboratory (Building 326) at the Hanford Site 300 Area north of Richland, Washington. The Thermal Properties Laboratory is operated by the Energy and Engineering Division of the Energy Sciences and Technology Directorate. Thermal diffusivity and thermal expansion test capabilities are available, in addition to a variety of metrology and sample preparation capabilities. The Thermal Properties Laboratory was recently renovated; it represents a state-of-the-art facility for integrated thermal properties measurements on unirradiated or irradiated materials. In addition, thermal properties testing of classified materials can also be accommodated. Included below is a list of references that highlight some of the recent work in the Thermal Properties Laboratory.

Thermal Diffusivity Testing

The centerpiece of the Thermal Properties Laboratory is a well-established laser flash thermal diffusivity measurement capability. Two diffusivity test units are available, a low temperature apparatus for testing from room temperature to 400 °C in air, and a high temperature unit (shown at above) for testing from 300 to 1500 °C in vacuum or inert gas. The low temperature unit utilizes an aluminum-block box furnace, while the high temperature system uses a tungsten-mesh tube furnace. Temperature control is facilitated by the use of thermocouples located near, but not touching, the test samples. Thermal diffusivity can be measured on either monolithic, isotropic composites, or layered materials. Samples can vary in size from 6 to 10 mm in diameter, and typical sample thicknesses range from 1 to 3 mm (optimum sample thickness is determined separately for each material based on its expected thermal diffusivity). Square or other cross-sections can be accommodated with custom fixturing. Ideally, the samples should be rigid and opaque, although the use of metallicor carbon coatings to render translucent samples opaque is possible. The high temperature unit tests one sample at a time, while the low temperature apparatus tests up to six samples simultaneously. Data acquisition, reduction, and analysis in both systems is performed computationally in near-real-time using software tailored to specific customer needs. Both systems can accommodate either unirradiated or irradiated materials. The units are maintained and operated such that they remain uncontaminated, and they may be used for unirradiated materials without risk of cross-contamination. Materials tested in the two systems include depleted-UO2 experimental light water reactor fuels, stainless steels, precious metals, refractory metal alloys, aluminum metal-matrix composites, alumina, zirconia, zirconium carbide, silicon nitride, silicon carbide, alumina particulate-reinforced alumina-matrix composites, silicon carbide particulate- and whisker-reinforced silicon carbide composites, and SiC-based fiber-reinforced SiC-matrix composites. In addition to measuring thermal diffusivity for determination of engineering properties, the systems also have been used to elucidate irradiation damage mechanisms and defect structures via isochronal annealing and in-situ measurement of thermal diffusivity on irradiated materials. The systems also have been used to evaluate the nature of fiber-matrix bonding in fiber-reinforced ceramic-matrix composites in order to optimize the composition and fiber architecture of these materials.

Thermal Expansion Testing

A complimentary thermal expansion testing capability also exists in the Thermal Properties Laboratory. Thermal expansion tests are performed in inert gas over a temperature range from room temperature to 1500 °C. Thermal expansion is measured using a dual alumina-pushrod dilatometer (shown at right) that utilizes absolute displacement transducers for simplicity of operation and increased reliability. Standard thermal expansion tests can be conducted with any combination of heating and cooling rates. The furnace can also hold temperatures to within a few degrees for any length of time to allow equilibrium thermal expansion tests or in-situ sintering or annealing studies. The system is completely automated and can accommodate testing of two samples simultaneously. Samples may be tested individually or they may be tested in comparison to a standard for more precise thermal expansion measurements. The standard sample length is 38 mm, but lengths from 13 to65 mm can be accommodated with custom fixturing. Samples can have round, rectangular, or other irregular cross-sections up to a maximum diameter of10 mm. Irradiated or unirradiated samples may be tested in this system without risk of cross-contamination. Previous testing experience includes thermal expansion measurements on monolithic ceramics, ceramic composites, metals, alloys, and metal-matrix composites. In addition, the system has been used for isochronal annealing tests on irradiated high purity silicon carbide specimens for the purpose of determining irradiation temperature. Used in conjunction with the thermal diffusivity systems, the isochronal annealing tests on irradiated materials offers complimentary data that can help to determine irradiation damage mechanisms and irradiation-induced defect structures. The system also has been used to measure, in-situ, the shrinkage of pre-ceramic polymer joints in SiC during curing and pyrolysis.

Radioactive Materials Characterization and Handling

The Thermal Properties Laboratory provides other capabilities that are necessary to support the thermal properties testing activities. Principal among these is an extensive metrology capability for precise dimensional measurements on unirradiated and irradiated materials. This capability has been used extensively for measuring irradiation-induced swelling in ceramics, ceramic composites, and ceramic fibers. A radioactive material glovebox is available for activities such as preparing metallography samples and metrology of dispersible radioactive materials. A large fume hood is available for work with chemicals or less dispersible radioactive materials. Two lead-shielded caves are available for safe and secure storage of radioactive materials.

Complimentary Capabilities

In addition to the Thermal Properties Laboratory, the Energy Technology Division operates three other laboratories within the Material Sciences Laboratory. All of these laboratories were recently renovated to serve as state-of-the-art general purposes laboratories with ample work areas, storage space, fixtures and utilities.

Tools available for general purpose use include a lathe, a drill press, and a bench grinder. Two non-radioactive, high-purity inert gas, low-moisture gloveboxes are available in the laboratories for work requiring a controlled atmosphere. One of the gloveboxes includes a large tube furnace with 50 to 1000°C temperature capability that can accommodate samples up to 25 mm in diameter and in excess of 500 mm in length. The gloveboxes recently have been used for such activities as sintering of composite metal-ceramic powders and experimental studies on stabilization of liquid sodium wastes. Three non-radioactive fume hoods are also available for work with chemicals or other hazardous materials. A variety of furnaces(some shown at right) are available that can be used over the temperature range 50 to 1600°C in air or vacuum. The furnaces all have controllers that permit automated operation. The furnaces are used for a variety of activities, including bakeout of porous ceramics, consolidation of metal powders, and long-term aging tests. All three laboratories are configured with access to process cooling water, tap water, compressed air, building vacuum, building nitrogen, and ample power (including 120V, 240V and 480V service) for maximum flexibility in meeting customer needs. In addition, the staff working in the laboratories have extensive experience in design, fabrication and operation of testing and production systems.

Recent References of Interest

Youngblood, GE, DJ Senor, RH Jones and S Graham. 2002. "The Transverse Thermal Conductivity of 2D-SiCf/SiC Composites," Composites Science and Technology, 62:1127-1139.

Youngblood, GE, DJ Senor, RH Jones and W Kowbel. 2001. "Optimizing the Transverse Thermal Conductivity of 2D-SiCf/SiC Composites," Proceedings of the Tenth International Conference on Fusion Reactor Materials (ICFRM-10), Baden-Baden, Germany, 14-19 October 2001.

Senor, DJ, GE Youngblood, RH Jones and S Graham. 2000. "Transverse Thermal Conductivity of Planar SiC/SiC Composites," Transactions of the American Nuclear Society, 83:189-190.

Senor, DJ, GE Youngblood, CE Chamberlin and DV Archer. 1999. "Recent Progress in Thermal Conductivity Testing of SiC-Based Materials for Fusion," Proceedings of the Third IEA Workshop on SiC/SiC Ceramic Composites for Fusion Structural Applications, Cocoa Beach, FL, 29-30 January 1999.

Senor, D.J., G.E. Youngblood, C.E. Moore, D.J. Trimble, G.A. Newsome and J.J. Woods. 1996. "Effects of Neutron Irradiation on Thermal Conductivity of SiC-Based Composites and Monolithic Ceramics," Fusion Technology, 30:943-955.

Senor, D.J., D.J. Trimble and G.A. Newsome. 1997. "Effect of Irradiation on Thermal Expansion of SiCf/SiC Composites," Ceramic Engineering and Science Proceedings, 18(3):591-598.

Point of Contact: Dave Senor, (509) 376-5610