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Ultrahigh temperature ceramics (UHTCs) are a class of materials that include the diborides of metals such as hafnium and zirconium. The materials are of interest to NASA for their potential utility as sharp leading edges for hypersonic vehicles. Such an application requires that the materials be capable of operating at temperatures, often in excess of 2,000 C. UHTCs are highly refractory and have high thermal conductivity, an advantage for this application. UHTCs are potentially applicable for other high-temperature processing applications, such as crucibles for molten-metal processing and high-temperature electrodes. UHTCs were first studied in the 1960 s by the U.S. Air Force. NASA s Ames Research Center concentrated on developing materials in the HfB2/SiC family for a leading-edge application. The work focused on developing a process to make uniform monolithic (2-phase) materials, and on the testing and design of these materials. Figure 1 shows arc-jet models made from UHTC materials fabricated at Ames. Figure 2 shows a cone being tested in the arc-jet. Other variations of these materials being investigated elsewhere include zirconium based materials and fiber-reinforced composites. Current UHTC work at Ames covers four broad topics: monoliths, coatings, composites, and processing. The goals include improving the fracture toughness, thermal conductivity and oxidation resistance of monolithic UHTCs and developing oxidation-resistant UHTC coatings for thermal-protection-system substrates through novel coating methods. As part of this effort, researchers are exploring compositions and processing changes that have yielded improvements in properties. Computational materials science and nanotechnology are being explored as approaches to reduce materials development time and improve and tailor properties.

Contents include the following: Background on Ultra High Temperature Ceramics - UHTCs. Summary UNTC processing: power processing, scale-up. Preliminary material properties: mechanical, thermal. Arc jet testing: flat face models, cone models. Summary.

Hafnium Diboride (HFB,) based materials have shown promise for use in a number of high temperature aerospace applications, including rocket nozzles and as leading edges on hypersonic reentry vehicles. The stability of the materials in relevant environments is key to determining their suitability for a particular application. In this program we have been developing HfB2/SiC materials for use as sharp leading edges. The program as a whole included processing and characterization of the HfBJSiC materials. The specific work discussed here will focus on studies of the materials oxidation behavior in simulated reentry environments through arc jet testing. Four flat face models were tested to examine the influence of heat flux and stagnation pressure on the materials oxidation behavior. The results from arc jet testing of two HfB2/SiC cone models will also be discussed. Each cone model was run multiple times with gradually increasing heat fluxes. Total run times on a single cone model exceeded 80 minutes. For both the flat face and cone models surface temperatures well in excess of 2200 C were measured. Post test microstructural examination of the models and correlations with measured temperatures will be discussed.

The objectives of this research are to: 1) Investigate the oxidation/ablation behavior of HfB2/SiC materials in simulated re-entry environments; 2) Use the arc jet test results to define appropriate use environments for these materials for use in vehicle design. The parameters to be investigated include: surface temperature, stagnation pressure, duration, number of cycles, and thermal stresses.

A brief history of diboride research, an overview of processing, and sintering studies are covered in this viewgraph presentation. UHTCs are a family of ceramic materials, including diborides of Hf and Zr, with extremely high melting temperatures. Spark Plasma Sintering (SPS) is a novel processing technique useful in consolidating difficult materials. The presentation also contains microphotographs of the microstructure of HfB2 and ZrB2 processed in different ways.

Contents include the following: Modified hot pressing schedule has significantly improved UHTC billet processing: density and microstructure uniformity have improved. 2 in. dia. x 2 in. tall UHTC billets have been successfully hot pressed: scaled up billets have slightly higher density gradients axially than 1 in. billets. Hot press schedule has not been optimized for scaled up billets. Strengths and strength distributions are improving with experience: need to evaluate strength uniformity in the center of the billets. CTE or ARC materials compares favorably with heritage materials. Thermal conductivity of ARC materials considerably different than that of heritage materials.

Ultra High Temperature Ceramics (UHTCs) are being developed for possible use in a number of structural applications including hypersonic vehicles, engines, plasma arc electrodes and high temperature shielding. Alternative methods of processing Ultra High Temperature Ceramics (UHTCs) will be discussed. Techniques that may improve oxidation resistance, strength, and reduce the processing temperature of the UHTCs will be presented. Hot-pressed UHTCs made using either milled/uncoated powders or non-milled coated powders will be compared.

Hafnium diboride based materials have shown promise for use in extremely high temperature applications, such as sharp leading edges on future reentry vehicles. During reentry, the oxygen and nitrogen in the atmosphere are dissociated by the shock layer ahead of the sharp leading edge such that surface reactions are determined by reactions of monatomic oxygen and nitrogen rather than O2, and N2. Simulation of the reentry environment on the ground requires the use of arc jet (plasma jet) facilities that provide monatomic species and are the closest approximation to actual flight conditions. Simple static or flowing oxidation studies under ambient pressures and atmospheres are not adequate to develop an understanding of a materials behavior in flight. Arc jet testing is required to provide the appropriate stagnation pressures, heat fluxes, enthalpies, heat loads and atmospheres encountered during flight. This work looks at the response of HfB2/SiC materials exposed to various simulated reentry environments.

Future reentry vehicles will need better maneuverability to improve safety and performance. Vehicles with sharp leading edges, as opposed to the blunt nose and leading edges on the current space shuttle, can provide improved lift-to-drag and thus improved maneuverability. Materials capable of operating at temperatures in excess of 2000 C are required. Ultrahigh temperature ceramics (UHTCs) are one class of material being investigated for this application. These materials are diborides of hafnium or zirconium with a second phase of sic. The benefits of using these materials will be discussed as developments in the processing of HfB2/SiC.

Previous work on refractory diboride composites has shown that these systems have the potential for use in high temperature leading edge applications for reusable reentry vehicles. Experiments in reentry environments have shown that these materials have multiple use temperatures greater than 1900 C. The work to be discussed focuses on three compositions: HfB2/SiC, ZrB2/SiC, and ZrB2/C/SiC. These composites have been hot pressed and their mechanical properties measured at room and elevated temperatures. Extensive microstructural characterization has been conducted on polished cross sections and the fracture surfaces have been examined to determine their failure origins.