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Evaluation of oxidation protection testing methods on ultra-high temperature ceramic coatings for carbon-carbon oxidation resistance

Ceramic Engineering and Science Proceedings

Corral, Erica L.; Ayala, Alicia A.; Loehman, Ronald E.

The development of carbon-carbon (C-C) composites for aerospace applications has prompted the need for ways to improve the poor oxidation resistance of these materials, In order to evaluate and test materials to be used as thermal protection system (TPS) material the need for readily available and reliable testing methods are critical to the success of materials development efforts, With the purpose to evaluate TPS materials, three testing methods were used to assess materials at high temperatures (> 2000°C) and heat flux in excess of 200 Wcm-2. The first two methods are located at the National Solar Thermal Test Facility (NSTTF) at Sandia National Laboratories, which are the Solar Furnace Facility and the Solar Tower Facility, The third method is an oxyacetylene torch set up according to ASTM E285-80 with oxidizing flame control and maximum achievable temperatures in excess of 2000°C In this study, liquid precursors to ultra high temperature ceramics (UHTCs) have been developed into multilayer coatings on C-C composites and evaluated using the oxidation testing methods. The tests will be discussed in detail and correlated with preliminary materials evaluation results with the aim of presenting an understanding of the testing environment on the materials evaluated for oxidation resistance.

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Tape casting of magnesium oxide

Corral, Erica L.; Loehman, Ronald E.; Bencoe, Denise N.

A tape casting procedure for fabricating ceramic magnesium oxide tapes has been developed as a method to produce flat sheets of sintered MgO that are thin and porous. Thickness of single layer tapes is in the range of 200-400 {micro}m with corresponding surface roughness values in the range of 10-20 {micro}m as measured by laser profilometry. Development of the tape casting technique required optimization of pretreatment for the starting magnesium oxide (MgO) powder as well as a detailed study of the casting slurry preparation and subsequent heat treatments for sintering and final tape flattening. Milling time of the ceramic powder, plasticizer, and binder mixture was identified as a primary factor affecting surface morphology of the tapes. In general, longer milling times resulted in green tapes with a noticeably smoother surface. This work demonstrates that meticulous control of the entire tape casting operation is necessary to obtain high-quality MgO tapes.

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Ultra high temperature ceramics for hypersonic vehicle applications

Loehman, Ronald E.; Corral, Erica L.; Kotula, Paul G.; Tandon, Rajan T.

HfB{sub 2} and ZrB{sub 2} are of interest for thermal protection materials because of favorable thermal stability, mechanical properties, and oxidation resistance. We have made dense diboride ceramics with 2 to 20 % SiC by hot pressing at 2000 C and 5000 psi. High-resolution transmission electron microscopy (TEM) shows very thin grain boundary phases that suggest liquid phase sintering. Fracture toughness measurements give RT values of 4 to 6 MPam{sup 1/2}. Four-pt flexure strengths measured in air up to 1450 C were as high as 450-500 MPa. Thermal diffusivities were measured to 2000 C for ZrB{sub 2} and HfB{sub 2} ceramics with SiC contents from 2 to 20%. Thermal conductivities were calculated from thermal diffusivities and measured heat capacities. Thermal diffusivities were modeled using different two-phase composite models. These materials exhibit excellent high temperature properties and are attractive for further development for thermal protection systems.

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Processing and Characterizing Alumina/Aluminum Composites with Tailored Microstructures Formed by Reactive Metal Penetration

Corral, Erica L.

In industry, the need to maximize energy efficiency depends on the availability of suitable advanced materials. Ceramic composites are exemplary materials for many advanced engineering applications because they exhibit good thermal stability, oxidation resistance and enhanced toughness. Presently, ceramic composite fabrication processes are costly, often requiring high temperatures and pressures to achieve reasonable densities. Our research is focused on developing a processing technique, that will allow production of alumina/aluminum composites using relatively low temperatures and without the application of an external force, thus reducing the processing costs. Our composites were formed using Reactive Metal Penetration (RMP), which is a process involving the reaction of molten Al with a dense ceramic preform. The result is a near net shape ceramic/metal composite with interpenetrating phases. The volume fraction of metal in the composites was varied by doping an aluminosilicate ceramic preform with silica. For this study we fabricated composites using pure mullite and mullite doped with 23 and 42 weight percent silica, yielding 18, 25, and 30 volume percent metal in the composites, respectively. Optical and Scanning Electron Microscopy were used to characterize the homogeneity and scale of the microstructure. The scale of the microstructure varied with preform composition, the reaction temperature and with secondary heat treatments. Four-point bend testing was used to evaluate the influence of microstructure on strength and reliability. During these studies a gradient in the microstructure was observed, which we further characterized using microhardness testing. Alumina/aluminum composites formed by RMP show higher toughness then monolithic alumina and have the potential for improved reliability when compared to monolithic ceramics.

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16 Results
16 Results