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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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Ceramic-Metal Brazing, From Fundamentals to Applications: A Review of Sandia National Laboratories Brazing Capabilities, Needs and Opportunities

Hosking, F.M.; Cadden, Charles H.; Stephens, John J.; Glass, Sarah J.; Johannes, Justine E.; Kotula, Paul G.; Lapetina, Neil A.; Loehman, Ronald E.; Swiler, Thomas P.; Webb, Edmund B.

The purpose of the report is to summarize discussions from a Ceramic/Metal Brazing: From Fundamentals to Applications Workshop that was held at Sandia National Laboratories in Albuquerque, NM on April 4, 2001. Brazing experts and users who bridge common areas of research, design, and manufacturing participated in the exercise. External perspectives on the general state of the science and technology for ceramics and metal brazing were given. Other discussions highlighted and critiqued Sandia's brazing research and engineering programs, including the latest advances in braze modeling and materials characterization. The workshop concluded with a facilitated dialogue that identified critical brazing research needs and opportunities.

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Report on the Fracture Analysis of HfB{sub 2}-SiC and ZrB{sub 2}-SiC Composites

Loehman, Ronald E.

Hafnium diboride-silicon carbide (HS) and zirconium diboride-silicon carbide (ZS) composites are potential materials for high temperature, thermal shock applications such as for components on re-entry vehicles. In order to establish material constants necessary for evaluation of in situ fracture, bars fractured in four-point flexure were examined using fractographic principles. The fracture toughness was determined from measurements of the critical crack sizes and the strength values and the crack branching constants were established to use in forensic fractography for future in-flight tests. The fracture toughnesses range from about 13 MPam{sup 1/2} at room temperature to about 6 MPam{sup 1/2} at 1400 C for ZrB{sub 2}-Sic composites and from about 13 MPam{sup 1/2} at room temperature to about 4 MPam{sup 1/2} at 1400 C for HfB{sub 2}-SiC composites. Thus, the toughnesses of either the HS or ZS composites have the potential for use in thermal shock applications. Processing and manufacturing defects limited the strength of the test bars. However, examination of the microstructure on the fracture surfaces shows that the processing of these composites can be improved. There is potential for high toughness composites with high strength to be used in thermal shock conditions if the processing and handling are controlled.

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Joining SI3N4 for Advanced Turbomachinery Applications

Glass, Sarah J.; Loehman, Ronald E.; Hosking, F.M.; Stephens, John J.; Vianco, Paul T.; Neilsen, Michael K.; Walker, Charles A.

The main objective of this project was to develop reliable, low-cost techniques for joining silicon nitride (Si{sub 3}N{sub 4}) to itself and to metals. For Si{sub 3}N{sub 4} to be widely used in advanced turbomachinery applications, joining techniques must be developed that are reliable, cost-effective, and manufacturable. This project addressed those needs by developing and testing two Si{sub 3}N{sub 4} joining systems; oxynitride glass joining materials and high temperature braze alloys. Extensive measurements were also made of the mechanical properties and oxidation resistance of the braze materials. Finite element models were used to predict the magnitudes and positions of the stresses in the ceramic regions of ceramic-to-metal joints sleeve and butt joints, similar to the geometries used for stator assemblies.

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Strength and toughness of ceramic-metal composites prepared by reactive hot pressing

Loehman, Ronald E.

Metal-reinforced Al{sub 2}0{sub 3}-matrix composites were prepared using reactive hot pressing. The volume fraction of the reinforcing phase was controlled by the stoichiometry of the particular displacement reaction used. Dense Al{sub 2}0{sub 3}-Ni and Al{sub 2}O{sub 3}-Nb composites were fabricated using this technique. The best combination of strength, 610 MPa, and toughness, 12 MPam{sup 1/2}, was found for the Al{sub 2}O{sub 3}-Ni composites. Indentation cracks and fracture surfaces showed evidence of ductile deformation of the Ni phase. The Al{sub 2}O{sub 3}-Nb composites had high strength, but the toughness was lower than expected due to the poor bonding between the Nb and A1{sub 2}0{sub 3}phases.

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24 Results
24 Results