MICROSTRUCTURAL INVESTIGATIONS OF SAMARIUM-DOPED ZIRCONIUM DIBORIDE FOR HYPERSONIC APPLICATIONS
thesisposted on 14.05.2019, 18:31 by Anneliese E Brenner
Sharp leading edges required for hypersonic vehicles improve the maneuverability as well as reduce aerodynamic drag. However, due to the sharp design, increased surface temperatures require materials that can withstand these extreme conditions. Ultra-high temperature ceramics are a material group being considered for the leading-edge material, specifically ZrB2/SiC (ZBS) which has a high thermal shock resistance, melting temperature, and thermal conductivity. Studies done by Tan et. al. has shown that adding samarium (Sm) as a dopant to ZBS has an emittance of 0.9 at 1600oC and develop oxide scales that have excellent ablation performance. However, it remained unknown how the Sm doped oxide scale formed as well as how the emittance and ablation performance are affected by the microstructure. This study investigates the oxide scale development of 3 mol% doped Sm-ZBS billets as well as how differences in microstructure affect the emittance and ablation performance. Samples were prepared via chemical infiltration of samarium nitrate into spray-dried powders of 80 vol.% ZrB2/20 vol.% SiC; powders were then pressed into billets and pressureless sintered. Samples cut and polished from these billets were then oxidized for 10, 60, or 300 s, respectively, using an oxyacetylene torch. X-ray diffraction was used to determine the sequence of oxidation of Sm-ZBS, beginning with the formation of ZrO2 and Sm2O3. The final oxide scale was determined to be c1-Sm0.2Zr0.8O1.9, with a melting temperature exceeding 2500oC. SEM and EDS were also used to investigate the microstructural formation that occurs from the bursting of convection cells. Samples with different microstructures revealed similar topographical microstructures post-ablation due to the sequence of the oxide formation. However, samples with rougher surfaces and higher porosities had a higher concentration of trapped glass in the cross-sectional oxide scale. It was also found that due to differences in heating the sample during emittance testing compared to ablation testing, the oxide developed was identical for all the samples. It was also found that variances in microstructure had no effect on the spectral emittance of Sm-ZBS at ultra-high temperatures. The fabrication of c1-Sm0.2Zr0.8O1.9 (SZO) as a bulk billet was also investigated to use as a thermal barrier coating (TBC) in replacement of Sm-ZBS.