Carbon fiber-containing refractory high-entropy ceramic matrix composites (C/RHECs) were fabricated through a reaction with carbon powders, transition metal carbides, and Zr–Ti alloys as a novel heat resistant material used for components of hypersonic vehicles cruising at Mach 7–10. With the infiltration of alloys at 1750 °C into a composite preform containing carbon and carbide powders for 15 min, a high-entropy matrix was successfully formed in situ. Arc-jet tests were conducted in the temperature range of 1800–1900 °C. Results showed the formation of an oxidized region composed of complex oxides, such as (Zr, Hf)O2, (Nb, Ta)2(Zr, Hf)6O17, (Zr, Hf)TiO4, and Ti(Nb, Ta)2O7, with an average thickness of ~600 μm, under which an unoxidized region remained. The porous oxidized region resulted from the evolution of CO(g) during oxidation, while a dense oxide region formed as the outermost region. This indicates that the dense oxide region acted as a barrier to oxygen diffusion for the unoxidized region during oxidation.
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