Tantalum carbide (TaC), hafnium carbide (HfC) and compounds in the Ta-Hf-C system have extremely high melting points (> 3700 ℃) making them potential candidate materials for thermal protection structures in next-generation hypersonic vehicles whose leading edges and nose caps have projected operating temperatures above 2000 ℃ in both neutral, oxidising and chemically-aggressive environments.However, a high sintering temperature and pressure have been required to densify monolithic Ta-Hf-C with starting TaC/HfC mixable powders because of its strong covalent bonding and low self-diffusion coefficients.Low-temperature densification of ceramics can be improved by refining the raw powder.In this paper, highly dispersed single phase Ta-Hf-C solid solution powders were synthesized by solvothermal treatment and carbothermal reduction reactions from an inorganic hybrid.The mean crystallite size of Ta-Hf-C particles was less than 100 nm, and the composition of Ta, Hf and C elements was near stoichiometric and homogeneously distributed in the powder samples.