The aim of the research was to obtain superfine homogeneous composite powders, which, due to their unique composition and morphology, will be used to obtain ceramics with improved properties for the thermal protection of supersonic aircraft. The novelty of research was microstructure refining methods, selection of sintering additives/dopants and their combining action. As regards sintering additives and dopants, B4C and graphite powder, carbon black and graphene structures were used. The use of the latter individually and in combination sintering additives was one of the innovations of the research. Several variants of zirconium boride nano powder with different stoichiometry and graphene nanostructures were produced by us. Composite nano powders were made on the basis of zirconium boride and silicon carbide. Scanning electron microscopy with Energy-dispersive X-ray spectroscopy method was used to study the mentioned composite micro and nano powders.