A thermal plasma process for the synthesis of nanoparticles and their immediate assembly into nanostructured films is discussed. In this process, known as hypersonic plasma particle deposition, a thermal plasma with injected precursors is expanded through a nozzle to nucleate nanoparticles, which are then inertially deposited onto a cooled substrate in vacuum. A lightly consolidated nanostructured film results. Particle and film diagnostics along with images of the plasma flow are used to explain the formation of nanostructured silicon carbide films by this process.