Reduction of vanadium(III) oxide with boron carbide and nanofibrous carbon in an induction furnace in argon was used to obtain a highly dispersed vanadium diboride powder. The characteristics of vanadium diboride powders were studied by various analytical methods. It was found that the material obtained contains only a single phase, vanadium diboride, with powder particles mostly aggregated, the average size of particles and aggregates being 9.8 μm at a wide particle size distribution. The optimal synthesis parameters were determined: V2O3: B4C: C ratio corresponding to the stoichiometry, temperature 1700°C, and keeping time 20 min.