It has been shown using X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, energy dispersive X-ray spectroscopy, and elemental analysis that phase-pure VB 2 with an average particle size in the range 20-35 nm can be prepared in the temperature range 595-930°C by reacting vanadium(III) chloride and sodium borohydride in the molar ratio 1 : 10 in an argon atmosphere for 14-28 h.