Vanadium pentoxide gel was synthesized by using sol-gel method,and freezed drying to get the vanadium pentoxide xerogel,which were ammonolyzed to vanadium nitride nanoparticals in high purity anhydrous NH3 atmosphere.The samples were characterized by transmission electron microscope(TEM)and X-ray diffraction(XRD),the vanadium nitride nanoparticles have homogeneous spherical structure with an average diameter of 12 nm,and its crystal structure belongs to face-cubic.