Vanadium sesquioxide (V2O3) nanopowder was successfully prepared by the solid phase reaction of themixture of vanadyl hydroxide (VO(OH)2) and ammonium chloride (NH4Cl) at 500 ℃. The as-obtained samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). V2O3 nanoparticles were well dispersed and displayed sphere-like particles with diameters in the range of 30~50 nm.