A new method for preparing V2O5 powders has been developed, which is based on decomposition of gas-phase VOCl3 in O-2/Ar/H-2 microwave plasma generated at the atmospheric pressure. The samples taken from different positions of the plasma reactor were the nano-structured powder, which was yellow and typical nano-sized particles, and the micro-structured powder, which was yellowish orange, had large carpet-or sponge-like areas, and was composed of a bundle of V2O5 needles. These two samples have been analyzed by EDX, SEM, XRD, Raman and TEM. (c) 2005 Elsevier B.V. All rights reserved.