The vanadiumdoped ZnO nanopowder (the atomic fraction of V is 2.5%) has been prepared by the SolGel method. The effects of different heat treatment processes on the crystal structure and morphology of the samples were investigated. The nanopowder was characterized by Xray diffraction (XRD) and scanning electron microscopy (SEM). The results show that the crystal structure of vanadiumdoped ZnO nanopowder is seriously affected if the temperature of the heat treatment is too low or the treatment time is too short. In addition, the grain size increases with the increase of heat treatment. The XRD shows that all the samples have hexagonal wurtzite structure and all of which are (101)preferred orientation. The grain sizes of the sample are in the range of 65~138 nm by SEM. In the samples of each process, the doping is uniform, the V content is basically the same as the design value, and the samples contain only three elements of Zn, V and O.