Abstract: Negative thermal expansion ZrV2O7 powders were prepared by wet chemical method, hydrothermal method and water bath method, respectively; The purity and morphology of the powders prepared by different methods were studied, as well as the effects of calcination temperature on purity and morphology. The results show that ZrV2O7 powders couldn′t be prepared by water bath method, but could be successfully preapared by the other methods, and the purity of ZrV2O7 powders prepared by hydrothermal method and wet chemical method was high, and the preparation efficiency of the latter was higher. The purity of ZrV2O7 powders increased and then increased with the increase of calcination temperature; When calcination temperature was 750 ℃, the purity of the powders prepared by hydrothermal method was the best, 97.95%, acicular and clubbed particles and the particles with smooth surface completely disappeared.