Abstract: V₂O₅ nano-powders were prepared by sol-gel method with ammonium metavanadate, urea, acetylacetone, ammonium tungstate, ammonia solution, methyl orange, deionized water and nickelnitrate as raw material, and the Ni doped V₂O₅ nano-powders and NiO/V₂O₅ nano-powders were prepared.XRD were used to study the influences of different prepared method and doping amount on V₂O₅ structure.Also, the effect on the performance of photocatalytic degradation of methyl orange of the nano-powders prepared by different method was studied.The results indicate that while prepared by the first method, the grain size of the powders increased, when the doped amount was 4%, the maximum degradation rate was 51%.The NiO/V₂O₅ powders prepared by the second method appeared much smaller grain size for NiO inhibitting grain size grown, and no second phase was discovered except NiO and V₂O₅.While the doped amount was 4%, the maximum degradation rate was 68.21%.