In this paper, ascorbic acid as combustion agent, composite oxides of nickel ferrite were prepared by combustion method. The optimal molar ratio of ferric nitrate to nickel nitrate was determined by XRD. The UV absorbance properties of composite were analyzed by UV spectra. The morphology of composites was characterized by scanning electron microscopy. The photocatalytic properties were studied using methylene blue as the degradation substrate and composite as catalyst. The experiment showed important effect of amount of catalyst, the pH value of the solution, the amount of hydrogen peroxide and irradiation time of the photocatalyst. The optimal photocatalytic condition is: dose of catalyst 20 mg, pH at 6, and hydrogen peroxide 6 mL. The results indicate that the nickel ferrite with molar ratio of nickel nitrate, ferric nitrateand ascorbic acid of 1:2:1 is photocatalytic effective under UV and visible light. Moreover, the nickel ferrite with molar ratio of nickel nitrate, ferric nitrateand ascorbic acid of 2:1:1 and 1:3:1 are photocatalytic effective under UV light.