Abstract: Nickel ferrite wet gelatin was prepared by citrin coordination method firstly, and then the precursor prepared via azeotropic distillation process was directly heated on a electric cooker and ignited at low temperature to prapare the nickel ferrite powders, which were characterized by X-ray diffraction, Transmission electronic microscopy (TEM) and laser scattering particle size analyzer. The results show that the nickel ferrite powders prepared by using azeotropic distillation process to dehydrate a mount of free water had single spinel structure, uniform and well-dispersed particles, and the particles diameter was 80-100 nm.