Electrophoretic deposition (EPD) technique is employed for fabricating Fe2O3 film on the Ni substrate, electroplating technology is used to deposite Ni from the Fe2O3 film, and Ni-Fe2O3 composite coating with high mass fraction of Fe2O3 is obtained. The impact of deposition voltage on the thickness of Fe2O3 film is investigated, Ni-Fe2O3 film sintering performance at high temperature and its oxidation mechanism are also studied. Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), EDS and X-ray diffraction(XRD) are used to characterize the deposited films. The results show that by changing the electric field or the distanc between the anode and cathode, Fe2O3 electrophoretic deposition thickness will change a lot. After heat processing at a certain temperature, the organic matter in the deposition layer is removed clean. The binding interface between the Ni-Fe2O3 coating and the substrate is closely and completely. After the oxidation of composite deposition layer at 1 000 ℃ high temperature, the material of nickel-iron spinel structure is obtained.