CeNi5 and Ni3Sn2 were prepared from NiO-CeO2 and NiO-SnO2 oxides by electro-deoxidization (FFC). The samples of mixed oxides sintered at different temperatures were used as cathode, and the graphite rod was used as anode. Then the reaction was completed under 3.1 V in the CaCl2 solution at 850 oC. The morphology and phase composition of the samples before and after deoxidization were analyzed by SEM and XRD. Results show that the sample has lower porosity and smaller electro-deoxidization current under the condition of higher sintering temperature. The product from samples sintered at different temperatures was pure CeNi5; the product from samples sintered at lower temperature was pure Ni3Sn2 with loose sponginess. The research provides a new method for cell materials preparation