Abstract: The micrometer material of NH<sub<4</sub<NiPO<sub<4</sub<·H<sub<2</sub<O was synthesized by solid state reaction at low temperature using ammonium dihydrogen phosphate and nickel acetate as raw materials and PEG-400 as a template as well as adding a few sodium hydroxide. The optimum reaction condition was researched by using XRD and cyclic voltammetry. The reaction product was characterized by using SEM, FT-IR and TG-DTA. It was found that the perfect crystal material could be easily obtained when the reaction time is 4 hour, the reaction temperature is 70 ℃ and the weight of nickel acetate is 4 times to the weight of sodium hydroxide. The product has been applied to make electric catalytic electrode. The research shows that, compared to the graphite base Pt/C electrode and graphite base Pt/C/NH<sub<4</sub<NiPO<sub<4</sub< electrode, the glassy carbon base Pt/C/NH<sub<4</sub<NiPO<sub<4</sub< electrode has better electro-catalytic activity. Also, the glassy carbon base Pt/C/NH<sub<4</sub<NiPO<sub<4</sub< electrode has the potential to replace other electrodes for ethanol electrocatalytic oxidation, as it has the characteristics of large oxidation current in an instant, low oxidation potential and certain electric capacity.