NiCr nano oxides have been synthesized by impregnation method and were used as the anode electrocatalysts for direct methanol fuel cell(DMFC). The catalysts were characterized by X-ray diffraction(XRD) and scanning electron microscopy(SEM). The activity of catalysts with different metal molar ratios and calcination temperatures on the methanol oxidation reaction were investigated by cyclic voltammetry(CV) and bulk electrolysis with coulometry. The results show that the NiCr nano oxides calcined at 500°C for 6h gave an excellent electrocatalytic performance in the anodic oxidation of methanol.