Carbon supported nano-nickel-platinum electrocatalyst samples of Ni-Pt (5wt%)/C were prepared by the colloidal-gelatin method. Transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were used to evaluate the metal particles’ morphology, crystal configuration, superficial element constitution and value. Moreover, cyclic voltammeter was employed to measure the catalytic activity for the electro-catalytic oxidation of methanol in an alkaline medium. The results show that Ni-Pt particles are distributed homogeneously on the carbon, with the particle sizes of 3-6 nm; the Pt doping improves largely the activity of Ni nano-particles, and the peak current density of alloy Ni-Pt(5wt%)/C catalyst reaches 85.6 mA/mg in the solution of 1.0 mol/L NaOH + 1.0 mol/L CH3OH, which is 8.7 times of that of Ni/C, and 15.3% of that of Pt/C. The current of Pt per unit mass is increased obviously.