10%Nb2O5·nH2O-20%Pt/C electrocatalyst for methanol oxidation was prepared by a deposition method, and it was heat treated in Ar atmosphere. The effects of heat treatment on morphology, microstructure and electrochemical performances were characterized by XRD, HRTEM, cyclic voltammetry and chronoamperograms. The results show that with the increase of heat-treatment temperature, the size of Pt particles is increased, and the catalytic performance becomes higher. In comparison with the 20%Pt/C without heat treatment, the catalytic performance of 10%Nb2O5·nH2O-20%Pt/C with heat treatment at 700 oC for methanol oxidation is best. Its initial potential of methanol oxidation is reduced by 150 mV, and the peak current for methanol oxidation is increased by 2.48 times