Direct methanol fuel cell (DMFC) is one of the ideal powers of low-power portable electrical devices, witch is cheap, safe, easy to store and rich source of fuel, and is more and more attentive and researched in recent years. In this paper, graphite electrode samples were coated by chemical plating Co and then by vacuum ion plating Pt. The microstructure of samples were observed by scanning electron microscope SEM and X-ray fluorescence spectrometry to analyze XRF then determined the surface composition of graphite electrode. The electrocatalysis properties of graphite electrodes were studied by electrochemical impedance spectra (EIS), cyclic voltammeter (CV) and linear sweep voltammeter (LSV). The results show that electrocatalysis properties of methanol on the electrode was stronger as the chemical plating time extended and methanol concentration increase if the parameters of the plating Pt in a vacuum ion plating process was unchanged, and Co Chemical Plating time was shouter than 120s.