Pt–Au nanoparticles supported on carbon aerogel, namely 2:1 has been synthesized by the microwave-assisted polyol process. The structure of Pt–Au nanoparticles is characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The electrochemical property of Pt–Au catalysts for methanol oxidation is evaluated by cyclic voltammetry (CV). The results show that Au-modified Pt catalysts exhibit a high methanol tolerance and improved electrochemical catalytic activity, suggesting that carbon aerogel supported Pt–Au catalysts are better catalysts for the electrochemical oxidation of methanol than conventional Pt catalysts.