A novel method to prepare an electrocatalyst with a new structure and high catalytic performance was reported. Two-dimensional (2D) PtRu nanoclusters have been successfully deposited on graphene oxide and carbon black supports. Compared with the commercial 3D E-TEK PtRu samples, the prepared 2D PtRu composites have larger electrochemically active surface area and display much higher catalytic activity toward methanol oxidation reaction. The preparation method mainly includes the following procedures: oxidation of carbon matrix, Pb2+ adsorption on the surface of carbon support, Pb2+ electrochemical reduction and galvanic displacement of Pb0 by Pt2+ and Ru3+. The method developed in this study could be viable for solving the problem of low electrocatalytic activity in direct methanol fuel cell anodes.