Abstract: Methanol-hydrogen peroxide single chamber fuel cell is a proton-free exchange membrane fuel cell with methanol as anode and hydrogen peroxide as cathode. Compared with traditional fuel cells, this fuel cell has lower cost, higher energy efficiency and is easy to miniaturize and integrate. It is regarded to be a promising research field. In this paper, Pt-based polymetallic catalysts with modified graphene oxide, carbon black XC-72 and modified XC-72 as carriers were prepared by different preparation methods. The effects of support types, metal components and preparation methods on the catalytic activity of catalysts for methanol electrooxidation were investigated. It was found that Z-PtNi prepared by hydrothermal synthesis method using carbon black XC-72 as carrier had the highest activity. The results provided a direction for the development of methanol anode catalyst and also the development of methanol hydrogen peroxide single chamber fuel cell system.