Pt-RuO2 catalysts in the form of pure powder or supported on carbon powder (Vulcan XC72) substrate were prepared by thermal decomposition of polymeric precursors. Catalysts displaying different metal compositions were prepared in order to investigate the influence of catalyst composition. XRD and EDX analyses were employed to determine the composition and crystallinity of the materials. Catalyst morphology was investigated by SEM and TEM. Evaluation of the catalytic activity of the materials toward methanol oxidation was performed in half-cell experiments by cyclic voltammetry and in a single direct methanol fuel cell (DMFC). Electrochemical experiments showed that the catalytic activity of the mixed electrodes toward methanol oxidation is higher than that of Pt alone. Particle dispersion on the carbon substrate and catalyst composition influences their performance toward methanol oxidation. Results indicated a low power density, but the thermal decomposition of polymeric precursors seems to be a promising method to prepare catalysts supported on carbon powder that can be applied to DMFC. (c) 2005 Elsevier B.V. All rights reserved.