Nano-sized of Pt and PtRu particles on solid polymer electrode (SPE) membrane were prepared by the modified Takenaka-Torika (T-T) method. The morphological characteristics and catalyst compositions were also studied on the Pt- and PtRu-SPEs. The electrodes were characterized using electrochemical measurements, scanning electron microscope with electron dispersive microscope (SEM-EDX) and X-ray diffraction analysis. The well-dispersed Pt and PtRu alloy nanoparticles with crystallite size of 12-6 nm were obtained in the preparation. The differences in morphology of the nano-, micro-structure and composition of these catalysts effected the electro-catalytic activity of methanol electro-oxidation reaction. The electrochemical result showed that the mole ratio between Ru and Pt at 0.10 was the best condition for the methanol electro-oxidation reaction in partial cell study.