Synthesis of carbon-supported PtM/C catalysts (M ) Co, Cr, or Fe) using a new preparation technique, a reverse micelle method, is reported. The catalysts were characterized by different surface techniques: X-ray diffraction, scanning electron microscope, transmission electron microscope, and energy dispersive X-ray microanalysis. Surface characterization showed that Pt/M nanoparticles on catalysts were synthesized using the reverse micelle method. Pt/M nanoparticles were observed to be uniform spherical objects. The performance of the PtM/C catalysts was tested by the rotating disk electrode technique.