A galvanostatic pulse electrodeposition technique of preparing nanoparticulate PtRu electrocatalyst for direct methanol fuel cells has been demonstrated. After extensive cyclic voltammetric analysis, we determined the optimized parameters for the methanol oxidation to be current on-time on 50 ms, current off-time of 400 ms, current density of 50 mA/cm2, and total charge of 8.0 C/cm2. In addition, the catalyst loading was measured at 68 μg/cm2, resulting in a mass; activity of 213 mA/Pt. mg. The composition for the nanoparticles was confirmed as Pt65Ru 35. High-magnification images on the specimen indicated fine particles in 4-20 nm with uniform distributions.