PtRu/C catalysts were prepared using an aqueous co-impregnation method with NaBH4 as a reducing agent. In order to investigate the effect of the reducing agent concentration, metal ions were reduced in different NaBH4 concentrations for which the molar ratios of NaBH4 to metal ions were controlled to 1, 2, 5, 15, 50, and 250. The electrochemical properties were studied by cyclic voltammetry in a 0.5M H2SO4 solution. The surface compositions and oxidation states of the catalysts were observed by X-ray photoelectron spectroscopy (XPS). According to the X-ray diffraction (XRD) results, Pt (fcc) peak shifts were observed and crystal sizes were calculated. The electro-catalytic activities of the prepared catalysts for methanol electro-oxidation were estimated using linear sweep voltammetry. Unit cell tests were carried out to compare the direct methanol fuel cell performances. The prepared catalysts in various NaHB4 concentrations showed not only different surface compositions but also differences in terms of the particle size and level of dispersion. The proper NaBH4 concentration is the medium range in which both the surface composition and the active metal surface area are optimized. Ratio of NaBH4 to metals at 5 and 15 are the optimum point for methanol electro-oxidation according to the findings of this study.