In order to improve the performance of direct-methanol fuel cell (DMFC) performance, the combinatorial method using a repeated cyclic voltammetry was used to optimize the metal composition for the anodic material and the highly porous carbon, which showed the higher Pt dispersion, was investigated using various characterization tools. The activity of newly-developqd electrocatalyst, Pt(77)Ru(17)Mo(4)W(2), whose composition was determined through high-throughput screening was more active and stable than Pt(50)Ru(50) in methanol electrooxidation. The Pt particles supported on highly porous carbons (C-gl/USY-1 and Csu/MCM-48-2) synthesized with USY zeolite and MCM-48 silica as a template showed the larger electrochemical active surface areas and the higher Pt dispersions, compared to Pt particles supported on Vulcan XC-72R carbon.