MPd (M = Co, or Cu) nanoparticles (NPs) were synthesized by borane-amine reduction of metal acetylacetonates. The size of the MPd NPs was controlled at 3.5 nm and their compositions were tuned by the molar ratios of the metal precursors. These MPd NPs were active catalysts for electrochemical oxidation of formic acid and the Cu30Pd70 NPs showed the highest mass activity at 1192.9 A gPd(-1), much higher than 552.6 A gPd(-1) obtained from the 3.5 nm Pd NPs. Our synthesis provides a facile route to MPd NPs, allowing further investigation of MPd NP catalysts for electrochemical oxidation and many other chemical reactions.