The Au-M (M = Fe, Co, Ni, Cu and Zn) bimetallic nanoparticles supported on the Vulcan XC-72R (Au-M/C) were synthesized by a reverse micelle method. The structures and compositions of the carbon supported Au-M catalysts were characterized by X-ray diffraction (XRD), energy dispersive X-ray analysis (EDS). The electrocatalytic activity of the Au-M bimetallic nanoparticles with respect to borohydride electro-oxidation for the application of fuel cell was investigated by voltammetry, chronoamperometry and chronopotentiometry. The results showed that alloying Au with 3d transition metals Fe, Co, Ni, Cu or Zn, a metal that leads to the maximum eight-electron oxidation of BH4- not only improved the electrode kinetics of BH4- oxidation but also reduced catalyst cost. Among the various investigated Au-M/C electrocatalysts, the Au-Zn, Au-Fe and Au-Cu catalysts showed no activity of NaBH4 hydrolysis, and Au-Zn presented an attractive catalytic activity for borohydride oxidation. Copyright (C) 2012, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.