Mechanically alloyed Co-20wt%Ni-10wt%Mo and Co-70wt%Ni-10wt%Mo (nominal compositions) alloy powders were produced by milling of pure elemental powders. Mechanically alloyed powders were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. MA powder specimens were tested electrollitically in a 30% KOH aqueous solution at 298 K. X-ray diffraction analysis and transmission electron microscopy of milled powders showed the presence of two phases, an fcc solid solution and intermetallic compounds of Ni or Co with Mo. These phases showed a nanometric size. The linear sweep voltammograms confirmed also the presence of two phases in both mechanically alloyed alloy powders. The Co-20wt%Ni-10wt%Mo alloy powders showed the best electrocatalytic activity for hydrogen evolution reaction. (C) 2003 Kluwer Academic Publishers.