Electrodeposited zinc-nickel alloys of various compositions were prepared. A suitable electrolyte and conditions to produce alloys of various compositions were identified. Alloys produced on electroformed nickel foils were etched in caustic to leach out zinc and to produce the Raney type, porous electro catalytic surface for hydrogen evolution. The electrodes were examined by polarization measurements, to evaluate their Tafel parameters, cyclic voltammetry, to test the change in surface properties on repeated cycling, scanning electron microscopy to identify their microstructure and X-ray diffraction. The catalytic activity as well as the life of the electrode produced from 50% zinc alloy was found to be better than others. (C) 2002 International Association for Hydrogen Energy. Published by Elsevier Science Ltd. All rights reserved.