A method for preparing Nickel-based skeletal catalyst as well as its characterization is reported. The catalyst has an intended use as a cathode in alkaline electrolysis. Skeletal catalyst electrodes were synthesized from equal weights (50% each) of aluminum and nickel powders. The catalyst was prepared with metal powders which were melted in an induction oven, allowing the alloy to solidify at room temperature to obtain the thermodynamically-stable phases of the alloy. Samples from the resulting alloy went through a leaching process in an alkaline solution using two different leaching times. After leaching, porous and amorphous electrodes were obtained and then subjected to a slow oxidative stage to avoid ignition. The structure, composition, morphology and electrochemical characteristics of the electrodes were studied. The leached samples showed a high exchange current density indicating that are good catalysts for the Hydrogen Evolution Reaction (HER), a property enhanced by the adsorption of hydrogen during the leaching process which facilitated the hydrogen reduction overall reaction. (C) 2010 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved.