Co-Cu-B, as a catalyst toward hydrolysis of sodium borohydride solution, has been prepared through chemical reduction of metal salts, CoCl2 center dot 6H(2)O and CuCl2, by an alkaline solution composed of 7.5wt% NaBH4 and 7.5wt% NaOH. The effects of Co/Cu molar ratio, calcination temperature, NaOH and NaBH4 concentration and reaction temperature on catalytic activity of Co-Cu-B for hydrogen generation from alkaline NaBH4 solution have been studied. X-ray diffraction (XRD), scanning electron microscope (SEM) and Nitrogen adsorption-desorption isotherm have been employed to understand the results. The Co-Cu-B catalyst with a Co/Cu molar ratio of 3:1 and calcinated at 400 degrees C showed the best catalytic activity at ambient temperature. The activation energy of this catalytic reaction is calculated to be 49.6 kJ mol(-1). (C) 2010 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved.