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Transition metallic catalysts with high performance and low cost are attractive for portable hydrogen systems using sodium borohydride.The catalyst used in this study is Fe-Co supported on Ni powder.Surface morphology and structural characteristic were studied using X-ray diffraction (XRD), scanning electron microscopy (SEM), cyclic voltammograms (CV) and X-ray photoelectron spectroscopy (XPS).Different weight ratios of Fe-Co/Ni catalysts were prepared by chemical reduction of cobalt and iron salts with sodium borohydride under vacuum treatment.The effect of weight ratio on hydrogen generation rate was also investigated.Results show that hydrogen generation rate is the highest when the metal loading is 67 wt%, meanwhile it has porous morphology to enhance the activity of catalyst.