Objective To optimize the preparation process of Cu-Co-P amorphous alloy and to study its catalytic performance for hydrogen generation in the hydrolysis of sodium borohydride. Methods The amorphous alloy Cu-Co-P was prepared on iron sheets by electroless deposition method. The effects of bath composition on deposition rate, bath stability and coating quality were investigated. The optimized formulation was screened out based on the research results. The supported amorphous alloy catalysts Cu-Co-P/ γ-Al2O3 were synthesized according to the optimized formulation. The composition, surface morphology and phase structure of the deposited Cu-Co-P / γ-Al2 O3 catalyst were characterized. The catalytic properties of the prepared multiple amorphous alloy catalysts Cu-Co-P were investigated using the hydrolysis reaction of sodium borohydride solution. Results The BET surface area of the obtained supported Cu-Co-P / γ-Al2 O3 amorphous alloy catalyst was 233 m2 / g, and it contained 57. 85wt% Cu, 39. 69wt% Co and 2. 46wt% P. A hydrogen generation rate of 1295 mL / (g·min) was achieved at 45 ℃ by hydrolysis of NaBH4 solution containing 1 g NaBH4 and 1 g NaOH. Conclusion The optimized electroless plating formulation of Cu-Co-P was 20 g / L cobalt sulfate heptahydrate, 0. 7 g / L copper sulfate pentahydrate, 40 g / L sodium hypophosphite monohydrate, 20 g / L trisodium citrate dehydrate, 10 g / L ethylenediamine tetraacetic acid disodium salt and 25 g / L ammonium fluoride. The process was controlled at (85±1) ℃ and pH = 9.