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Abstract: Amorphous catalyst alloy powders in form of Co–P, Co–B, and Co–P–B have been synthesized by chemical reduction of cobalt salt at room temperature for catalytic hydrolysis of NaBH4. Co–P–B amorphous powder showed higher efficiency as a catalyst for hydrogen production as compared to Co–B and Co–P. The enhanced activity obtained with Co–P–B (B/P molar ratio=2.5) powder catalyst can be attributed to: large active surface area, amorphous short range structure, and synergic effects caused by B and P atoms in the catalyst. The roles of metalloids (B and P) in Co–P–B catalyst have been investigated by regulating the B/P molar ratio in the starting material. Heat-treatment at 773K in Ar atmosphere causes the decrease in hydrogen generation rate due to partial Co crystallization in Co–P–B powder. Kinetic studies on the hydrolysis reaction of NaBH4 with Co–P–B catalyst reveal that the concentrations of both NaOH and catalyst have positive effects on hydrogen generation rate. Zero order reaction kinetics is observed with respect to NaBH4 concentration with high hydride/catalyst molar ratio while first order reaction kinetics is observed at low hydride/catalyst molar ratio. Synergetic effects of B and P atoms in Co–P–B catalyst lowers the activation energy (32kJmol−1) for hydrolysis of NaBH4. The stability, reusability, and durability of Co–P–B catalyst have also been investigated and reported in this work. It has been found that by using B/P molar ratio of 2.5 in Co–P–B catalyst, highest H2 generation rate of about ∼4000mlmin−1 g−1 can be achieved. This can generate 720W for Proton Exchange Membrane Fuel Cells (0.7V): which is necessary for portable devices. [Copyright &y& Elsevier]