Cobalt-phosphorus (Co-P) catalysts, which were electroless deposited on Cu sheet, have been investigated for hydrogen generation from alkaline NaBH4 solution. The microstructures of the as-prepared Co-P catalysts and their catalytic activities for hydrolysis of NaBH4 are analyzed in relation to pH value, NaH2PO2 concentration, and the deposition time. Experimental results show that the Co-P catalyst formed in the bath solution with pH value of 12.5, NaH2PO2 concentration of 0.8 M, and the deposition time no more than 6 min presents the highest hydrogen generation rate of 1846 mL min(-1) g(-1). Furthermore, the as-prepared catalyst also shows good cycling capability and the corresponding activation energy is calculated to be 48.1 kJ mol(-1). The favorable catalytic performance of the electroless-deposited Co-P catalysts indicates their potential application for quick hydrogen generation from hydrolysis of NaBH4 solution. (C) 2009 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved.