Cobalt-Boron (Co-B) catalysts are prepared on the nickel foam substrate (NiFS) by in situ reduction of Co2+ ions in sodium borohydride (NaBH4) solution for the catalytic generation of hydrogen from NaBH4. The formation of Co-B catalysts on the substrate is much faster by using a dip-coating and extended drying ("dry-dip-coating method") followed by chemical reduction as compared to that prepared by a conventional dip-coating method followed by chemical reduction. The dry treatment results in a significant reduction in the re-dissolution of the dip-coated Co-B catalysts during the following dipping processes. Co-B catalysts on I'd modified NiFS have also been prepared using dry-dip-coating method. The factors affecting the performance of the catalysts such as dipping time, calcination temperature, Co-B loadings, Pd formation time and operating temperature, are studied. The best catalytic activity and stability is obtained on Co-B on Pd modified NiFS. (C) 2008 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights reserved.