Solid-state composites of NaBH4 and Co-based catalyst have been fabricated for hydrogen generation via a novel mechanochemical technique, i.e. the high-energy ball milling, in which the gravimetric storage capacity of hydrogen has reached 6.7 wt%, meeting the 2010 target of at least 0.06 kg H-2/kg set by the U.S. Department of Energy (DOE). The active catalysts used in the hydrolysis reaction of sodium borohydride for hydrogen generation are mainly cobalt oxides. Controlled addition of water, namely water used as a limiting agent, to the solid composites of NaBH4 and Co-based catalyst greatly improves the H-2 storage capacity and resolved the issues of low gravimetric H-2 storage in conventional aqueous system of sodium borohydride. Factors influencing the performance of hydrogen production such as amounts of H2O added, catalyst loadings and durations of ball-milling processes are investigated. Moreover the hydrolyzed products of NaBH4 and spent catalysts are analyzed as well. (C) 2010 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved.