Two types of Pt- and Ni-based alloy catalysts were synthesized and comparatively tested for hydrogen generation from aqueous borazane (ammonia- borane, BH(3)NH(3)) solution. The experimental results demonstrated that hydrogen release rates from some of the Pt alloys such as PtRu and PtAu are nearly 9 times higher than those from pure Pt surface, and similarly, most of the Ni alloy catalysts exhibit greatly enhanced catalytic activities than pure Ni catalyst. Particularly, hydrogen release from NiAg-catalyzed BH(3)NH(3) hydrolysis can complete quickly at room temperature showing a stable hydrogen yield at H(2)/BH(3)NH(3) ratio = 2.9 (molar ratio), corresponding to 8.7 wt % hydrogen release. Since the Ni alloy catalysts are less costly and highly efficient, it is feasible to use the Ni alloy catalysts for practical hydrogen generation in portable applications. (c) 2008 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights reserved.