Non-noble Cu@FeCo core-shell nanoparticles (NPs) containing Cu cores and FeCo shells have been successfully in situ synthesized via a facile chemical reduction method. The NPs exerted composition-dependent activities towards the catalytic hydrolysis of ammonia borane (NH3BH3, AB). Among them, the [email protected] NPs showed the best catalytic activity, with which the max hydrogen generation rate of AB can reach to 6674.2 mL min(-1) g(-1) at 298 K. Kinetic studies demonstrated that the hydrolysis of AB catalysed by [email protected] NPs was the first order with respect to the catalyst concentration. The activation energy (Ea) was calculated to be 38.75 kJ mol(-1). Furthermore, the TOF value (mol of H-2. (mol of catalyst. min)(-1)) of [email protected] NPs was 10.5, which was one of the best catalysts in the previous reports. The enhanced catalytic activity was largely attributed to the preferable synergistic effect of Cu, Fe and Co in the special core -shell structured NPs. Copyright (C) 2013, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.