We report on Co-Mo-B nanoparticles supported on foam Ni as catalysts for hydrogen generation from hydrolysis of ammonia borane (NH3BH3) solution. The Co-Mo-B/foam Ni catalysts with different molar ratios of Co2+ and MoO42- were synthesized via the electroless-deposition technique at ambient temperature. In order to analyze the phase composition, chemical composition, microstructure, and electron bonding structure of the as-prepared samples, powder X-ray diffraction (XRD), inductively coupled plasma-mass spectroscopy (ICP-MS), scanning electron microscopy (SEM), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS) were used. The results showed that Co-Mo-B nanoparticles were variously dispersed on the surface of the foam Ni and the catalytic activity correlated with the molar ratio of Co2+ and MoO42-. The highest hydrogen generation rate was 5331.0 mL min(-1) g(cat)(-1) at 298 K, and the activation energy was calculated to be 45.5 kJ mol(-1) toward the hydrolysis of NH3BH3 solution. The better catalytic activity was largely attributed to the smaller particle size, higher surface roughness and the novel three-dimensional cone-like architectures of the obtained samples. The kinetic results show that the hydrolysis of NH3BH3 is a first-order reaction in catalyst concentration. In addition, the reusability experiment exhibited that the catalytic activity was reduced after 5 cycles and the reason of the decay was also investigated. (C) 2019 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.