The supported amorphous alloy catalysts Ni-Co-P/gamma-Al2O3 were synthesized by electroless plating for hydrogen generation from catalytic hydrolysis of sodium borohydride solution. The influences of deposition time, pH, NaBH4 concentration and the Co/Ni atomic ratio on the hydrogen generation rate were investigated in this paper. The reported work also includes the full experimental details for the collection of a wealth of kinetic data to determine the activation energy (E-a = 52.05 kJ mol(-1)). Energy dispersive X-ray spectrometer (EDS), field emission scanning electron Microscope (SEM), inductively coupled plasma-atomic emission spectrometer (ICP-AES) and X-ray diffraction (XRD), nitrogen adsorption -desorption isotherm were used to characterize surface element composition, morphology and structure of the amorphous alloy. Copyright (C) 2014, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.