The amorphous Co-Ni-P films were electroplating on Cu sheets. The effects of NiSO4 concentrations on the deposit plating rate and the catalytic activities for NaBH4 hydrolysis were investigated. The surface morphology and phase structure of the deposited Co-Ni-P films were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. The composition was analyzed by energy dispersive spectrometer (EDX). Experimental results showed that adding NiSO4 in Co-P bath could increase the deposition rate. When 0.01 M of NiSO4 was used, the highest deposition rate and the highest hydrogen generation rate of 3636 mL (min g-catalyst)(-1) were obtained. The activation energy (E-a) for the NaBH4 hydrolysis was 38 kJ mol(-1), which was comparable to the value of noble metal catalysts. (C) 2013 Elsevier B.V. All rights reserved.