Development of electrocatalyst with higher electrochemical activity, better stability and low cost are extremely desirable for hydrogen production. In this work, nanostructure NiCeO2Gd doped nanocomposite deposited on copper foam by pulse electrodeposition method was used as electrocatalyst for hydrogen evolution reaction (HER). SEM, TEM, EDAX, XRD and XPS were used to characterize the surface morphology, chemical composition, preferred orientation and oxidation states of the as-prepared Ni and Ni-CeO2Gd doped nanocomposite. The electrocatalytic activity and stability of the Ni and Ni-CeO2Gd doped nanocomposite for HER were investigated by Linear Sweep Voltammetry (LSV). The results show that Ni-CeO2Gd doped nanocomposite exhibits higher catalytic activity with low onset overpotential (160 mV), lower Tafel slope (102 mV/dec) and larger exchange current density (0.1231 mA cm(-2)) than nickel. Ni-CeO2Gd doped nanocomposite is highly promising as a new material for the excellent electrocatalytic activity in hydrogen production process. (C) 2017 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.