Nanoparticles of mixed oxides of Fe and Ni are prepared by a low temperature coprecipitation method. The effects of Ni content in synthesized nanoparticles on the electrocatalysts performance for hydrogen evolution reaction are investigated by electrochemical techniques. Scanning electron microscopy and X-ray diffraction spectroscopy are used for studying the morphology and structure of Ni-ferrite nanoparticles (NPs). Electrocatalytic activity of Ni-ferrite NPs for hydrogen evolution reaction is found to increase in the order of Fe3O4 <= Ni0.6Fe2.4O4 < Ni0.2Fe2.8O4 <= Ni0.8Fe2.8O4 < Ni0.4Fe2.6O4. The Tafel slopes for the hydrogen evolution reaction are found to be between 97.75 mV dec(-1) and 122.19 mV dec(-1) on carbon paste electrodes modified with ferrite NPs and kinetic parameters show that the Volmer step must control the hydrogen evolution reaction. The electrodes are resistive to passivation and they can be renewed easily. (C) 2012 Elsevier Ltd. All rights reserved.