This work is devoted to the preparation and characterization of the spinel Ni prepared by nitrate route and its application for the hydrogen evolution under visible illumination. The X-ray diffraction revealed a cubic symmetry and a crystallite size of 40 nm, determined from the full width at half maximum. The oxide possesses a forbidden band of 1.84 eV and the transport properties indicate p-type conduction. The photo-electrochemical characterization gives a conduction band of -1.79 V-SCE and the spinel is tested with success for the hydrogen formation under visible irradiation (29 mW cm(-2)). An evolution rate of 65 mu L g(-1) min(-1) and a quantum yield of 0.15% are obtained within 30 min under optimal conditions (0.5 mg of catalyst/mL, pH similar to 12 and 50 degrees C) in presence of SO32- as holes scavenger. (c) 2017 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.