Considering the synergy effect between g-C3N4 and Ti-Fe2O3, the novel g-C3N4/Ti-Fe2O3 heterojuncted hybrids are constructed. g-C3N4 nanoparticles are prepared from bulk g-C3N4 via corrosion by strong acid and alkali, respectively, and then deposited onto Ti-Fe2O3 nanosheets. The physical and optical properties of the g-C3N4 modified Ti-Fe2O3 are characterized and the effect of g-C3N4 on the photoelectrochemical performance is studied. The photoelectrochemical activity of the Ti-Fe2O3 nanosheets is significantly enhanced upon the incorporation of g-C3N4 nanoparticles under visible light irradiation. The improved photoelectrochemical performance is ascribed to the synergy effect at the interface of the g-C3N4. and Ti-Fe2O3, including favorable contact, matched energy band levels of the two semiconductors and enhanced charge separation. Possible mechanism is proposed for the high photoelectrochemical activity of g-C3N4/Ti-Fe2O3 to guide the design of photoelectrodes. Copyright (C) 2016, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.