Using non-toxic red phosphorus as the phosphorus source, Ni2P was synthesized and in situ loaded on Cd0.5Zn0.5S photocatalyst by a simple solvothermal method for photocatalytic H-2 evolution under visible light (lambda >= 420 nm) irradiation. The as-prepared samples were characterized by X-ray diffraction (XRD), Xray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM), ultraviolet-visible diffuse reflectance spectra (UV-Vis DRS), Brunauer-Emmett-Teller (BET) surface area measurements and electrochemistry techniques. The photocatalytic hydrogen evolution activity over Cd0.5Zn0.5S is significantly increased by in situ-loaded Ni2P due to the intimate interface contact and efficient charge transfer from Cd0.5Zn0.5S to Ni2P. The 4 wt% Ni(2)Ploaded Cd0.5Zn0.5S photocatalyst shows five times higher H-2 evolution rate than that of the pristine Cd0.5Zn0.5S. The highest H-2 evolution rate of 65.6 lmol/h and the apparent quantum yield (AQY) of 29% at 420 nm is achieved under the optimized conditions. The noble metal free Ni2P is stable during 20 h photocatalytic reaction. (C) 2018 Elsevier B.V. All rights reserved.