Ni nanoparticles were prepared via chemical reduction of NiCl2 by NaBH4 in the presence of polyvinlylpyrolidone (PVP), and loaded on the surface of CdS by photo-induced electrons while water splitting reaction occurred simultaneously. Resultant Ni/CdS was characterized by high-resolution transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, ultraviolet-visible light diffuse reflectance spectrometry, and photoluminescence spectrometry. It was found that as-prepared Ni nanoparticles are about 3 nm, and preferentially deposited on (1 0 0), (0 0 2), and (1 01) crystal planes of CdS. Meanwhile, loading nickel decreases the photoluminescence intensity of CdS, which means nickel functions as the trapper of photo-generated electrons. Therefore, nano-Ni/CdS photocatalyst with a Ni loading of 2.5% possesses the best visible-light catalytic activity for water splitting-hydrogen evolution and provides a hydrogen production rate of up to 9050 mu mol h(-1) g(-1), while it exhibits stabilized activity towards H-2 evolution as well. (C) 2014 Elsevier Ltd. All rights reserved.