NixSy/NiSe2 hybrid nanoparticle film grown in situ on F-doped SnO2 (FTO) glass is synthesized by a gentle solvothermal method and used as efficient counter electrode for dye-sensitized solar cells (DSSCs). The two-step strategy involving sulfuration and subsequent selenization reaction using nickel hydroxide as the precursor can effectively avoid the film cracking and detaching thus to obtain a uniform hybrid nanoparticle film with rich catalytic active sites and good electron transport ability. The electrocatalytic activity of hybrid catalyst compared with single NiSe2 and NixSy is investigated in detail by cyclic voltammetry (CV), electrochemical impedance spectra (EIS) and Tafel polarization measurements. Due to the synergistic effect of different components, the hybrid NixSy/NiSe2 exhibits higher electrocatalytic performance for I-3 reduction. As a result, the DSSCs with NixSy/NiSe2 hybrid electrode shows an impressive higher short circuit photocurrent and power conversion efficiency (8.64%) than that with NixSy (7.95%) and NiSe2 (7.47%) counter electrodes, just a little bit inferior to Pt (9.01%), which indicates that this new kind of material can work as a promising alternative low-cost catalyst for DSSCs or other electrocatalytic applications. (C) 2017 Elsevier Ltd. All rights reserved.