CuS-TiO2 composite coating was deposited onto transparent indium tin oxide (ITO) conductive glass surface by electrophoretic deposition, and via heat treatment subsequently at 450 degrees C for 40 min on air atmosphere. The CuS-TiO2 composite coating was characterized by Scanning Electron Microscope (SEM), X-ray Diffraction (XRD), Energy Dispersive X-ray Detector (EDX), UV-Vis Diffuse Reflectance Spectrum (DRS) and Fourier Transform Infrared Spectrophotometer (FT-IR). The photoelectrochemical properties of the CuS-TiO2 composite coating electrode such as cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and Tafel polarization curve were tested on 0.50 mol/L CH3OH as electroactive species in pH = 9.51 Na2CO3-NaHCO3 buffer solution as supporting electrolyte by CHI 660C Electrochemical Workstation under the visible light irradiation. The results showed that TiO2 with 0.5-1.0 mu m particle size and CuS with 0.5-1.5 mu m grain size had dispersed in the CuS-TiO2 composite coating, the mass percentage of CuS had reached 3.99%. Electrochemical measurements indicated that the CuS-TiO2 composite coating electrode had exhibited a better photoelectrocatalytic activity than pure TiO2 electrode and taken on excellent photoelectrocatalytic activity for oxidation-reduction of methanol in buffer solution under the visible light irradiation. (C) 2011 The Electrochemical Society. [DOI: 10.1149/2.075112jes] All rights reserved.