The photo-electrochemical characterization of the hetero-system CuFe2O4/TiO2 was undertaken for the Ni2+ reduction under solar light. The spinel CuFe2O4 was prepared by nitrate route at 940 oC and the optical gap (1.66 eV) was well matched to the sun spectrum. The flat band potential (-0.21 VSCE) is more cathodic than the potential of Ni2+/Ni couple (-0.6 VSCE), thus leading to a feasible nickel photoreduction. TiO2 with a gap of 3.2 eV is used to mediate the electrons transfer. The reaction is achieved in batch configuration and is optimized with respect to Ni2+ concentration (30 ppm); a reduction percentage of 72% is obtained under sunlight, the Ni2+ reduction is strongly enhanced and follows a first order kinetic with a rate constant of 4.6×10-2 min-1 according to the Langmuir-Hinshelwood model.