A new magnetic semiconductor material was synthesized to enable separation after a liquid-type photocatalysis process. Core@shell-structured CuFeS 2 @TiO 2 magnetic nanoparticles were prepared by a combination of solvothermal and wet-impregnation methods for photocatalysis applications. The materials obtained were characterized using X-ray diffraction, transmission electron microscopy, ultraviolet-visible, photoluminescence spectroscopy, Brunauer-Emmett-Teller surface area measurements, and cyclic voltammetry. This study confirmed that the light absorption of CuFeS 2 was shifted significantly to the visible wavelength compared to pure TiO 2 . Moreover, the resulting hydrogen production from the photo-splitting methanol/water solution after 10 hours was more than 4 times on the core@shell structured CuFeS 2 @TiO 2 nanocatalyst than on either pure TiO 2 or CuFeS 2 .