In this work, a synergy structure to improve the photocatalytic properties of materials was proposed. CuSbS 2 nanoparticles synthesized by microwave irradiation method were dispersed in TiO 2 sol to form CuSbS 2-TiO 2 nanoparticles. The properties of composite materials with different TiO 2 sol concentration were investigated by XRD, XPS, etc. The results indicated the as-synthesized CuSbS 2 nanoparticles exhibited chalcostibite structure and the TiO 2 showed anatase phase. The CuSbS 2-TiO 2 nanoparticles had high absorbance in the visible light and good photocatalysts for the photodegradation reaction of Rhodamine B (RhB). When TiO 2 sol concentration was 0.23 mol/L, the sample possessed a photocatalytic degradation rate of 0.002 min −1 for the degradation of RhB, which was 3 times higher than that by the bare amorphous TiO 2 (0.0007 min −1).