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CuInS2–ZnO nanocomposites were prepared by two combined approaches, namely solvothermal and chemical precipitation. The structure, morphology, composition and optical properties of the nanocomposites was studied by X-ray diffraction (XRD), scanning transmission electron microscopy (STEM), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and diffuse reflectance spectroscopy (DRS). The influence of ZnO content on the photocatalytic activity of these nanocomposites was studied. The results showed that CuInS2-ZnO samples possess photocatalytic activity against a Rhodamine B (RhB) synthetic solution. Additionally, electron spin resonance spectroscopy (ESR) coupled with spin trapping technique was used to characterize the reactive oxygen species (ROS). The photocatalytic mechanism was discussed according to ROS generation that were able to degrade the RhB. The photodegradation rate for RhB removal by CuInS2–ZnO nanoparticles increased with the addition of ZnO nanoparticles on their surface. During the irradiation, both hydroxyl radical (OH−) and superoxide anion (O2−) were highlighted suggesting that the CuInS2–ZnO nanocomposites are suitable for use in water depollution by photocatalysis. [ABSTRACT FROM AUTHOR]