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This work reports the fabrication of ZnO@MoS2 core–shell micro/nanomaterials and their photocatalytic performances. First, the ZnO@MoS2 core–shell micro/nanorods heterostructures were grown by a two-step, hydrothermal method. Second, X-ray diffraction, scanning-electron microscopy, Raman spectra, and UV-visible spectra were applied to confirm and characterize the ZnO@MoS2 core–shell micro/nanorods. Third, methylene blue was employed to investigate the photocatalytic performance of the ZnO@MoS2 core–shell micro/nanorods heterostructures. It was found that the shape of the MoS2 shell layer depended on the growth time. The shell layer was composed of MoS2 nanoparticles before the growth time of 6 h and then turned into MoS2 nanosheets. It was also found that the photocatalytic performance was significantly affected by the growth time of the MoS2 nanosheets. When the growth time of the MoS2 nanosheets was between 6 and 10 h, ZnO@MoS2 core–shell heterostructures grown for 6 h exhibited a best photocatalytic efficiency value of 69.24% after 3 h catalysis. [ABSTRACT FROM AUTHOR]