| Summary: | This work reports the fabrication of ZnO@MoS<sub>2</sub> core–shell micro/nanomaterials and their photocatalytic performances. First, the ZnO@MoS<sub>2</sub> 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@MoS<sub>2</sub> core–shell micro/nanorods. Third, methylene blue was employed to investigate the photocatalytic performance of the ZnO@MoS<sub>2</sub> core–shell micro/nanorods heterostructures. It was found that the shape of the MoS<sub>2</sub> shell layer depended on the growth time. The shell layer was composed of MoS<sub>2</sub> nanoparticles before the growth time of 6 h and then turned into MoS<sub>2</sub> nanosheets. It was also found that the photocatalytic performance was significantly affected by the growth time of the MoS<sub>2</sub> nanosheets. When the growth time of the MoS<sub>2</sub> nanosheets was between 6 and 10 h, ZnO@MoS<sub>2</sub> core–shell heterostructures grown for 6 h exhibited a best photocatalytic efficiency value of 69.24% after 3 h catalysis.
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