Constructing wide and narrow band gap heterogeneous semiconductors is a method to improve the activity of photocatalysts. In this paper, CMS/ZnO heterojunctions were prepared by solvothermal loading of ZnO particles on the surface of CuMoS nanosheets. The photocatalytic H precipitation rate is about 545 μmol·g·h, which is 6.8 times that of CuMoS and 3 times that of ZnO without any cocatalyst. After etching modification of CMS, the photocatalytic hydrogen production efficiency of the ECMS/ZnO heterojunction is further improved. Its hydrogen production efficiency reaches about 1115 μmol·g·h, which is 9 times that of ECMS and 6 times that of ZnO. The reasons are mainly attributed to the following two factors: (1) the formation of the ECMS/ZnO type-II-type heterojunction facilitates the effective separation of photogenerated electrons and holes; (2) the band structure of CuMoS was optimized by etching modification, which made the ECMS/ZnO heterojunction have lower interfacial charge transfer resistance and improved the photocatalytic hydrogen production activity of the heterojunction.
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