LAUSR

Copper‐doped ZnS/ZnO (CSO) hexahedrons in egg tart‐like morphology were fabricated by an in‐situ synthetic strategy to promote photocatalytic hydrogen (H2) production. Hexahedral CuO/ZnO precursors in micro sizes were prepared by a solvothermal method. A subsequent moderate sulfurization of the precursor led to the formation of ZnS/ZnO heterostructures without alteration of the hexahedral morphology. In addition, the in‐situ methodology ensured the homogeneous doping of copper species with ZnS/ZnO heterostructures, which significantly improved the electric conductivity of these hybrid materials. Because of the structural and compositional features of the hybrid materials, a maximum H2 production rate of 1.044 mmol g−1 h−1 with high recycling stability (even after 12 h) has been delivered based on an interfacial catalysis. Thus, this study may provide an efficient strategy to optimize the physical and chemical properties of photocatalysts in microsize scale.