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The novel 2D/2D S-scheme heterostructure of BiOCl nanosheets coupled with CaIn₂S₄ nanosheets (CaIn₂S₄/BiOCl-SOVs), which contains surface oxygen vacancies (SOVs), has been successfully prepared by high-temperature calcination combined with a solvothermal synthetic strategy. Under visible-light irradiation, the apparent rate constant (<i>K</i>_app/mim⁻¹) for phenol degradation on the 1 wt% CaIn₂S₄/BiOCl-SOVs photocatalyst is about 32.8 times higher than that of pure BiOCl. The superior performance was attributed to the synergistic effect between the SOVs, CaIn₂S₄, and BiOCl, which can effectively narrow the bandgap and accelerate the interfacial charge separation of CaIn₂S₄/BiOCl-SOVs heterojunctions. Subsequently, it significantly promotes the generation of superoxide radicals (O₂⁻), hydroxyl radicals, and h⁺, which participate in the photodegradation process of phenol. The catalyst still maintained a relatively high activity after repeated tests as a demonstration of its photostability. This work successfully proposed an efficient method to design a new 2D/2D S-scheme heterostructure with SOVs as possible photocatalysts in the field of environmental remediation.