Regulating Functional Transition Metal Complexes for Solar‐Driven Selective Conversion of Hydrogen Peroxide to Singlet Oxygen in Wastewater Treatment

The selective generation of the electrophilic oxidant singlet oxygen ( 1 O 2 ) in the photo‐Fenton process is crucial for achieving precise control over organic pollutants in environmental applications. Herein, we rationally designed a CuS/MoO 3 (CM‐1.0) heterojunction featuring a coherent heterojunction interface characterized by Mo‐O‐Cu covalent bridging bonds and a low lattice mismatch of 1.04%. This design significantly enhances the intrinsic electric field strength of CM‐1.0 (54 times that of MoO 3 and 195 times that of CuS) and the separation efficiency of photogenerated charge carriers. Simultaneously, benefiting from rapid electron transfer between Cu sites (O‐Cu) and H 2 O 2 under alkaline conditions, the in‐situ formation of transition metal complexes (O‐Cu‐OOH) is facilitated. This composite achieves nearly 100% selective production of 1 O 2 while scavenging electrons from ·O 2 − (electron donor), thereby enabling a rapid tandem reaction of H 2 O 2 ‐ 1 O 2 . Experimental results have shown that CM‐1.0 achieves a 99.2% removal rate of tetracycline (TC) within 10 min, with a first‐order kinetic constant ( k obs ) of 0.3814 min −1 . Furthermore, through experiments with different water quality conditions, under actual sunlight exposure, and in flow systems demonstrate that the system exhibits excellent interference resistance, excellent stability, and potential for practical remediation applications.