AbstractIn advanced oxidation processes, the efficient activation of H2O2 and the selective production of reactive oxygen species are the key steps to achieve the removal of organic pollutants in the water environment. Studies have shown that the precise regulation of catalyst metal active sites can break through the limitation of H2O2 activation and realize the efficient selective conversion of H2O2. Therefore, FeCu bimetallic active sites are developed by constructing FeCu4 alloy nanocluster metal catalyst (FeCu/NC). The introduction of Cu metal sites realized charge redistribution, promoted rapid electron transfer, reduced the spin state of Fe in the catalyst, diminished the interaction between Fe and O, weakened the strong and persistent adsorption between Fe center and *H2O2, lowered the energy barrier of intermediate products in hydroxyl radicals (·OH) generation process, achieved efficient activation of H2O2 and selective generation of ·OH. In addition, a complete electron circulation path is formed between FeCu active sites and the substrate, breaking the contradiction between single metal and H2O2 redox relationship, promoting efficient reduction of Fe3+ to Fe2+. The first‐order kinetic constant (kobs) of FeCu/NC is 0.081 min−1, which is 3.68 and 7.36 times higher than those of single Fe metal species (FeFe/NC) and single Cu metal species (CuCu/NC) catalysts, respectively, and has excellent catalytic performance).
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