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Iron containing MOFs have been currently estimated as greater candidates for heterogeneous Fenton catalysts due to their open pores and well dispersed metallic components. However, metals in majority of MOFs are bounded by organic linkers, which reduces Lewis acid sites and make them not available for H₂O₂ activation. Creating coordinatively unsaturated metal centers (CUCs), acting as Lewis acid sites, is a feasible approach for efficient photo-Fenton activity. Here, we successfully synthesized a photo-Fenton CUCs-MIL-88B-Fe catalyst with mixed-valence (Fe^II/Fe^III) on ultrathin Ti₃C₂ nanosheets. The Lewis acidity was probed by TPD-NH₃ and IR-pyridine analysis and tested for pollutants degradation. The results showed that CUCs-MIL-88B-Fe/Ti₃C₂ displayed highest photo-Fenton activity under visible light irradiation at pH 3.0 and 10 mM H₂O₂. This could be attributed with the CUCs, fast H₂O₂ …