Metal–Organic Frameworks Derived Cu _<i>x</i> O/TiO ₂ /C Nanocomposites with Enhanced Photocatalytic Performance

Efficient photocatalysts for hydrogen production and pollutant degradation are crucial to address energy and environmental challenges. metal–organic framework (MOF)‐derived Cu x O/TiO 2 /C (TCC) composites are synthesized from Cu‐doped NH 2 ‐MIL‐125(Ti) and their performance in photodegradation of pollutants and photocatalytic hydrogen generation are evaluated. These porous TCC composites demonstrate rapid adsorption capacities and greatly enhance photocatalytic degradation of organic pollutants under visible light, with TCC‐1 achieving complete pollutants removal in 90 min due to adsorption and photocatalysis. Moreover, these Cu x O/TiO 2 /C composites exhibit superior photocatalytic hydrogen evolution performance, and TCC‐2 achieves the highest hydrogen production rate of 2339 μmol g −1 h −1 , 13 times greater than TiO 2 /C. The enhanced activity is attributed to the formation of type‐II band alignment between the coexisted anatase and rutile TiO 2 phases, the presence of Cu 2 O/CuO heterojunctions that facilitate p–n charge separation, and Cu 0 clusters as electron sinks to accelerate proton reduction. Porous carbon boosts adsorption and also provides rapid electron transport pathways. Additionally, the coexistence of multiple Cu species (Cu 2+ /Cu + ) facilitates reversible redox shuttling, suppressing electron–hole recombination. The synergistic effects of these structural and electronic features lead to superior hydrogen generation and pollutant degradation activity of TCC composites, demonstrating the promise of MOF‐derived photocatalysts for sustainable energy and environmental applications.