Improving greatly the separation efficiency of interfacial charge carrier is a major challenge in photocatalysis. Herein, a new class of C60‐mediated NH2‐MIL‐125(Ti)/Zn0.5Cd0.5S S‐scheme heterojunction with enhanced interfacial charge carrier separation is designed and synthesized. The constructed S‐scheme heterojunction thermodynamically favors photocatalytic H2 evolution because of the large driving force resulting from its strong redox abilities. As a consequence, the optimum proportion of C60‐mediated NH2‐MIL‐125(Ti)/Zn0.5Cd0.5S S‐scheme heterojunction displays comparable H2 evolution activity with a rate of 7825.20 µmol h−1 g−1 under visible light irradiation, which is about 93.05 times, 6.38 times and 2.65 times higher than that of 2% C60/NH2‐MIL‐125(Ti), Zn0.5Cd0.5S and 45% NH2‐MIL‐125(Ti)/Zn0.5Cd0.5S, and outperforms the majority of the previously reported MOFs‐based photocatalysts. Spectroscopic characterizations and theory calculations indicate that the S‐scheme heterojunction can powerfully promote the separation of photogenerated carriers. This work offers a new insight for future design and development of highly active MOFs‐based photocatalysts.

Interior and surface synergistic modifications can endow the photocatalytic reaction with tuned photogenerated carrier flow at the atomic level. Herein, a new class of 2D/2D SnNb 2 O 6 /Ni-doped ZnIn 2 S 4 (SNO/Ni-ZIS) S-scheme heterojunctions is synthesized by a simple hydrothermal strategy, which was used to evaluate the synergy between interior and surface modifications. Theoretical calculations show that the S-scheme heterojunction boosts the desorption of H atoms for rapid H 2 evolution. As a result, 25% SNO/Ni 0.4 -ZIS exhibits significantly improved PHE activity under visible light, roughly 4.49 and 2.00 times stronger than that of single ZIS and Ni 0.4 -ZIS, respectively. In addition, 25% SNO/Ni 0.4 -ZIS also shows superior structural stability. This work provides advanced insight for developing high-performance S-scheme systems from photocatalyst design to mechanistic insight.

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Over the past decade, layered double hydroxides (LDHs) have attracted much attention due to their many advantages in the field of CO2 photoreduction, such as superior CO2 adsorption and tunable...