Modifying CdZnS with precious metal at the atomic scale is a promising approach for maximizing its photocatalytic performance. Herein, Rh single atoms (Rh) were successfully anchored on hollow microflower MoS/sulfur-vacancy-rich CdZnS (CZS-SVs) to boost H generation. The optimal catalyst Rh@MoS/CZS-SVs reaches a H productivity of 39,827 μmol h g, representing 5.64 and 4.36-folds enhancement compared with pristine CZS and CZS-SVs, respectively. The enhanced H generation activity was due to Rh single atoms and sulfur-vacancy defects, both of which can effectively promote carrier separation and prolong carrier lifespan. Notably, density functional theory (DFT) calculations suggest that introducing Rh single-atom sites on MoS/CZS-SVs significantly facilitated electron transfer, leading to efficient conversion of the H* intermediate to H (|ΔGH*| = 0.44 eV). Consistently, in situ Raman analysis confirmed Rh and S dual proton-reduction sites. Due to the accumulation of abundant electric charges, S atoms sites can also participate in H evolution process.
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