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Rational design hybrid nanostructure photocatalysts with efficient charge separation and transfer, and good solar light harvesting ability have critical significance for achieving high solar‐to‐chemical conversion efficiency. Here a highly active and stable composite photocatalyst is reported by integrating ultrathin ZnIn2S4 nanosheets on surface of hollow CdS cube to form the cube‐in‐cube structure. Experimental results combined with density functional theory calculations confirm that the Z‐scheme ZnIn2S4/CdS heterojunction is formed, which highly boosts the charge separation and transfer under the local‐electric‐field at semiconductor/semiconductor interface, and thus prolongs their lifetimes. Moreover, such a structure affords the highly enhanced light‐harvesting property. The optimized ZnIn2S4/CdS nanohybrids exhibit superior H2 generation rate under visible‐light irradiation (λ ≥ 420 nm) with excellent photochemical stability during 20 h continuous operation. The stable composite photocatalyst integrated by ultrathin ZnIn2S4 nanosheets on surface of hollow CdS exhibits outstanding visible‐light‐driven photocatalytic H2 generation activity, due to that: i) the Z‐scheme charge transfer route facilitates charge separation, prolongs carrier lifetimes, and remains strong electron reduction capacity; ii) the unique cube‐in‐cube structure brings abundant active sites, improves light harvesting ability, shortens charge transfer distance.

Species of metal ions in carbon dots‐metal ions complex nanozymes boost enzyme‐mimicking activities. However, the relationship between ligand regulation of the catalytic activity of carbon dots‐metal ions complex nanozymes still lacks clarity, which hinders the design of high‐performance nanozymes. Herein, to understand the influence of ligands on nanozyme activities, three kinds of carbon dots‐ferriic ions (CDs‐Fe) nanozymes with three ligands, including allyltriphenylphosphonium bromide (TPP), 1‐hydroxyethane‐1,1‐diphosphonic acid (HEDP), and diethylenetriaminepentaacetic acid (DTPA), are synthesized via sequential hydrothermal carbonization and coordination chemistry. The effects of ligand on peroxidase (POD)‐mimicking and UV‐induced oxidase‐mimicking activities are then systematically evaluated. All CDs‐Fe nanozymes exhibit dual POD‐mimicking and UV‐induced oxidase (OXD)‐mimicking activities. Type of ligand significantly determines catalytic performance, for example, HEDPCDs‐Fe exhibits the highest POD‐mimicking activity (Vm 2.68 × 10−7 M s−1), meanwhile TPPCDs‐Fe showing superior UV‐induced OXD‐mimicking activity (Vm 2.26 × 10−7 M s−1). Crucially, the synergistic effect of UV‐enhanced POD‐OXD is observed, where UV‐induced processes enhanced POD‐mimicking catalysis, motivating significantly improved reaction kinetics with lower Km (1.05 mm) and higher Vm (5.17 × 10−7 M s−1). POD‐mimicking activity with UV irradiation is 1.93 times that in the dark. Ligand‐regulation strategy of CDs‐Fe nanozyme based on coordination chemistry offers an idea to design and synthesize high catalytic activities of CDs‐metal ions nanozymes. Three CDs‐Fe nanozymes functionalized with tailor‐made ligands (TPP, HEDP, and DTPA) are synthesized via hydrothermal carbonization and coordination chemistry. A ligand‐regulation strategy for CDs‐Fe nanozymes achieves tunable enzyme‐mimicking activities and a powerful synergistic effect between POD and UV‐induced OXD pathways, paving the way for designing high‐performance nanozymes.