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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 ZnIn 2 S 4 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 ZnIn 2 S 4 /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 ZnIn 2 S 4 /CdS nanohybrids exhibit superior H 2 generation rate under visible-light irradiation (𝝀 ≥ 420 nm) with excellent photochemical stability during 20 h continuous operation.

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The design on synthesizing a sturdy, low‐cost, clean, and sustainable electrocatalyst, as well as achieving high performance with low overpotential and good durability toward water splitting, is fairly vital in environmental and energy‐related subject. Herein, for the first time the growth of sulfur (S) defect engineered self‐supporting array electrode composed of metallic Re and ReS2 nanosheets on carbon cloth (referred as Re/ReS2/CC) via a facile hydrothermal method and the following thermal treatment with H2/N2 flow is reported. It is expected that, for example, the as‐prepared Re/ReS2‐7H/CC for the electrocatalytic hydrogen evolution reaction (HER) under acidic medium affords a quite low overpotential of 42 mV to achieve a current density of 10 mA cm−2 and a very small Tafel slope of 36 mV decade−1, which are comparable to some of the promising HER catalysts. Furthermore, in the two‐electrode system, a small cell voltage of 1.30 V is recorded under alkaline condition. Characterizations and density functional theory results expound that the introduced S defects in Re/ReS2‐7H/CC can offer abundant active sites to advantageously capture electron, enhance the electron transport capacity, and weaken the adsorption free energy of H* at the active sites, being responsible for its superior electrocatalytic performance.

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