Hierarchical 0D NiSe2/2D ZnIn2S4 Nanosheet‐Assembled Microflowers for Enhanced Photocatalytic Hydrogen Evolution

Abstract Hierarchical structure design and use of cocatalyst are effective strategies to improve the photocatalytic performance of semiconductor catalysts. Herein, 0D NiSe 2 nanoparticles decorated 2D ZnIn 2 S 4 ultrathin nanosheet‐assembled microflowers using a facile solvothermal approach are synthesized. The as‐obtained NiSe 2 /ZnIn 2 S 4 nanocomposites exhibit enhanced visible‐light photocatalytic H 2 ‐evolution activity of 1487 µ mol (g h) –1 , three times higher than that of pure ZnIn 2 S 4 . The hierarchical structure of ZnIn 2 S 4 microflowers exposes more surface‐active sites and enhances light harvesting. Meanwhile, the formation of heterojunctions between ZnIn 2 S 4 nanosheets and NiSe 2 nanoparticles creates a space‐charge separation region that facilitates the transfer and separation of photoinduced electrons and holes, resulting in improved photocatalytic H 2 production. This work provides a promising strategy for designing and constructing 0D/2D heterojunctions for efficient solar‐driven energy conversion.