Abstract
The photocatalytic reduction of CO(2) into valuable chemicals and fuels is considered a promising solution to address the energy crisis and environmental challenges. In this work, we introduce a Co-ZIL-L mediated in situ etching and integration process to prepare NiCo-OH with an ultrathin nanosheet-assembled 2D leaf-like superstructure (NiCo-OH UNLS). The resulting catalyst demonstrates excellent photocatalytic performance for CO(2) reduction, achieving a CO evolution rate as high as 309.5 mmol g(-1) h(-1) with a selectivity of 91.0%. Systematic studies reveal that the ultrathin nanosheet structure and 2D leaf-like architecture not only enhance the transfer efficiency of photoexcited electrons but also improve the accessibility of active reaction sites. Additionally, the Ni-Co dual sites in NiCo-OH UNLS accelerate CO(2) conversion kinetics by stabilizing the *COOH intermediate, significantly contributing to its high activity. This work offers valuable insights for designing advanced photocatalysts for CO(2) conversion.