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Article Abstract
Artificial photosynthesis presents a highly promising approach for addressing global energy and environmental challenges. However, its efficiency remains constrained by rapid charge recombination and inefficient CO activation. To overcome these limitations, cobalt-nickel layered double hydroxide (CN-LDH) is decorated onto BiOBr nanosheets to enhance Lewis alkaline sites and facilitate charge separation. The resultant composite, denoted as BC, exhibits a stronger internal electric field than its individual components, promoting efficient migration of photogenerated carriers. This engineered structure directs photoinduced electrons accumulated in CN-LDH for CO reduction, as verified by in situ Kelvin probe force microscopy. Furthermore, in situ diffuse reflectance infrared Fourier transform spectroscopy combined with pulsed chemisorption studies identifies the critical activated carbonate intermediates (*CO and *COOH) as essential precursors for CO production. Consequently, the optimized BC catalyst achieves a remarkable CO evolution rate of 88.92 μmol g with 100% selectivity. This work provides pivotal insights into the charge transfer dynamics and intermediate evolution pathways during photocatalytic CO reduction.
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