Abstract
<h2>Summary</h2> Aqueous electrochemical CO<sub>2</sub> reduction (CO<sub>2</sub>R) on Cu can generate a variety of valuable fuels, yet challenges remain in the improvement of electrosynthesis pathways for highly selective fuel production. Mechanistically, understanding CO<sub>2</sub>R on Cu, particularly identifying the product-specific active sites, is crucial. Herein, we rationally designed and fabricated nine large-area single-crystal Cu foils with various surface orientations as electrocatalysts and identified the voltage- and facet-dependent CO<sub>2</sub>R selectivities. <i>Operando</i> grazing incidence X-ray diffraction (GIXRD) and electron back-scattered diffraction (EBSD) were applied to track the top-surface reconstructions of Cu, and we correlate the structural evolution with the change of product selectivities. We extracted three distinct structural descriptors, including crystal facet, atomic coordination number, and step-terrace angle, to reveal the intrinsic structure-function relationships and uniquely identify the specific product-producing sites for CO<sub>2</sub>R. Our work guides the rational design of Cu-based CO<sub>2</sub>R electrocatalysts and, more importantly, establishes a paradigm to understand the structure-function correlation in catalysis.
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