Visualizing Electrochemical CO2 Conversion via the Emerging Scanning Electrochemical Microscope: Fundamentals, Applications and Perspectives

Abstract With the rapid development and maturity of electrochemical CO 2 conversion involving cathodic CO 2 reduction reaction (CO 2 RR) and anodic oxygen evolution reaction (OER), conventional ex situ characterizations gradually fall behind in detecting real‐time products distribution, tracking intermediates, and monitoring structural evolution, etc. Nevertheless, advanced in situ techniques, with intriguing merits like good reproducibility, facile operability, high sensitivity, and short response time, can realize in situ detection and recording of dynamic data, and observe materials structural evolution in real time. As an emerging visual technique, scanning electrochemical microscope (SECM) presents local electrochemical signals on various materials surface through capturing micro‐current caused by reactants oxidation and reduction. Importantly, SECM holds particular potentials in visualizing reactive intermediates at active sites and obtaining instantaneous morphology evolution images to reveal the intrinsic reactivity of active sites. Therefore, this review focuses on SECM fundamentals and its specific applications toward CO 2 RR and OER, mainly including electrochemical behavior observation on local regions of various materials, target products and onset potentials identification in real‐time, reaction pathways clarification, reaction kinetics exploration under steady‐state conditions, electroactive materials screening and multi‐techniques coupling for a joint utilization. This review undoubtedly provides a leading guidance to extend various SECM applications to other energy‐related fields.