Dual-mode in situ monitoring of CO2 conversion via pH indicator and UV-vis spectroscopy

The integration of the KHCO₃-fed bipolar membrane (BPM) electrolyzer with potassium hydroxide (KOH)-based carbon dioxide (CO₂) capture enables directly <i>in situ</i> conversion of captured CO₂ into valuable carbonaceous products, eliminating costly CO₂ recovery and compression steps. Even this integrated BPM system assembly holds promise; the critical lack of CO₂ adsorption intermediate species tracking necessitates the development of a monitoring platform. This work pioneers a novel dual-modal strategy employing simultaneous indicator-based sensing with <i>in situ</i> ultraviolet-visible (UV-vis) spectroscopy, achieving real-time visualization of triphasic dynamics during integrated CO₂ capture-regeneration-conversion. Within this synergistic process involving Ar-saturated KHCO₃ decomposition and electrochemical reduction, an etched indium (In) catalyst achieves 50% formate Faradaic efficiency (FE) at -1.1 V vs. RHE (reversible hydrogen electrode). The synergistic application of these complementary <i>in situ</i> diagnostics unlocks fundamental mechanistic insights into integrated CO₂ capture and conversion systems, establishing them as critical enablers for advancing efficient and scalable electrochemical CO₂ valorization.