Abstract
Localized concentration gradients within the electrochemical double layer during various electrochemical processes can have wide-ranging impacts; however, experimental investigation to quantitatively correlate the rate of surface-mediated electrochemical reaction with the interfacial species concentrations has historically been lacking. In this work, we demonstrate a spectroscopic method for the in situ determination of the surface pH using the CO2 reduction reaction as a model system. Attenuated total reflectance surface-enhanced infrared absorption spectroscopy is employed to monitor the ratio of vibrational bands of carbonate and bicarbonate as a function of electrode potential. Integrated areas of vibrational bands are then compared with those obtained from calibration spectra collected in electrolytes with known pH values to determine near-electrode proton concentrations. Experimentally determined interfacial proton concentrations are then related to the resultant concentration overpotentials to exam...
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