III- Electrochemical cleaning For noble electrodes such as Au, an electrochemical cleaning procedure was employed after the electrolysis experiments as follows: After sonication in 0.5 molar HNO3, the electrode was subjected to electrochemical washing in a 0.1 molar H2SO4 aqueous solution. The electrochemical cleaning process involved the recording of cyclic voltammograms (CVs) with 20 cycles at a scan rate of 1 V/sec, followed by 10 cycles at 100 mV/sec within the voltage range of 0.2 to 1.5 V versus Ag/AgCl. Figure S2.6 provides an illustration of the electrochemical cleaning procedure for the Au electrode. The cleaning process was continued until repeatable cycles were achieved. However, electrochemical cleaning for non-noble metals such as Cu resulted in poor electrochemical behavior. Figure S2.7a illustrates the cleaning results of a Cu electrode, which does not exhibit a reversible reduction and oxidation cycle as observed for the Au electrode. Comparatively, Figures S2.7b and S2.7c present the cyclic voltammetry results for Au and Cu Figure S2.6. Electrochemical cleaning of Au electrode in a 0.1 molar H2SO4 aqueous solution. (a)The first 20 cycles demonstrate the gradual attainment of repeatable cycles. The initial cycle displays a noticeable oxidation peak, indicating the removal of carbon species from the electrode surface, which was previously exposed to CO2 electrolysis experiments. (b) Subsequent cycles exhibit consistent and repeatable behavior. The electrochemical cleaning process was conducted immediately after CO2 electrolysis in a 0.5 mol% MM NTf2 electrolyte solution in anhydrous MeCN. a b
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