To mitigate the challenge of reductive Ag deposition in electrolysis experiments, a novel protocol was developed and implemented in this study, which is illustrated in Figures 2.6 and 2.7. In this new approach, the initial step involved conducting all linear sweep voltammetry (LSV) measurements and electrolysis experiments using a graphite rod as both the counter and reference electrode (Figure 2.6a). A critical requirement of this protocol was that the size of the graphite counter electrode consistently exceeded that of the working electrode. Additionally, the applied current in the cell was deliberately restricted to the bulk concentration of the reactant, specifically CO2 in acetonitrile. By adhering to these conditions, the undesired impacts of the counter electrode on the working electrode and its associated reaction were effectively minimized. In the second step of the protocol, once a stable electrochemical response was obtained using the two-electrode configuration, a reference solution containing Figure 2.5. Scanning electron microscopy (SEM) results along with associated energy-dispersive X-ray spectroscopy (EDX) analysis of the Pt electrode investigated in Figure 2.3. The bottom left panel illustrates a schematic representation of the coordination of metal nanoparticles with NHC (N-heterocyclic compound) compounds, adapted from reference5.
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