Preparation of Catalysts and Associated Characterizations. As per our previous discussions, in our pursuit of the perfect catalyst for electrochemically reducing CO2 into a valuable energy feedstock, we aim to utilize the Cu58-I and Cu58-II NCs and evaluate their efficacy against the regular Cu58 NC. For the electrochemical evaluation, thin film electrodes were fabricated utilizing the spray coating technique. This involved spray-casting a slurry of the NC containing Carbon Black (CB) onto a thin carbon paper (CP) substrate as depicted in the experimental section. We confirmed that there is no change in the electronic and geometric structure of Cu58-I and Cu58-II NCs during the loading processes by the X-ray absorption fine structure (XAFS) spectra (Figure and). The X-ray absorption near-edge structure (XANES) spectrum at the Cu K-edge for both the Cu58-I and Cu58-II NCs, as well as the loaded catalysts (Cu58-I NC/CB and Cu58-II NC/CB) demonstrates excellent alignment, indicating the electronic stability of these NCs after loading on CB. In both cases, the pre-edge peak ~8980 resembles that of standard Cu2O, suggesting the presence of Cu(I) species in all cases (Figure