“…From Figure c, the Cu/C-700 sample can be observed to include a peak at 530.0 eV, due to oxygen in metal oxides (i.e., O–Cu), consistent with results from TEM measurements that the CuO and Cu 2 O species were formed in the sample (additional components at 531.3, 532.2, and 533.2 eV are due to OC, SO 4 2– , and O–C, respectively). − Interestingly, for the Cu/C-700 EC sample, whereas the OC, SO 4 2– , and O–C peaks remained virtually unchanged (with an additional peak at 535.4 eV corresponding to CF 2 –O–CF 2 of residual Nafion), the O–Cu peak actually shifted to a markedly higher binding energy (530.8 eV), again, confirming the formation of electron-deficient copper oxides. ,, Taken together, these results suggest that electrochemical activation led to effective enrichment of the Cu 2 O species on the nanocomposite surface . As Cu 2 O is far more active than CuO in catalyzing the 2e – ORR (Figure S12), the observed structural evolution is in excellent agreement with the enhanced selectivity of H 2 O 2 production with Cu/C-700 EC , as compared to Cu/C-700. − This can also account for the best ORR performance of Cu/C-700 among the three as-produced samples, as it possessed the highest Cu + concentration of 0.61 at %, in comparison to 0.35 at % for Cu/C-600 and 0.21 at % for Cu/C-800 (Figures S8b, S13, and S14 and Table S1).…”