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SEM images of NPC (A) and RuPC/NPC (B) and energy-dispersive X- ray spectroscopic maps of N (C) and Ru (D) on RuPC/NPC. consistent with enhanced CO2 reduction by the surface-bound Ru(II) polypyridyl carbene. To probe for CO2-reduction products, bulk electrolysis was performed on RuPC/NPC electrodes in CO2-saturated 0.5 M KHCO3 aqueous solutions with potentials from −0.87 to −1.17 V (vs. NHE). The liquid and gas products were detected by gas chromatography and 1H NMR. Ethanol, acetate, methanol, CO, and formate have been identified as CO2-reduction products for RuPC/NPC (SI Appendix, Fig. S4). To confirm that these prod- ucts originated from catalyzed CO2 reduction, bulk electrolysis on the RuPC/NPC electrode was performed in Ar-saturated 0.5 M KHCO3 aqueous solutions at −0.97 and −1.07 V (vs. NHE). As expected, there was no evidence for carbon-containing compounds after 1 h of electrolysis. The 13CO2-reduction ex- periment was performed at −0.97 V (vs. NHE), and the liquid products were analyzed by 1H NMR. In the 1H NMR spectrum (SI Appendix, Fig. S5), H–13C signals for ethanol, acetate, methanol, and formate with peak splitting were clearly observed, while H–12C signals were negligible, confirming that the products were derived from CO2 reduction. Fig. 5B shows the Faradaic efficiency for the products that appeared after CO2 reduction on the RuPC/NPC electrode for 1 h. In the data, it is notable that the Faradaic efficiency for ethanol (21.0 to 27.5%) is much higher than efficiencies for other products at potentials from −0.87 to −1.07 V (vs. NHE). For example, at −0.97 V (vs. NHE), the efficiency for ethanol for- mation was 2.5 to 5.2 times higher than efficiencies for acetate, methanol, CO, and formate. The experimental observations show that RuPC/NPC has a high selectivity for ethanol pro- duction at relatively low overpotentials. The total efficiencies for the multicarbon products, ethanol and acetate, were 31.0 to 38.4% at −0.87 to −1.07 V (vs. NHE). When the potential was shifted negatively from −0.87 to −1.17 V (vs. NHE), both the current densities (SI Appendix, Fig. S6) and efficiencies for ethanol and acetate increased initially and then decreased at potentials more negative than −1.07 V (vs. NHE). Over the same potential range, the current density and efficiencies for CO in- creased gradually. The electrolysis results show that ethanol production is favored on the RuPC/NPC electrode at less neg- ative potentials. Increasing the potential to or beyond −1.17 V (vs. NHE) caused CO to become the major CO2-reduction product to give syngas, CO, and H2 (SI Appendix, Fig. S7). Syngas is an important chemical feedstock for synthesizing bulk chemicals and fuels such as methanol, acetic acid, and others. The molar ratio of H2/CO syngas was 2.9:1 at −0.87 V (vs. NHE), which decreased gradually to 2:1 as potential shifted negatively from −0.87 to −1.17 V (vs. NHE) (Fig. 5C). However, it increased to 2.4:1 at more negative potential (−1.17 V vs. NHR). The potential Fig. 3. Fig. 4. N 1s XPS spectrum of NPC (A), Ru 3d and C 1s spectrum of RuPC/NPC (B), and cyclic voltammograms of NPC (C) and RuPC/NPC (D) electrodes in 0.1 M TBAPF6/MeCN at a scan rate of 10 mV·s−1. a.u., arbitrary units. Liu et al. PNAS Latest Articles | 3 of 6 Downloaded by guest on May 6, 2021 CHEMISTRYPDF Image | Steering CO2 electroreduction toward ethanol production
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