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Current density (A) and Faradaic efficiencies (B) for CO2 reduction on RuPC/NPC over a 3-h period in 0.5 M KHCO3 aqueous solutions (−0.97 V vs. NHE). Materials and Methods Preparation of RuPC/NPC Electrode. A total of 60.0 mg of NPC was added into 10.0 μL of Nafion (5 wt%) and 490.0 μL of isopropanol. RuPC dissolved at 1. O. S. Bushuyev et al., What should we make with CO2 and how can we make it? Joule 2, 825–832 (2018). 2. C. G. Morales-Guio et al., Improved CO2 reduction activity towards C2+ alcohols on a tandem gold on copper electrocatalyst. Nat. Catal. 1, 764–771 (2018). 3. R. G. Mariano, K. McKelvey, H. S. White, M. W. Kanan, Selective increase in CO2 electroreduction activity at grain-boundary surface terminations. Science 358, 1187– 1192 (2017). 4. W. Luo, J. Zhang, M. Li, A. Züttel, Boosting CO production in electrocatalytic CO2 reduction on highly porous Zn catalysts. ACS Catal. 9, 3783–3791 (2019). 5. Q. Li et al., Tuning Sn-catalysis for electrochemical reduction of CO2 to CO via the core/shell Cu/SnO2 structure. J. Am. Chem. Soc. 139, 4290–4293 (2017). 6. Y. Liu, S. Chen, X. Quan, H. Yu, Efficient electrochemical reduction of carbon dioxide to acetate on nitrogen-doped nanodiamond. J. Am. Chem. Soc. 137, 11631–11636 (2015). 7. M. D. Sampson, C. P. Kubiak, Manganese electrocatalysts with bulky bipyridine li- gands: Utilizing Lewis acids to promote carbon dioxide reduction at low over- potentials. J. Am. Chem. Soc. 138, 1386–1393 (2016). 8. C. Costentin, S. Drouet, M. Robert, J. M. Savéant, A local proton source enhances CO2 electroreduction to CO by a molecular Fe catalyst. Science 338, 90–94 (2012). 9. M. L. Clark, P. L. Cheung, M. Lessio, E. A. Carter, C. P. Kubiak, Kinetic and mechanistic effects of bipyridine (bpy) substituent, labile ligand, and brønsted acid on electro- catalytic CO2 reduction by Re(bpy) complexes. ACS Catal. 8, 2021–2029 (2018). 10. S. Lin et al., Covalent organic frameworks comprising cobalt porphyrins for catalytic CO2 reduction in water. Science 349, 1208–1213 (2015). DMSO-D6 (100 μM, 50 μL) was added into the suspension. After sonication for 10 min and stirring for 12 h, the suspension was drop-coated on carbon-fiber substrate with a catalyst loading of 0.03 g·cm−2. The pre- pared RuPC/NPC electrode was washed by isopropanol to remove Ru polypyridyl carbene, which was not anchored on NPC, and vacuum dried at 80 °C. Electrochemical Experiments. All of the electrochemical tests were conducted in a 3-electrode system at room temperature. RuPC/NPC or NPC was used as the working electrode, and Pt foil was used as the counterelectrode. The amount of Ru polypyridyl carbene anchored on the RuPC/NPC electrode was measured by cyclic voltammograms in Ar saturated in 0.1 M TBAPF6/MeCN with Ag as reference electrode. The potential was converted to vs. NHE by using ferrocene for calibration. All CO2-reduction experiments were tested with Ag/AgCl as reference electrode, and the potentials were converted to vs. NHE by using the equation of Evs. NHE = Evs. Ag/AgCl + 0.2 (V). The activity of RuPC/NPC for electrocatalytic CO2 reduction was examined by linear-sweep voltammo- grams in CO2- or Ar-saturated 0.5 M KHCO3 aqueous electrolyte (scan rate of 10 mV·s−1). CO2 bulk electrolysis was performed at −0.87 to approximately −1.17 V (vs. NHE) in a gas-tight H-type 2-chamber cell separated by Nafion 117 membrane, which was filled with CO2-saturated 0.5 M KHCO3 aqueous solution. Product Analysis. After bulk electrolysis, gas samples were drawn from the headspace of the gas-tight cell and injected into gas chromatography (Varian 450) equipped with a thermal conductivity detector. The liquid products were measured by a 1H NMR spectrum (Bruker B600) and gas chromatography (Shimadzu, catalog no. GC-2010) equipped with a flame ionization detector (FID). For 1H NMR spectra, solvent suppression was applied for CO2-reduction product analysis to reduce the intensity of water peak. The samples were collected into 10% D2O with DMSO as in- ternal standard for quantification. The amount of ethanol produced was confirmed by gas chromatography (Shimadzu, catalog no. GC-2010) equipped with an FID detector and DB-Wax column (30 m × 0.25 mm × 0.50 μm). The Faradaic efficiency (FE) for CO2 reduction was calculated via the equation of FE = nNF/Q, where n is the number of electron transferred for CO2 reduction to products, N is the molar quantity of CO2-reduction prod- ucts (mol), F is the Faraday constant (C·mol−1), and Q is the amount of charge passed through the cell (C). Data Availability. All data are included in the main text and SI Appendix. ACKNOWLEDGMENTS. This work was supported by the US Department of Energy, Office of Basic Energy Sciences Award DE-SC0015739; and National Natural Science Foundation of China Grants 21707016 and 51708085. Y.L. was supported by the State Scholarship Fund from the China Scholarship Council. 11. F. Lei et al., Metallic tin quantum sheets confined in graphene toward high-efficiency carbon dioxide electroreduction. Nat. Commun. 7, 12697 (2016). 12. M. Liu et al., Enhanced electrocatalytic CO2 reduction via field-induced reagent concentration. Nature 537, 382–386 (2016). 13. A. S. Hall, Y. Yoon, A. Wuttig, Y. Surendranath, Mesostructure-induced selectivity in CO2 reduction catalysis. J. Am. Chem. Soc. 137, 14834–14837 (2015). 14. S. Gao et al., Partially oxidized atomic cobalt layers for carbon dioxide electro- reduction to liquid fuel. Nature 529, 68–71 (2016). 15. Y. Zhou et al., Dopant-induced electron localization drives CO2 reduction to C2 hy- drocarbons. Nat. Chem. 10, 974–980 (2018). 16. T. T. H. Hoang et al., Nanoporous copper-silver alloys by additive-controlled electro- deposition for the selective electroreduction of CO2 to ethylene and ethanol. J. Am. Chem. Soc. 140, 5791–5797 (2018). 17. C. Zhao et al., Ionic exchange of metal-organic frameworks to access single nickel sites for efficient electroreduction of CO2. J. Am. Chem. Soc. 139, 8078–8081 (2017). 18. K. Jiang et al., Isolated Ni single atoms in graphene nanosheets for high-performance CO2 reduction. Energy Environ. Sci. 11, 893–903 (2018). 19. I. Hod et al., Fe-porphyrin-based metal-organic framework films as high-surface concentration, heterogeneous catalysts for electrochemical reduction of CO2. ACS Catal. 5, 6302–6309 (2015). 20. Z. Weng et al., Electrochemical CO2 reduction to hydrocarbons on a heterogeneous molecular Cu catalyst in aqueous solution. J. Am. Chem. Soc. 138, 8076–8079 (2016). 21. N. Han et al., Supported cobalt polyphthalocyanine for high-performance electro- catalytic CO2 reduction. Chem 3, 652–664 (2017). Fig. 6. Liu et al. 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