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Nature Catalysis Articles EE was calculated on the basis of the cathodic CO2RR coupled with anodic water oxidation reaction (O2+4H+ + 4e– ↔ 2H2O; 1.23 V versus RHE). where Eoxo CO2RRIto ethanoIl (0.09V versus RHE), respectively and Eox and Ered are the applied potentials at anode and cathode, respectively. For the calculation of the half-cell CEE, the anodic reaction was assumed to occur with an overpotential of 0 V (that is Eox = 1.23 V). For full-cell EE calculation, the equation then was simplified to 17. Zhou, Y. et al. Dopant-induced electron localization drives CO2 reduction to C2 hydrocarbons. Nat. Chem. 10, 974–980 (2018). 18. De Luna, P. et al. Catalyst electro-redeposition controls morphology and oxidation state for selective carbon dioxide reduction. Nat. Catal. 1, 103–110 (2018). 19. Liang, Z.-Q. et al. Copper-on-nitride enhances the stable electrosynthesis of multi-carbon products from CO2. Nat. Commun. 9, 3828 (2018). 20. Ren, D., Ang, B. S.-H. & Yeo, B. S. Tuning the selectivity of carbon dioxide electroreduction toward ethanol on oxide-derived CuxZn catalysts. ACS Catal. 6, 8239–8247 (2016). 21. Vojvodic, A. & Nørskov, J. K. New design paradigm for heterogeneous catalysts. Natl Sci. Rev. 2, 140–143 (2015). 22. Peterson, A. A. & Nørskov, J. K. Activity descriptors for CO2 electroreduction to methane on transition-metal catalysts. J. Phys. Chem. Lett. 3, 251–258 (2012). 23. Calle-Vallejo, F. & Koper, M. T. Theoretical considerations on the electroreduction of CO to C2 species on Cu(100) electrodes. Angew. Chem. Int. Ed. 52, 7282–7285 (2013). 24. Montoya, J. H., Shi, C., Chan, K. & Nørskov, J. K. Theoretical insights into a CO dimerization mechanism in CO2 electroreduction. J. Phys. Chem. Lett. 6, 2032–2037 (2015). 25. Xiao, H., Cheng, T. & Goddard, W. A. Atomistic mechanisms underlying selectivities in C1 and C2 products from electrochemical reduction of CO on Cu(111). J. Am. Chem. Soc. 139, 130–136 (2017). 26. 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On the effect of coverage-dependent adsorbate–adsorbate interactions for CO methanation on transition metal surfaces. J. Catal. 307, 275–282 (2013). 33. Cheng, T., Xiao, H. & Goddard, W. A. Full atomistic reaction mechanism with kinetics for CO reduction on Cu(100) from ab initio molecular dynamics free-energy calculations at 298K. Proc. Natl Acad. Sci. USA 114, 1795–1800 (2017). 34. Costentin, C., Drouet, S., Robert, M. & Savéant, J. M. A local proton source enhances CO2 electroreduction to CO by a molecular Fe catalyst. Science 338, 90–94 (2012). 35. Costentin, C., Robert, M. & Savéant, J. M. Catalysis of the electrochemical reduction of carbon dioxide. Chem. Soc. Rev. 42, 2423–2436 (2013). 36. Lin, S. et al. Covalent organic frameworks comprising cobalt porphyrins for catalytic CO2 reduction in water. Science 349, 1208–1213 (2015). 37. Hu, X. M., Rønne, M. H., Pedersen, S. U., Skrydstrup, T. & Daasbjerg, K. Enhanced catalytic activity of cobalt porphyrin in CO2 electroreduction upon immobilization on carbon materials. Angew. Chem. Int. Ed. 56, 6468–6472 (2017). 38. Zhang, X. et al. Highly selective and active CO2 reduction electrocatalysts based on cobalt phthalocyanine/carbon nanotube hybrid structures. Nat. Commun. 8, 14675 (2017). 39. Smith, P. T. et al. Iron porphyrins embedded into a supramolecular porous organic cage for electrochemical CO2 reduction in water. Angew. Chem. Int. Ed. 57, 9684–9688 (2018). 40. Joya, K. S., Morlanés, N., Maloney, E., Rodionov, V. & Takanabe, K. Immobilization of a molecular cobalt electrocatalyst by hydrophobic interaction with a hematite photoanode for highly stable oxygen evolution. Chem. Commun. 51, 13481–13484 (2015). 41. Bertheussen, E. et al. Acetaldehyde as an intermediate in the electroreduction of carbon monoxide to ethanol on oxide-derived copper. Angew. Chem. Int. Ed. 55, 1450–1454 (2016). 42. Weekes, D. M., Salvatore, D. A., Reyes, A., Huang, A. & Berlinguette, C. P. Electrolytic CO2 reduction in a flow cell. Acc. Chem. Res. 51, 910–918 (2018). 43. Sheppard, N. & Nguyen, T. T. Advances in Infrared and Raman Spectroscopy. (Heyden, 1978). 44. Gunathunge, C. M. et al. Spectroscopic observation of reversible surface reconstruction of copper electrodes under CO2 reduction. J. Phys. Chem. C. 121, 12337–12344 (2017). 45. Tsubaki, M., Srivastava, R. B. & Yu, N. T. Resonance Raman investigation of carbon monoxide bonding in (carbon monoxy)hemoglobin and -myoglobin: �E EE 1⁄4 red Eoxo are the thermodynamic potentials for water oxidation and EEfullcell 1⁄4 where Efull cell is the applied voltage of the MEA system and Eo 1⁄4 Eoxo I �E o . o Eox � Ered ́ FEethanol ð3Þ and E red o Eo Efull cell ́FEethanol ð4Þ red Materials characterization. Scanning electron microscopy was performed using a Hitachi S-5200. X-ray photoelectron spectroscopy measurements were carried out using a Thermo Scientific K-Alpha spectrophotometer with a monochromated Al Kα X-ray radiation source. X-ray diffraction patterns were recorded on a Rigaku MiniFlex600 G6. ICP–MS was measured on a Bruker Aurora M90. Hard XAS measurements were performed using a modified flow cell59 at the 9BM beamline of the Advanced Photon Source located in the Argonne National Laboratory. XAS data were processed with Demeter (v.0.9.26)60. In situ Raman measurements were carried out using a Renishaw inVia Raman microscope in a modified flow cell (Supplementary Fig. 24) with a water immersion objective. A 785-nm laser was used and signals were recorded using a 5-s integration and by averaging five scans. The gas (CO2,Arand13CO2)withaflowrateof40standardcm3min−1wasflowedthroughthe cell for corresponding experiments. An Ag/AgCl (3 M KCl) electrode and a Pt wire were used as the reference and counter electrodes, respectively, in all measurements. Data availability The datasets generated during, and/or analysed during, the present study, are available from the corresponding author on reasonable request. Received: 26 April 2019; Accepted: 14 October 2019; Published online: 16 December 2019 references 1. Ross, M. B. et al. Designing materials for electrochemical carbon dioxide recycling. Nat. Catal. 2, 648–658 (2019). 2. Birdja, Y. Y. et al. Advances and challenges in understanding the electrocatalytic conversion of carbon dioxide to fuels. Nat. Energy 4, 732–745 (2019). 3. Shih, C. F., Zhang, T., Li, J. & Bai, C. Powering the future with liquid sunshine. Joule 2, 1925–1949 (2018). 4. Spurgeon, J. & Kumar, B. A comparative technoeconomic analysis of pathways for commercial electrochemical CO2 reduction to liquid products. Energy Environ. Sci. 11, 1536–1551 (2018). 5. Hori, Y. in Modern Aspects of Electrochemistry Vol. 42 (eds Vayenas, C. G. et al.) 89–189 (Springer, 2008). 6. Gao, D., Arán-Ais, R. M., Jeon, H. S. & Roldan Cuenya, B. Rational catalyst and electrolyte design for CO2 electroreduction towards multicarbon products. Nat. Catal. 2, 198–210 (2019). 7. Kortlever, R., Shen, J., Schouten, K. J., Calle-Vallejo, F. & Koper, M. T. Catalysts and reaction pathways for the electrochemical reduction of carbon dioxide. J. Phys. Chem. Lett. 6, 4073–4082 (2015). 8. Kuhl, K. P., Cave, E. R., Abram, D. N. & Jaramillo, T. F. New insights into the electrochemical reduction of carbon dioxide on metallic copper surfaces. Energy Environ. Sci. 5, 7050–7059 (2012). 9. Ma, S. et al. One-step electrosynthesis of ethylene and ethanol from CO2 in an alkaline electrolyzer. J. Power Sources 301, 219–228 (2016). 10. Dinh, C.-T. et al. CO2 electroreduction to ethylene via hydroxide-mediated copper catalysis at an abrupt interface. Science 360, 783–787 (2018). 11. Jiang, K. et al. Metal ion cycling of Cu foil for selective C–C coupling in electrochemical CO2 reduction. Nat. Catal. 1, 111–119 (2018). 12. Clark, E. L., Hahn, C., Jaramillo, T. F. & Bell, A. T. Electrochemical CO2 reduction over compressively strained CuAg surface alloys with enhanced multi-carbon oxygenate selectivity. J. Am. Chem. Soc. 139, 15848–15857 (2017). 13. Hoang, T. T. H. et al. Nano porous 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). 14. Li, C. W., Ciston, J. & Kanan, M. W. Electroreduction of carbon monoxide to liquid fuel on oxide-derived nanocrystalline copper. Nature 508, 504–507 (2014). 15. Zhuang, T.-T. et al. Steering post-C–C coupling selectivity enables high efficiency electroreduction of carbon dioxide to multi-carbon alcohols. Nat. Catal. 1, 421–428 (2018). 16. Jouny, M., Luc, W. W. & Jiao, F. General techno-economic analysis of CO2 electrolysis systems. Ind. Eng. Chem. Res. 57, 2165–2177 (2018). NATurE CATALYSiS | VOL 3 | JanUarY 2020 | 75–82 | www.nature.com/natcatal 81PDF Image | Cooperative CO2-to-ethanol conversion via enriched intermediates
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