Progress in tracking electrochemical CO2 reduction intermediates over single-atom catalysts using operando ATR-SEIRAS

doi:10.1016/S1872-2067(24)60068-9

Chinese Journal of Catalysis ›› 2024, Vol. 62: 32-52.DOI: 10.1016/S1872-2067(24)60068-9

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Progress in tracking electrochemical CO₂ reduction intermediates over single-atom catalysts using operando ATR-SEIRAS

Jing Yan^a, Jiaqi Ni^a, Hongli Sun^a^,^*(), Chenliang Su^a^,^*(), Bin Liu^b^,^c^,^*()

^aInternational Collaboration Laboratory of 2D Materials for Optoelectronics Science and Technology of Ministry of Education, Institute of Microscale Optoelectronics, Shenzhen University, Shenzhen 518060, Guangdong, China
^bDepartment of Materials Science and Engineering, City University of Hong Kong, Hong Kong SAR 999077, China
^cDepartment of Chemistry, Hong Kong Institute of Clean Energy (HKICE) & Center of Super-Diamond and Advanced Films (COSDAF), City University of Hong Kong, Hong Kong SAR 999077, China

Received:2024-03-21 Accepted:2024-05-27 Online:2024-07-18 Published:2024-07-10
Contact: *E-mail: hlsun@szu.edu.cn (H. Sun), chmsuc@szu.edu.cn (C. Su), bliu48@cityu.edu.hk (B. Liu).
About author:Hongli Sun (Institute of Microscale Optoelectronics, Shenzhen University) received her bachelor’s and master’s degrees at Wuhan University of Technology, China in 2013 and 2016, respectively, and completed his doctoral degree at the Chinese University of Hongkong in 2019. After spending two years as postdoctoral fellow in Shenzhen University, China, she joined Institute of Microscale Optoelectronics at Shenzhen University as an Assistant Professor in March 2023. Her research focuses on photo(electro)catalysis for energy conversion and environmental remediation and in-situ/operando characterizations.
Chenliang Su (Institute of Microscale Optoelectronics, Shenzhen University) received his BS degree (2005) and PhD degree (2010) in the Department of Chemistry from Zhejiang University of China (2010). After that he worked as a research fellow at the Advanced 2D Materials and Graphene Research Centre in the National University of Singapore (2010-2015). He is now a full-professor at the International Collaborative Laboratory of 2D Materials for Optoelectronics Science and Technology (ICL-2D MOST), Shenzhen University and a Principal Investigator of ICL-2D MOST in materials science. His current interests focus on the chemical design of nano materials for catalysis and energy related applications.
Bin Liu (Department of Materials Science and Engineering, City University of Hong Kong) received his bachelor of engineering (1st Class Honours) and master of engineering degrees at the National University of Singapore, Singapore in 2002 and 2004, respectively, and completed his doctoral degree at the University of Minnesota, USA in 2011. After spending a year as postdoctoral fellow in the University of California Berkeley, USA, he joined School of Chemical and Biomedical Engineering at Nanyang Technological University as an Assistant Professor in June 2012 and was promoted to Associate Professor in March 2017. In February 2023, Professor Liu joined the Department of Materials Science and Engineering at City University of Hong Kong as a Professor. His research focuses on photo(electro)catalysis and in-situ/operando characterization.
Supported by:
National Natural Science Foundation of China(21972094);National Natural Science Foundation of China(22102102);National Natural Science Foundation of China(22372102);Educational Commission of Guangdong Province(839-0000013131);Shenzhen Science and Technology Program(RCJC20200714114434086);City University of Hong Kong start up fund, and the Guangdong Basic and Applied Basic Research Foundation(2020A1515010982);China Postdoctoral Science Foundation(2023M742395);Shenzhen Science and Technology Program(20231122120657001);Shenzhen University Start Up Fund, Shenzhen Peacock Plan(20210308299C);Research Team Cultivation Program of Shenzhen University(2023QNT013)

Abstract

Abstract:

Owing to the multiple proton-coupled electron transfer steps involved in the electrochemical carbon dioxide reduction reaction (CO₂RR), single-atom catalysts (SACs) are ideal platforms for studying such complex chemical reaction processes. The structural simplicity and homogeneity of SACs facilitate the understanding of the structure-performance relationship and reaction mechanisms of the CO₂RR. Operando attenuated total reflection surface-enhanced infrared absorption spectroscopy (ATR-SEIRAS) is a valuable tool to identify the dynamic intermediate transformation processes in the CO₂RR occurring on SACs and to study the impact of local reaction environments on the CO₂RR performance. This article reviews operando ATR-SEIRAS and its key applications in the SAC-catalyzed CO₂RR. The review briefly introduces the surface enhancement mechanism of electrochemical in situ infrared spectroscopy, formation mechanisms of the C1 and C2 products, function of operando ATR-SEIRAS in investigating the mechanisms of single-/dual-atom catalysts in converting CO₂/CO to C1 and C2 products, and methods of using spectroscopic information to determine the interfacial H₂O and local pH at the electrode. Finally, the review provides perspectives on the future development of operando ATR-SEIRAS.

Key words: Electrochemical carbon dioxide, reduction, Single-atom catalyst, Electrochemical operando attenuated, total reflection surface-enhanced, infrared absorption spectroscopy, Reaction dynamic transformation, processes, Interfacial H₂O

Jing Yan, Jiaqi Ni, Hongli Sun, Chenliang Su, Bin Liu. Progress in tracking electrochemical CO₂ reduction intermediates over single-atom catalysts using operando ATR-SEIRAS[J]. Chinese Journal of Catalysis, 2024, 62: 32-52.

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Figures/Tables 14

Scheme 1. Schematic illustration showing the applications of operando IR spectroscopy for studying the CO2RR catalyzed over SACs.

Fig. 3. Schematic diagrams illustrating the four in situ IR spectroscopy modes: transmission (a), external reflection (the resistance of the solution is high, resulting in a correspondingly slow potential response; the surface should be relatively smooth) (b), internal reflection Kretschmann (the resistance of the solution is low, resulting in a correspondingly rapid potential response (c); suitable for metal thin-film electrodes), and internal reflection Otto thin-layer modes (the resistance of the solution is high, resulting in a correspondingly slow potential response; suitable for powder electrodes and other non-mirror reflective electrodes) (d). (e) Intensity of the s and p components of incident and reflected beams. Reprinted with permission from Ref. [40]. Copyright 2019, John Wiley and Sons.

Fig. 4. Most commonly used geometries for IR experiments at the electrode-electrolyte interface: external (a) and internal (b) reflections. (c) Excitation of the localized surface plasmon resonance (LSPR). (d) Simulated electromagnetic field strength around a nanoparticle. (e) Schematic illustration showing the dipole change in the same/opposite direction as the dipole of a vibrational mode normal/parallel to the surface. Reprinted with permission from Ref. [40]. Copyright 2019, John Wiley and Sons.

Table 1 Comparison of the intensity of in situ IR signals during CO2RR recorded using different enhancement modes.

Catalyst	Electrolyte		Modes for in situ IR spectroscopy	Intensity of in situ IR signals	Ref.
Nonmetal phosphorus SAC (P-SAC-NG)	0.5 mol L^-1 KHCO₃		internal reflection	strong	[17]
SnPc/CNT-OH	0.1 mol L^-1 K₂SO₄		internal reflection	strong	[88]
Pb1Cu SAA	0.5 mol L^-1 KHCO₃		internal reflection	strong	[91]
Cu-SAs/HGDY	0.5 mol L^-1 KHCO₃		internal reflection	strong	[100]
Ni SAC	0.5 mol L^-1 KHCO₃		no enhancement	weak	[80]
Ni-NCN	0.5 mol L^-1 KHCO₃	no enhancement		weak	[85]

Fig. 5. (a) Schematic diagram illustrating the Ni-(CO)2 and Ni-CO models. (b) Synchrotron radiation IR absorption spectroscopy (SR-IRAS) spectra collected in the potential range of -0.2 to -0.8 VRHE in 0.5 mol L-1 KHCO3. Reprinted with permission from Ref. [80]. Copyright 2023, Springer Nature. (c) Schematic diagram illustrating the surface coverage of CO. In situ ATR-SEIRAS spectra of (d) P-SAC-NG collected in CO2-saturated 0.5 mol L-1 KHCO3 in the potential window of OCV to -1.1 V vs. RHE. Reprinted with permission from Ref. [17]. Copyright 2023, The Royal Society of Chemistry. (e) COOH* intermediate model. (f) Operando Fourier transform IR (FTIR) spectrum of Ni-NCN. Reprinted with permission from Ref. [85]. Copyright 2023, Elsevier.

Fig. 6. (a) Proposed reaction pathway of the CO2RR over the O-Sn-N4 site and identification of the surface reactive species. (b,c) Operando ATR-SEIRAS spectra of SnPc/CNT-OH collected at various applied cathodic potentials (from 0 to -1.5 V vs. RHE and from -1.5 V vs. RHE to 0 V) in CO2-saturated 0.1 mol L-1 K2SO4. Reprinted with permission from Ref. [88]. Copyright 2023, American Chemical Society. (d) Schematic diagram illustrating the selective adsorption of CO2 at Cu sites. (e,f) In situ ATR-FTIR spectra recorded at different applied potentials (without iR compensation) for the Pb1Cu SAA. Reprinted with permission from Ref. [91]. Copyright 2021, Springer Nature. (g) Schematic diagram illustrating the adsorption behaviors and material transformations of Cu-SnO2 and SnO2 during CO2RR under low/high reduction potentials. (h) In situ ATR-IR results of Cu-SnO2 (left) and SnO2 (right) recorded at different potentials. Reprinted with permission from Ref. [94]. Copyright 2023, American Chemical Society.

Fig. 7. (a) Proposed CO2RR pathway over Cu-SAs/HGDY. (b) In situ ATR-FTIR spectra of Cu-SAs/HGDY recorded in the potential range of -0.7 to -1.5?V vs. RHE. Reprinted with permission from Ref. [100]. Copyright 2023, John Wiley and Sons. (c) Schematic illustration showing the formation of *CHO intermediates at Cu sites. In situ ATR-IR spectra for BNC-Cu (d) and NC-Cu (e). Reprinted with permission from Ref. [104]. Copyright 2023, Springer Nature. (f) DFT-optimized structures of H-CoPc-CO (top) and H-CoPc-CO (bottom). (g) In situ FTIR spectra of CoPc/MWCNT measured at E = -0.3? ?to?-0.8?V vs. RHE. Reprinted with permission from Ref. [112]. Copyright 2023, Springer Nature. (h) Model of CoTAPc and iminium-CONs. (i) In situ ATR-SEIRAS spectra recorded over iminium-CONs and CoTAPc in a CO2-saturated 0.5 mol L-1 KHCO3 solution. Reprinted with permission from Ref. [113]. Copyright 2023, John Wiley and Sons.

Fig. 8. (a) Proposed CO2RR mechanism on a Bi-decorated Cu alloy [BiCu(111)-SAA]. Detection of the reaction intermediates of the CO2RR on both BiCu-SAA and Cu-nano (Cu-N) catalysts. (b) Time-dependent in situ SEIRAS spectra obtained at -1.10 V vs. RHE. (c) Operando SR-FTIR spectra recorded at different potentials. Reprinted with permission from Ref. [118]. Copyright 2023, John Wiley and Sons. (d) Proposed CO2RR mechanism on a single-atom Ni with nanoscale Cu (Cu/Ni-NAC) catalyst. (e) In situ SEIRAS spectra of Cu/Ni-NAC catalysts recorded under CO2RR conditions. Reprinted with permission from Ref. [121]. Copyright 2022, American Chemical Society. (f) Proposed CO2RR mechanism over PcCu-Cu-O. (g,h) In situ ATR-FTIR spectra of PcCu-Cu-O recorded during electrochemical CO2RR. Reprinted with permission from Ref. [123]. Copyright 2021, American Chemical Society.

Fig. 9. (a) Local active site structure and intermediate state. (b) Operando SR-FTIR spectra of Cu/N0.14C. (c) Operando SR-FTIR spectra recorded over Cu/N0.14C in a D2O electrolyte. Reprinted with permission from Ref. [126]. Copyright 2022, Springer Nature. (d) Proposed mechanism of the CO2 reduction to EtOH over CuSn-HAB. (e) Time-dependent operando ATR-FTIR spectra recorded on CuSn-HAB at -0.57 V vs. RHE in a 1 mol L-1 KOH electrolyte. Reprinted with permission from Ref. [131]. Copyright 2023, American Chemical Society. (f) Electrocatalytic CO2RR to CH3COOH mechanism. (g) In situ ATR-FTIR spectra of PcCu-TFPN recorded during electrocatalytic CO2RR. Reprinted with permission from Ref. [135]. Copyright 2022, John Wiley and Sons.

Fig. 10. In situ ATR-SEIRAS spectra recorded over TeN2-CuN3 (a) and TeN3 (b) in a CO2-saturated KHCO3 solution. (c) Corresponding 3D intensity profiles of two pairs of DAC sites. Reprinted with permission from Ref. [141]. Copyright 2023, Springer Nature. In situ ATR-SEIRAS spectra recorded in the potential window of 0 to -0.9 V vs. RHE over Fe1/PNG (d) and Fe1/NG (e). Gaussian fits of three O-H stretching modes over Fe1/PNG (f) and Fe1/NG (g). Reprinted with permission from Ref. [145]. Copyright 2023, John Wiley and Sons. (h) Comparison of the ATR-SEIRAS spectra recorded over Fe1-NC, Mo1-NC, and DMCPFe1-Mo1-NC at -0.6 V vs. RHE. (i) In situ ATR-SEIRAS spectra recorded over DMCPFe1-Mo1-NC in CO2-saturated 0.5 mol L-1 KHCO3. (j) Proposed CO2RR mechanism of DMCPFe1-Mo1-NC. Reprinted with permission from Ref. [148]. Copyright 2023, American Chemical Society.

Fig. 11. Operando ATR-SEIRAS spectra of the CORR over B-CoPc-400 (a,c) and M-CoPc-400 (b,d) in CO-saturated 0.5 mol L-1 KOH. The spectra were collected at constant potentials with a 0.1 V interval in the cathodic direction from OCP to -0.9 V (vs. RHE). Reprinted with permission from Ref. [153]. Copyright 2023, Springer Nature. (e,f) In situ ATR-SEIRAS spectra recorded during CO electroreduction on Cu@NH2 and Cu in CO-saturated 0.5 mol L-1 KOH. (g) Top view images of *CO + H*, transition state 1, *CHO, *CHO + *CO, transition state 2, and *OCCHO on Cu@NH2(111) and Cu. Reprinted with permission from Ref. [155]. Copyright 2023, American Chemical Society.

Fig. 12. (a) Real-time ATR-SEIRAS spectra recorded during the cathodic scan over a Cu thin-film electrode. (b) ATR-IR spectra recorded over a bare ZnSe prism in a 0.1 mol L-1 K2CO3 + 0.1 mol L-1 KOH electrolyte. (c) Real-time ATR-SEIRAS spectra recorded during the anodic scan over a Cu thin-film electrode in a CO2-saturated 0.1 mol L-1 KHCO3 solution. Reprinted with permission from Ref. [102]. Copyright 2017, American Chemical Society. ATR-SEIRAS spectra (black line) and peak fits (red dashed line) in 0.1 mol L-1 NaHCO3 at -0.9 V vs. RHE under 1 atm CO2 (d) and 0.1 V vs. RHE at pH = 8.97 (e). Carbonate (purple) and bicarbonate (blue) peak positions and widths were obtained from the Gaussian fits of the pure carbonate (pH = 12.95) and bicarbonate (pH = 7.55) spectra. Reference spectra were collected in water at OCP. CO2 (aq.) spectra as a function of the potential without stirring (f) and under stirring at 1800 r min-1 (g) in CO2-saturated 0.5 mol L-1 NaHCO3. Surface pH (left axis) and the corresponding change in the proton ηc versus the uncorrected potential (left axis) in CO2-saturated 0.25 mol L-1 NaHCO3 (h), 0.5 mol L-1 NaHCO3 without stirring (solid squares) and under stirring at 1800 r min-1 (open squares) (i), and1.0 mol L-1 NaHCO3 (j). (k) Surface pH change versus current density in CO2-saturated 0.25 (red), 0.5 (purple), and 1.0 mol L-1 (black) NaHCO3 with (open squares) and without (filled squares) stirring. Reprinted with permission from Ref. [158]. Copyright 2018, American Chemical Society.

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Progress in tracking electrochemical CO₂ reduction intermediates over single-atom catalysts using operando ATR-SEIRAS

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