In situ studies of energy-related electrochemical reactions using Raman and X-ray absorption spectroscopy

doi:10.1016/S1872-2067(21)63874-3

Abstract

Abstract:

Electrochemical energy conversion technologies involving processes such as water splitting and O₂/CO₂reduction, provide promising solutions for addressing global energy scarcity and minimizing adverse environmental impact. However, due to a lack of an in-depth understanding of the reaction mechanisms and the nature of the active sites, further advancement of these techniques has been limited by the development of efficient and robust catalysts. Therefore, in situ characterization of these electrocatalytic processes under working conditions is essential. In this review, recent applications of in situ Raman spectroscopy and X-ray absorption spectroscopy for various nano- and single-atom catalysts in energy-related reactions are summarized. Notable cases are highlighted, including the capture of oxygen-containing intermediate species formed during the reduction of oxygen and oxidation of hydrogen, and the detection of catalyst structural transformations occurring with the change in potential during the evolution of oxygen and reduction of CO₂. Finally, the challenges and outlook for advancing in situ spectroscopic technologies to gain a deeper fundamental understanding of these energy-related electrocatalytic processes are discussed.

Key words: Raman spectroscopy, X-ray absorption spectroscopy, In situ characterization, Electrocatalysis, Energy conversion and storage

Heng-Quan Chen, Lie Zou, Di-Ye Wei, Ling-Ling Zheng, Yuan-Fei Wu, Hua Zhang, Jian-Feng Li. In situ studies of energy-related electrochemical reactions using Raman and X-ray absorption spectroscopy[J]. Chinese Journal of Catalysis, 2022, 43(1): 33-46.

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Figures/Tables 11

Fig. 1. The development and application of SERS.

Fig. 2. In situ EC-SHINERS spectra obtained during ORR of Pt (111) (a), Pt (100) (b), Pt (110) (c), Pt (311) (d), and Pt (211) (e) in 0.1 M O2-saturated HClO4 solution. Adapted with permission from Ref. [36,37]. Copyrights 2019 and 2020, Springer Nature and American Chemical Society. (f) SHINERS spectra of Pt (111), Pt (311), and P (211) in 0.1 M O2-saturated HClO4 solution at 0.8 V (vs. RHE). Adapted with permission from Ref. [37]. Copyright 2020, American Chemical Society.

Fig. 3. (a) Schematic diagram of in situ SERS employing the borrowing strategy; (b) In situ SERS spectra of Au@Pt and Au@PtNi in 0.1 M O2-saturated HClO4 solution; (c) Raman peak shift and half-wave potential vs. Ni content. Adapted with permission from Ref. [40]. Copyright 2020, American Chemical Society.

Fig. 4. (a) Schematic diagram of in situ SERS employing the SHINERS-satellite strategy; In situ SHINERS spectra of ORR on Pt3Co catalysts in 0.1 M HClO4 (b) and 0.1 M KOH (c). Adapted with permission from Ref. [41]. Copyright 2020, John Wiley and Sons.

Fig. 5. (a) In situ XANES of FePhenMOF-ArNH3; (b) In situ EXAFS of Fe PhenMOF-ArNH3; (c) Δμ-XANES of Fe-N-C obtained during ORR under potentials of 0.3 to 1.0 V; (d) Δμ-XANES derived from theoretical calculations and the Fe-N4-C8 model (inset). Adapted with permission from Ref. [45]. Copyright 2016, The Royal Society of Chemistry. (e) Three structural models of Fe-N4-Cx, labeled as D1, D2, and D3. Adapted with permission from Ref. [50]. Copyright 2015, American Chemical Society.

Fig. 6. In situ Raman spectra of Co (a), Au (b), ~0.4 ML Co oxides (c) on Au surfaces and ~87 ML Co oxides on Au surfaces (d) in 0.1 M KOH under various potentials. (a-d) Adapted with permission from Ref. [58]. Copyright 2011, American Chemical Society. (e) Chronopotentiometry measurements at 0.5 mA; (f) Raman spectra obtained in situ during the chronopotentiometry measurement. (e,f) Adapted with permission from Ref. [59]. Copyright 2019, John Wiley and Sons.

Fig. 7. (a) In situ Raman spectra of prepared NiSe2 in 1 M KOH. (a) Adapted with permission from Ref. [64]. Copyright 2020, John Wiley and Sons. In situ XANES (b) and Fourier-transformed EXAFS (c) of CoFeP during the OER in alkaline electrolyte. (b,c) Adapted with permission from Ref. [66]. Copyright 2019, American Chemical Society. (d) In situ Fourier-transformed EXAFS at Co k edge of Co-N-C. Adapted with permission from Ref. [69]. Copyright 2019, American Chemical Society.

Fig. 8. In situ SERS of Au@Pt (a) and Au @PtNi (b) in 0.1 M H2-saturated solution. (a,b) Adapted with permission from Ref. [75]. Copyright 2021, John Wiley and Sons. Ru K-edge in situ XANES of Ru/C (c) and PtRu/C (d) in H2-saturated solution under various potentials; In situ Δu-XANES of Ru/C (e) and PtRu/C (f) and their corresponding theoretical models (inset). (c-e) adapted with permission from Ref. [76]. Copyright 2017, John Wiley and Sons.

Fig. 9. In situ SERS of Ag@MoS2 in 0.1 M HClO4 electrolyte (a) and in 0.1 M DClO4 electrolyte (b). (a,b) adapted with permission from Ref. [81]. Copyright 2020, American Chemical Society. In situ Raman of SANi-I (c) and O-A-Ni-OH (d) under varying potentials. (c,d) adapted with permission from Ref. [83]. Copyright 2019, John Wiley and Sons.

Table 1 Various pathways for the CO2RR.

Half electrochemical reaction	Standard potential/ V (vs. RHE)
CO₂ + 2H⁺ + 2 e^- → HCOOH	-0.258
CO₂ + H₂O (l) + 2e^- → HCOO^- + OH^-	-1.078
CO₂+ 2H⁺ + 2 e^- → CO (g) + H₂O (l)	-0.106
CO₂ + 4H⁺ + 4 e^- → CH₂O (g) + H₂O (l)	-0.700
CO₂ + 3H₂O (l) + 4e^-→ CH₂O (g) + 4OH^-	-0.898
CO₂ + 6H⁺ +6e^- → CH₃OH (l) + H₂O (l)	0.016
CO₂ +5H₂O (l) + 6e^- → CH₃OH (l) + 6OH^-	-0.812
CO₂+ 8H⁺ + 8e^- → CH₄(g) + 2H₂O (l)	0.169
CO₂ + 6H₂O (l) + 8e^-→ CH₄(g) + 8OH^-	-0.659
2CO₂ + 2H⁺ +2e^- → H₂C₂O₄	-0.500
2CO₂ + 12H⁺ + 12e^- → CH₂CH₂ (g) + 4H₂O (l)	0.064
2CO₂ + 8H₂O (l) + 12e^- → CH₂CH₂ (g) + 12OH^-	-0.764
2CO₂ + 9H₂O (l) + 12e^- → CH₃CH₂OH + 12OH^-	-0.744

Fig. 10. (a) Ex situ Raman spectra of Cu, Zn, and CuxZn; In situ Raman spectra of Cu (b), Zn (c), and Cu4Zn (d). (a-d) Adapted with permission from Ref. [88]. Copyright 2016, American Chemical Society. Raman spectra focusing on the carboxyl/formate intermediate vibrational range for Cu, Cu12Sn, Cu5Sn6 at -0.4 V (vs. RHE) (e) and at -0.5 V (vs. RHE) (f). In situ Raman spectra of CO2RR on Cu5Sn6 (g) and Cu12Sn (h) in CO2-saturated 0.1 M KHCO3 electrolyte. (e-h) Adapted with permission from Ref. [89]. Copyright 2019, American Chemical Society. (i) In situ XANES of copper oxides and reference species. Adapted with permission from Ref. [90]. Copyright 2016, Springer Nature.

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