Surface-enhanced vibrational spectroscopies in electrocatalysis: Fundamentals, challenges, and perspectives

doi:10.1016/S1872-2067(22)64157-3

Abstract

Abstract:

Electrocatalysis offers a promising approach towards chemical synthesis driven by renewable energy. Molecular level understanding of the electrochemical interface remains challenging due to its compositional and structural complexity. In situ interfacial specific characterization techniques could help uncover structure-function relationships and reaction mechanism. To this end, electrochemical surface-enhanced Raman spectroscopy (SERS) and surface-enhanced infrared absorption spectroscopy (SEIRAS) thrive as powerful techniques to provide fingerprint information of interfacial species at reaction conditions. In this review, we first introduce the fundamentals of SERS and SEIRAS, followed by discussion regarding the technical challenges and potential solutions. Finally, we highlight future directions for further development of surface-enhanced spectroscopic techniques for electrocatalytic studies.

Key words: Surface-enhanced Raman spectroscopy, Surface-enhanced infrared absorption spectroscopy, In situ characterization, Electrocatalysis, Structure-function relationship, Reaction mechanism

Hai-Sheng Su, Xiaoxia Chang, Bingjun Xu. Surface-enhanced vibrational spectroscopies in electrocatalysis: Fundamentals, challenges, and perspectives[J]. Chinese Journal of Catalysis, 2022, 43(11): 2757-2771.

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Figures/Tables 8

Fig. 1. Schematic of surface plasmonic resonance (a) and the electromagnetic enhancement of SERS (b). (c) Transmission electron microscopy image of typical Au@SiO2 nanoparticles with 55 nm-Au core and 2 nm-SiO2 shell. Reprinted with permission from Ref. [28]. Copyright 2020, American Chemical Society.

Fig. 2. Schematics of SERS nanostructures to monitor in situ electrocatalytic reactions. (a) SERS core-shell; (b) SHINs-satellite; (c) SHINs on flat electrodes.

Fig. 3. Schematics of two typical electrochemical spectral cells for SERS experiments. (a) A home-built cell. Reprinted with permission from Ref. [51]. Copyright 2013, Nature America, Inc. (b) A commercial cell. Reprinted with permission from Ref. [28]. Copyright 2020, American Chemical Society.

Fig. 4. Schematic of internal (a) and external (b) reflection modes for in situ FTIR experiments.

Fig. 5. Schematics of electrochemical cells for in situ ATR-SEIRAS experiments. (a) A typical cell. Reprinted with permission from Ref. [55]. Copyright 2019, American Chemical Society. (b) A side-facing cell. Reprinted with permission from Ref. [64]. Copyright 2022, Springer Nature. (c) A side-facing sell with stirring. Reprinted with permission from Ref. [65]. Copyright, 2020 American Chemical Society. (d) A modified cell for both in situ SEIRAS and SERS measurements. Reprinted with permission from Ref. [64]. Copyright 2022, Springer Nature.

Table 1 Comparison of surface-enhanced Raman and infrared absorption spectroscopies. E represents the enhancement of electromagnetic field.

Characteristic	SERS	SEIRAS
Vibrational mode	Changing polarizability	Changing dipole moment
Optical cross-section	Raman scattering ~10^-30 cm² sr^-1	IR absorption ~10^-20 cm² sr^-1
Spectral range	~10-4000 cm^-1	~1000-4000 cm^-1 for conventional Si prisms (600-4000 cm^-1 with thin micromachined Si wafers)
Absorption of H₂O	Weak	Strong
Surface enhancement	Proportional to E⁴, routinely larger than 10⁶	Proportional to E², usually 10-10³
Irradiation source	Monochromatic laser, typically visible or near-IR laser	Continuum wavelength, typically in mid-IR region
Photo damage	Relatively high	Relatively low

Fig. 6. (a) In situ SEIRAS and SERS spectra on oxide-derived Cu film. (b) Plots of CO peak frequency as a function of potential. The Stark tuning rates were labeled. (c) In situ SEIRA spectra on oxide-derived Cu film at -0.7 VRHE with and without stirring. (d) Normalized peak area of COatop peaks (blue) and the current density (black) during the SEIRAS test in (c). Reprinted with permission from Ref. [74]. Copyright 2022, Springer Nature.

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