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In situ electrochemical Raman spectroscopy and ab initio molecular dynamics study of interfacial water on a single-crystal surface

Nature Protocols volume 18, pages 883–901 (2023)Cite this article

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Abstract

The dynamics and chemistry of interfacial water are essential components of electrocatalysis because the decomposition and formation of water molecules could dictate the protonation and deprotonation processes on the catalyst surface. However, it is notoriously difficult to probe interfacial water owing to its location between two condensed phases, as well as the presence of external bias potentials and electrochemically induced reaction intermediates. An atomically flat single-crystal surface could offer an attractive platform to resolve the internal structure of interfacial water if advanced characterization tools are developed. To this end, here we report a protocol based on the combination of in situ Raman spectroscopy and ab initio molecular dynamics (AIMD) simulations to unravel the directional molecular features of interfacial water. We present the procedures to prepare single-crystal electrodes, construct a Raman enhancement mode with shell-isolated nanoparticle, remove impurities, eliminate the perturbation from bulk water and dislodge the hydrogen bubbles during in situ electrochemical Raman experiments. The combination of the spectroscopic measurements with AIMD simulation results provides a roadmap to decipher the potential-dependent molecular orientation of water at the interface. We have prepared a detailed guideline for the application of combined in situ Raman and AIMD techniques; this procedure may take a few minutes to several days to generate results and is applicable to a variety of disciplines ranging from surface science to energy storage to biology.

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Fig. 1: Schematic representation.
Fig. 2: Equipment setup.
Fig. 3: Schematic diagram and characterization of single crystals by CV.
Fig. 4: Characterization of SHINs.
Fig. 5: Confocal depth test of laser.
Fig. 6: SEM image of SHINs on Au single-crystal surface.
Fig. 7: Schematic diagram of electrochemical Raman cell.
Fig. 8: Schematic diagram of effective spot area.
Fig. 9: Schematic illustration of AIMD simulations for the analysis of interfacial water.
Fig. 10: Raman spectra.
Fig. 11: Enhancement test of SHINs.

Data availability

Data generated or analyzed during this study are included in this article and ref. 44. Source data are provided with this paper.

Code availability

The code that supports the findings of this research is available from the corresponding authors upon reasonable request.

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Acknowledgements

This work was financially supported by the National Key Research and Development Program of China (2019YFA0705400), the National Natural Science Foundation of China (21925404, 21991151, 21902137, 22104124, 22109003 and 22021001), the Shenzhen Fundamental Research Program (no. GXWD20201231165807007-20200807111854001), the Soft Science Research Project of Guangdong Province (2017B030301013), the ‘111’ Project (B17027) and the State Key Laboratory of Fine Chemicals, Dalian University of Technology (KF2002). We thank the Major Science and Technology Infrastructure Project of Material Genome Big-science Facilities Platform supported by Municipal Development and Reform Commission of Shenzhen.

Author information

Author notes

  1. These authors contributed equally: Yao-Hui Wang, Shunning Li.

Authors and Affiliations

  1. College of Materials, State Key Laboratory of Physical Chemistry of Solid Surfaces, MOE Key Laboratory of Spectrochemical Analysis and Instrumentation, iChEM, College of Chemistry and Chemical Engineering, College of Energy, College of Physical Science and Technology, Xiamen University, Xiamen, China

    Yao-Hui Wang, Ru-Yu Zhou, Yue-Jiao Zhang, Jin-Chao Dong, Zhi-Lin Yang, Zhong-Qun Tian & Jian-Feng Li

  2. School of Advanced Materials, Peking University, Shenzhen Graduate School, Shenzhen, China

    Shunning Li, Shisheng Zheng & Feng Pan

  3. Innovation Laboratory for Sciences and Technologies of Energy Materials of Fujian Province (IKKEM), Xiamen, China

    Yue-Jiao Zhang, Jin-Chao Dong, Zhong-Qun Tian & Jian-Feng Li

  4. College of Optical and Electronic Technology, China Jiliang University, Hangzhou, China

    Jian-Feng Li

  5. Shenzhen Research Institute of Xiamen University, Shenzhen, China

    Jian-Feng Li

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Contributions

J.-F.L., Z.-Q.T. and F.P. designed the project. Y.-H.W. and S.L. conceived of and designed the protocol. Y.-H.W., Y.-J.Z. and R.-Y.Z. performed the experiments and analyzed the results. S.L., Z.-L.Y. and S.Z. performed the computations and the data analysis. Y.-H.W., J.-C.D., Y.-J.Z. and S.L. wrote the protocol. All authors discussed the results and contributed to the manuscript review.

Corresponding authors

Correspondence to Feng Pan or Jian-Feng Li.

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Nature Protocols thanks Alexis Grimaud and the other, anonymous, reviewer(s) for their contribution to the peer review of this work.

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Key references using this protocol

Wang, Y. H. et al. Nature 600, 81–85 (2021): https://doi.org/10.1038/s41586-021-04068-z

Li, C. Y. et al. Nat. Mater. 18, 697–701 (2019): https://doi.org/10.1038/s41563-019-0356-x

Supplementary information

Source data

Source Data Fig. 3

CV data normalized by electrode area.

Source Data Fig. 4

Fig. 4b,c,e, background normalized Raman data; Fig. 4d, unprocessed Raman data.

Source Data Fig. 5

Recorded Raman intensity.

Source Data Fig. 10

Normalized Raman data.

Source Data Fig. 11

Fig.11a, background normalized Raman data; Fig. 11b, unprocessed Raman data.

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Wang, YH., Li, S., Zhou, RY. et al. In situ electrochemical Raman spectroscopy and ab initio molecular dynamics study of interfacial water on a single-crystal surface. Nat Protoc 18, 883–901 (2023). https://doi.org/10.1038/s41596-022-00782-8

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