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Nano Research 2023, 16(7): 10011-10017 https://doi.org/10.1007/s12274-023-5664-4
Research Article | Issue | Published: 13 March 2023

Fast Scan mode of scanning electrochemical microscopy: In-situ characterization of phase transition and mapping the hydrogen evolution activity for MoS2

Show Author's Information Zhenyu Wang1,  Tong Sun1( ),  Changan HuangFu2,  Sisi Jiang1,  Chaoqun Gu1,  Liying Jiao2,  Zonghua Wang1( )
College of Chemistry and Chemical Engineering, College of Materials Science and Engineering, Shandong Sino-Japanese Center for Collaborative Research of Carbon Nanomaterials, Instrumental Analysis Center of Qingdao University, Qingdao University, Qingdao 266071, China
Key Laboratory of Organic Optoelectronics and Molecular Engineering of the Ministry of Education, Department of Chemistry, Tsinghua University, Beijing 100084, China
Keywords:
molybdenum disulfide, phase transition, hydrogen evolution reaction, scanning electrochemical microscopy, high-speed scanning
Topics:
Electron microscopy
Cite this article:
Wang Z, Sun T, HuangFu C, et al. Fast Scan mode of scanning electrochemical microscopy: In-situ characterization of phase transition and mapping the hydrogen evolution activity for MoS2. Nano Research, 2023, 16(7): 10011-10017. https://doi.org/10.1007/s12274-023-5664-4
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Abstract Full text Electronic supplementary material About this article

Scanning electrochemical microscopy (SECM) is an attractive technology to in-situ characterize the structural evolution and catalytic performance for various electrocatalysts. However, spatial and temporal resolution coupling are still the obstacles that limit its wide applications. Herein, a new operation mode, Fast Scan mode, was developed by improving the dual-pass scan mode, designing novel hardware structure, and employing thermal drift calibration software to achieve a high spatial and temporal resolution simultaneously. The temporal speed can achieve 4 Hz for a high spatial resolution (less than 30 nm) image. This operation mode was employed to dynamically track the phase transition process of molybdenum disulfide (MoS2) over time and characterize the hydrogen evolution reaction (HER) catalytic activity on the edge of semiconducting MoS2 quantitatively while minimizing the diffusional broadening effect and total amount of catalytic products generated above the surface. This new approach should be useful for in-situ tracking dynamic electrochemical processes, establishing the structure-activity relationship for structural complex electrocatalysts, and offering a strategy for high-speed scanning with other electrochemical imaging techniques.


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About this article

Fast Scan mode of scanning electrochemical microscopy: In-situ characterization of phase transition and mapping the hydrogen evolution activity for MoS2

Show Author's information Zhenyu Wang1, Tong Sun1( ), Changan HuangFu2, Sisi Jiang1, Chaoqun Gu1, Liying Jiao2, Zonghua Wang1( )
College of Chemistry and Chemical Engineering, College of Materials Science and Engineering, Shandong Sino-Japanese Center for Collaborative Research of Carbon Nanomaterials, Instrumental Analysis Center of Qingdao University, Qingdao University, Qingdao 266071, China
Key Laboratory of Organic Optoelectronics and Molecular Engineering of the Ministry of Education, Department of Chemistry, Tsinghua University, Beijing 100084, China

Abstract

Scanning electrochemical microscopy (SECM) is an attractive technology to in-situ characterize the structural evolution and catalytic performance for various electrocatalysts. However, spatial and temporal resolution coupling are still the obstacles that limit its wide applications. Herein, a new operation mode, Fast Scan mode, was developed by improving the dual-pass scan mode, designing novel hardware structure, and employing thermal drift calibration software to achieve a high spatial and temporal resolution simultaneously. The temporal speed can achieve 4 Hz for a high spatial resolution (less than 30 nm) image. This operation mode was employed to dynamically track the phase transition process of molybdenum disulfide (MoS2) over time and characterize the hydrogen evolution reaction (HER) catalytic activity on the edge of semiconducting MoS2 quantitatively while minimizing the diffusional broadening effect and total amount of catalytic products generated above the surface. This new approach should be useful for in-situ tracking dynamic electrochemical processes, establishing the structure-activity relationship for structural complex electrocatalysts, and offering a strategy for high-speed scanning with other electrochemical imaging techniques.

Keywords: molybdenum disulfide, phase transition, hydrogen evolution reaction, scanning electrochemical microscopy, high-speed scanning

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Publication history
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Acknowledgements

Publication history

Received: 28 January 2023
Revised: 08 March 2023
Accepted: 12 March 2023
Published: 13 March 2023
Issue date: July 2023

Copyright

© Tsinghua University Press 2023

Acknowledgements

Acknowledgements

The support of this work by the National Natural Science Foundation of China (No. 22204088), the Natural Science Foundation of Shandong Province (Nos. ZR202103040753 and ZR2020MB063) and the Taishan Scholar Program of Shandong Province (No. ts201511027) is gratefully acknowledged. The authors would like to thank Dr. Gong Zhang from Tsinghua University and Dr. Michael V. Mirkin from City University of New York for helpful discussions. And the authors also thank Dr. Xiyue Cao, Dr. Huiqi Wang, Dr. Lili Lv and Dr. Ru Li from Instrumental Analysis Center of Qingdao University for their assistance with the characterization of MoS2.

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