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Electrochemical Energy Reviews ›› 2026, Vol. 9 ›› Issue (2): 12-.doi: 10.1007/s41918-026-00278-z

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Multiple In Situ/Operando Synchrotron Spectroscopic Characterizations Decrypting Electrocatalytic Water Splitting Dynamics

Yuanli Li1, Mikhail A. Soldatov2, Bogdan O. Protsenko2, Alexander A. Guda2, Daiki Kido3,4, Weiren Cheng5, Fengwen Pan6, Qinghua Liu7   

  1. 1. Innovation Center of Nuclear Environmental Safety Technology, School of Materials and Chemistry, Southwest University of Science and Technology, Mianyang, 621010, Sichuan, China;
    2. The Smart Materials Research Institute, Southern Federal University, Rostov-on-Don, 344090, Rostov Oblast, Russia;
    3. Institute of Materials Structure Science, High Energy Accelerator Research Organization, Tsukuba, 3050801, Ibaraki, Japan;
    4. Materials Structure Science Program, Graduate Institute for Advanced Studies, Tsukuba, 3050801, Ibaraki, Japan;
    5. Department of Materials Science and Engineering, University of Science and Technology of China, Hefei, 230026, Anhui, China;
    6. National Center of Technology Innovation for Fuel Cell, Weichai Power Co., Ltd., Weifang, 261205, Shandong, China;
    7. National Synchrotron Radiation Laboratory, University of Science and Technology of China, Hefei, 230029, Anhui, China
  • 收稿日期:2025-08-29 修回日期:2025-11-17 接受日期:2026-01-11 出版日期:2026-06-20 发布日期:2026-05-13
  • 通讯作者: Fengwen Pan Email:E-mail:panfengwen@outlook.com;Qinghua Liu Email:E-mail:qhliu@ustc.edu.cn E-mail:panfengwen@outlook.com;qhliu@ustc.edu.cn
  • 基金资助:
    This work was supported by National Key R&D Program of China (2022YFB4004400 (F. W. P.)), National Natural Science Foundation of China (12305366 (Y. L. L.)), a grant from the Russian Science Foundation (25-42-00116 (M. A. S.)), the Taishan Industrial Experts Program, and University of Science and Technology of China-Southwest University of Science and Technology Counterpart Cooperation and Development Joint Fund (24LHJJ04 (Q. H. L.)).

Multiple In Situ/Operando Synchrotron Spectroscopic Characterizations Decrypting Electrocatalytic Water Splitting Dynamics

Yuanli Li1, Mikhail A. Soldatov2, Bogdan O. Protsenko2, Alexander A. Guda2, Daiki Kido3,4, Weiren Cheng5, Fengwen Pan6, Qinghua Liu7   

  1. 1. Innovation Center of Nuclear Environmental Safety Technology, School of Materials and Chemistry, Southwest University of Science and Technology, Mianyang, 621010, Sichuan, China;
    2. The Smart Materials Research Institute, Southern Federal University, Rostov-on-Don, 344090, Rostov Oblast, Russia;
    3. Institute of Materials Structure Science, High Energy Accelerator Research Organization, Tsukuba, 3050801, Ibaraki, Japan;
    4. Materials Structure Science Program, Graduate Institute for Advanced Studies, Tsukuba, 3050801, Ibaraki, Japan;
    5. Department of Materials Science and Engineering, University of Science and Technology of China, Hefei, 230026, Anhui, China;
    6. National Center of Technology Innovation for Fuel Cell, Weichai Power Co., Ltd., Weifang, 261205, Shandong, China;
    7. National Synchrotron Radiation Laboratory, University of Science and Technology of China, Hefei, 230029, Anhui, China
  • Received:2025-08-29 Revised:2025-11-17 Accepted:2026-01-11 Online:2026-06-20 Published:2026-05-13
  • Contact: Fengwen Pan Email:E-mail:panfengwen@outlook.com;Qinghua Liu Email:E-mail:qhliu@ustc.edu.cn E-mail:panfengwen@outlook.com;qhliu@ustc.edu.cn
  • Supported by:
    This work was supported by National Key R&D Program of China (2022YFB4004400 (F. W. P.)), National Natural Science Foundation of China (12305366 (Y. L. L.)), a grant from the Russian Science Foundation (25-42-00116 (M. A. S.)), the Taishan Industrial Experts Program, and University of Science and Technology of China-Southwest University of Science and Technology Counterpart Cooperation and Development Joint Fund (24LHJJ04 (Q. H. L.)).

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摘要： Electrocatalytic water splitting represents a sustainable and efficient approach for producing high-purity hydrogen, playing an increasingly pivotal role in addressing global energy sustainability challenges. However, dynamic and complex electrocatalytic processes pose significant obstacles to unraveling electrocatalytic mechanisms and advancing catalyst design. This review first discusses fundamental principles for conducting reliable in situ/operando synchrotron radiation (SR) spectroscopic measurements in electrocatalytic systems, proposing guidelines for standardizing practices across the community. Then, cutting-edge in situ/operando SR-based spectroscopic techniques applied in electrocatalytic water splitting are systematically examined, highlighting their distinctive advantages while critically evaluating inherent methodological limitations. Moving beyond conventional single-technique approaches, we focus on complementary probes based on in situ/operando multi-SR spectroscopic technologies to achieve panoramic visualization of the dynamic evolution for the water splitting process, spanning from the atomic and molecular scales to the electronic level. Finally, key bottlenecks and frontier research opportunities are outlined, aiming to inspire a paradigm shift from fragmented analysis toward integrated, system-level mechanistic understanding in electrocatalytic water splitting.The standardized principle of in situ/operando synchrotron radiation characterization has been proposed, and multiple technical probes have been integrated to achieve panoramic and multiscale visualization of water splitting, guiding the future of rational catalyst design.

关键词: In situ, Operando, Synchrotron radiation, Water splitting, Electrocatalysis

Abstract: Electrocatalytic water splitting represents a sustainable and efficient approach for producing high-purity hydrogen, playing an increasingly pivotal role in addressing global energy sustainability challenges. However, dynamic and complex electrocatalytic processes pose significant obstacles to unraveling electrocatalytic mechanisms and advancing catalyst design. This review first discusses fundamental principles for conducting reliable in situ/operando synchrotron radiation (SR) spectroscopic measurements in electrocatalytic systems, proposing guidelines for standardizing practices across the community. Then, cutting-edge in situ/operando SR-based spectroscopic techniques applied in electrocatalytic water splitting are systematically examined, highlighting their distinctive advantages while critically evaluating inherent methodological limitations. Moving beyond conventional single-technique approaches, we focus on complementary probes based on in situ/operando multi-SR spectroscopic technologies to achieve panoramic visualization of the dynamic evolution for the water splitting process, spanning from the atomic and molecular scales to the electronic level. Finally, key bottlenecks and frontier research opportunities are outlined, aiming to inspire a paradigm shift from fragmented analysis toward integrated, system-level mechanistic understanding in electrocatalytic water splitting.The standardized principle of in situ/operando synchrotron radiation characterization has been proposed, and multiple technical probes have been integrated to achieve panoramic and multiscale visualization of water splitting, guiding the future of rational catalyst design.

Key words: In situ, Operando, Synchrotron radiation, Water splitting, Electrocatalysis

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