TY - JOUR
T1 - In situ Spectroscopy
T2 - Delineating the mechanistic understanding of electrochemical energy reactions
AU - Theerthagiri, Jayaraman
AU - Karuppasamy, K.
AU - Justin Raj, C.
AU - Aruna Kumari, M. L.
AU - John Kennedy, L.
AU - Maia, Gilberto
AU - Vadivel, Neshanth
AU - Prasad Murthy, Arun
AU - Alfantazi, Akram
AU - Kheawhom, Soorathep
AU - Choi, Myong Yong
N1 - Publisher Copyright:
© 2025 Elsevier Ltd
PY - 2025/6
Y1 - 2025/6
N2 - The development of in situ spectroscopy methods has enabled detailed studies of the surface chemistry and structures of electrodes and/or electrocatalysts under active electrochemical conditions, providing real-time insights into reaction pathways at the electrode–electrolyte interface, which is mandatory for understanding electrochemical processes in energy devices. Key challenges in understanding the high electrochemical selectivity and activity of catalysts for energy reactions include measuring reaction kinetics, detecting changes in the chemical environment, identifying reaction intermediates, and linking material properties to device performance. This review examines the advanced utilities of various in situ and operando spectroscopic methods, such as Fourier transform infrared, Raman, X-ray absorption, and X-ray photoelectron spectroscopy, in the study of rechargeable lithium-ion batteries, supercapacitors, water-splitting (O2 and H2 evolution), and hybrid electrolysis with small molecule oxidation into hydrogen fuel and value-added chemical production. Emphasizing the significance of the various in situ/operando methods in optimizing catalyst design and improving energy storage and conversion efficiency and durability, we provide a systematic assessment of their roles in addressing major challenges in energy material research, summarizing their operational mechanisms, benefits, and limitations, and delivering guidance for future experimental strategies.
AB - The development of in situ spectroscopy methods has enabled detailed studies of the surface chemistry and structures of electrodes and/or electrocatalysts under active electrochemical conditions, providing real-time insights into reaction pathways at the electrode–electrolyte interface, which is mandatory for understanding electrochemical processes in energy devices. Key challenges in understanding the high electrochemical selectivity and activity of catalysts for energy reactions include measuring reaction kinetics, detecting changes in the chemical environment, identifying reaction intermediates, and linking material properties to device performance. This review examines the advanced utilities of various in situ and operando spectroscopic methods, such as Fourier transform infrared, Raman, X-ray absorption, and X-ray photoelectron spectroscopy, in the study of rechargeable lithium-ion batteries, supercapacitors, water-splitting (O2 and H2 evolution), and hybrid electrolysis with small molecule oxidation into hydrogen fuel and value-added chemical production. Emphasizing the significance of the various in situ/operando methods in optimizing catalyst design and improving energy storage and conversion efficiency and durability, we provide a systematic assessment of their roles in addressing major challenges in energy material research, summarizing their operational mechanisms, benefits, and limitations, and delivering guidance for future experimental strategies.
KW - Electrochemical energy reactions
KW - Electrode/electrolyte interface reactions
KW - Energy conversion and storage
KW - In situ/operando spectroscopy
KW - Real-time reaction monitoring
UR - https://www.scopus.com/pages/publications/85217066179
U2 - 10.1016/j.pmatsci.2025.101451
DO - 10.1016/j.pmatsci.2025.101451
M3 - Review article
AN - SCOPUS:85217066179
SN - 0079-6425
VL - 152
JO - Progress in Materials Science
JF - Progress in Materials Science
M1 - 101451
ER -
