(Invited) In-Situ Synchrotron X-Ray Characterization of Electrocatalyst Structural Evolution during Reactions

Abstract

Meeting the global challenge of clean and sustainable energy calls for continuous advancements in functional materials designed for energy conversion, storage, and catalysis. The performance of such materials is inherently linked to their atomic and electronic configurations, as well as the interfacial dynamics that dictate their operational behavior. Synchrotron-based X-ray techniques offer powerful analytical capabilities, enabling precise characterization with exceptional elemental sensitivity and spatial resolution. Among these, X-ray absorption and emission spectroscopies stand out for their ability to unravel complex material architectures and elucidate interactions between key components. The integration of in situ and operando approaches further allows for real-time tracking of atomic and electronic structural changes under realistic operating environments—providing vital mechanistic insights to inform rational material design. Understanding the influence of solid–liquid interfaces on electrochemical processes demands careful investigation of surface chemistry at the electrode–electrolyte junction. In this presentation, I will showcase examples of dynamic transformations in surface composition and structure that critically affect a material’s catalytic performance for water splitting across various media. I will also highlight how NSRRC beamlines play a central role in advancing this research. Our findings emphasize the indispensable value of in situ and operando X-ray characterization techniques in uncovering the true mechanistic pathways of catalytic reactions. These insights serve as a bridge between fundamental design principles and the practical challenges encountered in real-world energy systems, where additional complexities must be addressed. References [1] Li,Y.; Peng,C.K.; Sun,.; Nicole, S.L.D.; Chang, Y.C.; Chen, S.Y.; Zhou, Y.; Lin, Y.G.; Lee, J.M.; Operando Elucidation of Hydrogen Production Mechanisms on Sub-Nanometric High-Entropy Metallenes. Nature Communications, 2024, 15, 10222. [2] Peng, C.K.; Lin, Y.C.; Chiang, C.L.; Qian, Z.; Huang, Y.C.; Dong, C.L.; Li, J.F.; Chen, C.T.; Hu, Z.; Chen, S.Y.; Lin, Y.G.; Zhang-Rice singlets state formed by two-step oxidation for triggering water oxidation under operando conditions. Nature Communications, 2023, 14, 529. [3] Lim, S.C.; Chiang, C.L.; Peng, C.K.; Wu, W.B.; Lin, Y.C.; Lin, Y.R.; Chen, C.L.; Lin, Y.G.; Realizing the bifunctional electrocatalysis via local charge rearrangement of α-CrOOH-modulated Co@CoMoOx for overall water splitting. Chemical Engineering Journal, 2023, 452, 139715. [4] Li, Y.; Peng, C.K.; Hu, H.; Chen, S.Y.; Choi, J.; Lin, Y.G.; Lee, J.M.; Interstitial boron-triggered electron-deficient Os aerogels for enhanced pH-universal hydrogen evolution. Nature Communications, 2022, 13, 1143. [5] Lin, Y.C.; Peng, C.K.; Lim, S.C.; Chen, C.L.; Nguyễn, T.N.; Wang, T.T.; Lin, M.C.; Hsu, Y.J.; Chen, S.Y.; Lin, Y.G.; Tailoring the Surface Oxygen Engineering of a Carbon-Quantum-Dot-Sensitized ZnO@H-ZnO1-x Multijunction toward Efficient Charge Dynamics and Photoactivity Enhancement. Applied Catalysis B: Environmental, 2021, 285, 119846.