Operando Structural Characterization of Model Electrodes using Surface X-ray Diffraction

Leon Jacobse^a

^aDepartment of Interface Science, Fritz Haber Institute of the Max Planck Society, 14195 Berlin, Germany

Materials for Sustainable Development Conference (MATSUS)
Proceedings of MATSUS Spring 2024 Conference (MATSUS24)

#InOpCat - In situ and operando characterization of electrocatalytic interfaces

Barcelona, Spain, 2024 March 4th - 8th

Organizers: Esther Alarcon-Llado, Jesus Barrio Hermida and Paula Sebastian Pascual

Invited Speaker, Leon Jacobse, presentation 300
DOI: https://doi.org/10.29363/nanoge.matsus.2024.300
Publication date: 18th December 2023

Structural characterization of an electrocatalyst under operando conditions is a prerequisite for fully understanding its activity and stability. Surface X-ray Diffraction (SXRD) is a powerful tool to obtain such information due to its high surface sensitivity and the possibility to probe the electrode-electrolyte interface in a noninvasive manner, especially when employing high energy photons. Furthermore, SXRD can easily be combined with other, e.g. spectroscopy or microscopy, techniques to aqcuire complementary information within the same experiment. Here, I will show the application of SXRD for atomic scale structural characterization of single crystal model electrocatalysts. First, I present the evolution of a Pt(111) surface under oxidizing (oxygen evolution as well as oxygen reduction reaction) conditions in a combined rotating disk electrode (RDE) SXRD experiment [1]. These experiments resolve the complete oxidation of the surface layer near the onset of the oxygen evolution reaction and the surface stability during oxygen reduction. Similar studies were performed under hydrogen evolution conditions in strong alkaline media to study the electrode restructuring due to cathodic corrosion under operando conditions. I further show how coupling SXRD with other techniques such as infrared reflection absorption spectroscopy (IRRAS) or surface optical reflectance (SOR) provides insights in the oxidation of CO on Pt(111) [2] and the reconstruction of Au(111) [3], respectively. Finally, I will discuss the applicability of SXRD for studying model electrocatalysts beyond bulk single crystals. This is exemplified by the characterization of epitaxial Cu thin films under CO2 electroreduction conditions.

References:

[1] L. Jacobse, R. Schuster, J. Pfrommer, X. Deng, S. Dolling, T. Weber, O. Gutowski, A.-C. Dippel, O. Brummel, H. Over, J. Libuda, V. Vonk, A. Stierle, Y. Lykhach, H. Over, J. Libuda, V. Vonk, and A. Stierle, Rev. Sci. Instrum. 93, 065111 (2022).

[2] O. Brummel, L. Jacobse, A. Simanenko, X. Deng, S. Geile, O. Gutowski, V. Vonk, Y. Lykhach, A. Stierle, and J. Libuda, J. Phys. Chem. Lett. 14, 8820 (2023).

[3] W. Linpé, L. Rämisch, G. Abbondanza, A. Larsson, S. Pfaff, L. Jacobse, J. Zetterberg, L. Merte, A. Stierle, Z. Hegedues, U. Lienert, E. Lundgren, and G.S. Harlow, J. Electrochem. Soc. 168, 096511 (2021).

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