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Graphene-Capped Liquid Thin Films for Electrochemical Operando X-ray Spectroscopy and Scanning Electron Microscopy

Title data

Falling, Lorenz J. ; Mom, Rik V. ; Sandoval-Diaz, Luis E. ; Nakhaie, Siamak ; Stotz, Eugen ; Ivanov, Danail ; Hävecker, Michael ; Lunkenbein, Thomas ; Knop-Gericke, Axel ; Schlögl, Robert ; Velasco-Vélez, Juan-Jesús:
Graphene-Capped Liquid Thin Films for Electrochemical Operando X-ray Spectroscopy and Scanning Electron Microscopy.
In: ACS Applied Materials & Interfaces. Vol. 12 (2020) Issue 33 . - pp. 37680-37692.
ISSN 1944-8252
DOI: https://doi.org/10.1021/acsami.0c08379

Abstract in another language

Electrochemistry is a promising building block for the global transition to a sustainable energy market. Particularly the electroreduction of CO2 and the electrolysis of water might be strategic elements for chemical energy conversion. The reactions of interest are inner-sphere reactions, which occur on the surface of the electrode, and the biased interface between the electrode surface and the electrolyte is of central importance to the reactivity of an electrode. However, a potential-dependent observation of this buried interface is challenging, which slows the development of catalyst materials. Here we describe a sample architecture using a graphene blanket that allows surface sensitive studies of biased electrochemical interfaces. At the examples of near ambient pressure X-ray photoelectron spectroscopy (NAP-XPS) and environmental scanning electron microscopy (ESEM), we show that the combination of a graphene blanket and a permeable membrane leads to the formation of a liquid thin film between them. This liquid thin film is stable against a water partial pressure below 1 mbar. These properties of the sample assembly extend the study of solid-liquid interfaces to highly surface sensitive techniques, such as electron spectroscopy/microscopy. In fact, photoelectrons with an effective attenuation length of only 10 angstrom can be detected, which is close to the absolute minimum possible in aqueous solutions. The in-situ cells and the sample preparation necessary to employ our method are comparatively simple. Transferring this approach to other surface sensitive measurement techniques should therefore be straightforward. We see our approach as a starting point for more studies on electrochemical interfaces and surface processes under applied potential. Such studies would be of high value for the rational design of electrocatalysts.

Further data

Item Type: Article in a journal
Refereed: Yes
Additional notes: WOS:000563074900088
Institutions of the University: Faculties > Faculty of Biology, Chemistry and Earth Sciences > Department of Chemistry
Faculties
Faculties > Faculty of Biology, Chemistry and Earth Sciences
Faculties > Faculty of Biology, Chemistry and Earth Sciences > Department of Chemistry > Chair Operando-Analytics of Electrochemical Energy Storage > Chair Operando-Analytics of Electrochemical Energy Storage - Univ.-Prof. Dr. Thomas Lunkenbein
Faculties > Faculty of Biology, Chemistry and Earth Sciences > Department of Chemistry > Chair Operando-Analytics of Electrochemical Energy Storage
Result of work at the UBT: No
DDC Subjects: 500 Science > 540 Chemistry
Date Deposited: 13 Jun 2025 06:57
Last Modified: 04 Jul 2025 11:32
URI: https://eref.uni-bayreuth.de/id/eprint/93698