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

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Sandoval Diaz,  Luis
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Nakhaie,  Siamak
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Ivanov,  Danail
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Hävecker,  Michael
Research Department Schlögl, Max Planck Institute for Chemical Energy Conversion, Max Planck Society;
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Lunkenbein,  Thomas
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Knop-Gericke,  Axel
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;
Research Department Schlögl, Max Planck Institute for Chemical Energy Conversion, Max Planck Society;

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Schlögl,  Robert
Research Department Schlögl, Max Planck Institute for Chemical Energy Conversion, Max Planck Society;
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Citation

Falling, L. J., Mom, R. V., Sandoval Diaz, L., Nakhaie, S., Stotz, E., Ivanov, D., et al. (2020). Graphene-Capped Liquid Thin Films for Electrochemical Operando X-ray Spectroscopy and Scanning Electron Microscopy. ACS Applied Materials and Interfaces, 12(33), 37680-37692. doi:10.1021/acsami.0c08379.


Cite as: http://hdl.handle.net/21.11116/0000-0007-A6E8-8
Abstract
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.