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

Falling, L., Mom, R., Sandoral-Diaz, L.-E., 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.

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 Creators:
Falling, Lorenz1, Author           
Mom, Rik1, Author           
Sandoral-Diaz, Luis-Ernesto1, Author           
Nakhaie, Siamak1, Author           
Stotz, Eugen1, Author           
Ivanov, Danail1, Author           
Hävecker, Michael1, 2, Author           
Lunkenbein, Thomas1, Author           
Knop-Gericke, Axel1, 2, Author           
Schlögl, Robert1, 2, Author           
Velasco Vélez, Juan1, 2, Author           
Affiliations:
1Inorganic Chemistry, Fritz Haber Institute, Max Planck Society, ou_24023              
2Department of Heterogeneous Reactions, Max-Planck-Institut für Chemische Energiekonversion, Stiftstr. 34-36, 45470 Mülheim, Germany, ou_persistent22              

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 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 Å 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.

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Language(s): eng - English
 Dates: 2020-05-072020-07-232020-07-232020-08-19
 Publication Status: Published in print
 Pages: 13
 Publishing info: -
 Table of Contents: -
 Rev. Type: Peer
 Identifiers: DOI: 10.1021/acsami.0c08379
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Title: ACS Applied Materials and Interfaces
  Other : ACS Applied Materials & Interfaces
  Abbreviation : ACS Appl. Mater. Interfaces
Source Genre: Journal
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Publ. Info: Washington, DC : American Chemical Society
Pages: 13 Volume / Issue: 12 (33) Sequence Number: - Start / End Page: 37680 - 37692 Identifier: ISSN: 1944-8244
CoNE: https://pure.mpg.de/cone/journals/resource/1944-8244