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Atmospheric pressure X-ray photoelectron spectroscopy apparatus: Bridging the pressure gap

MPS-Authors
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Velasco Vélez,  Juan
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;
MPI for Chemical Energy Conversion;

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Pfeifer,  Verena
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Hävecker,  Michael
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;
Department of Heterogeneous Reactions, Max Planck Institute for Chemical Energy Conversion;

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Algara-Siller,  Gerardo
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Stotz,  Eugen
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Teschner,  Detre
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Kube,  Pierre
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Schlögl,  Robert
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Knop-Gericke,  Axel
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Fulltext (public)

RSI_AtP-XPS-1.pdf
(Any fulltext), 2MB

Supplementary Material (public)

RSI_AtP-XPS-1.pdf
(Supplementary material), 2MB

Citation

Velasco Vélez, J., Pfeifer, V., Hävecker, M., Wang, R., Centeno, A., Zurutuza, A., et al. (2016). Atmospheric pressure X-ray photoelectron spectroscopy apparatus: Bridging the pressure gap. Review of Scientific Instruments, 87(5): 053121. doi:10.1063/1.4951724.


Cite as: http://hdl.handle.net/11858/00-001M-0000-002A-6B7F-3
Abstract
One of the main goals in catalysis is the characterization of solid/gas interfaces in a reaction environment. The electronic structure and chemical composition of surfaces become heavily influenced by the surrounding environment. However, the lack of surface sensitive techniques that are able to monitor these modifications under high pressure conditions hinders the understanding of such processes. This limitation is known throughout the community as the “pressure gap”. We have developed a novel experimental setup that provides chemical information on a molecular level under atmospheric pressure and in presence of reactive gases and at elevated temperatures. This approach is based on separating the vacuum environment from the high-pressure environment by a silicon nitride grid–that contains an array of micrometer-sized holes–coated with a bilayer of graphene. Using this configuration, we have investigated the local electronic structure of catalysts by means of photoelectron spectroscopy, and in presence of gases at 1 atmosphere. The reaction products were monitored on-line by mass spectrometry and gas chromatography. The successful operation of this setup was demonstrated with three different examples: the oxidation/reduction reaction of iridium (noble metal) and copper (transition metal) nanoparticles and with the hydrogenation of propyne on Pd black catalyst (powder).