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  Reaction cell for in situ soft x-ray absorption spectroscopy and resonant inelastic x-ray scattering measurements of heterogeneous catalysis up to 1 atm and 250 °C

Kristiansen, P. T., Rocha, T., Knop-Gericke, A., Guo, J. H., & Duda, L. C. (2013). Reaction cell for in situ soft x-ray absorption spectroscopy and resonant inelastic x-ray scattering measurements of heterogeneous catalysis up to 1 atm and 250 °C. Review of Scientific Instruments, 84(11): 113107. doi:10.1063/1.4829630.

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 Creators:
Kristiansen, Paw Toldbad1, 2, 3, Author           
Rocha, Tulio2, Author           
Knop-Gericke, Axel2, Author           
Guo, J. H.4, Author
Duda, L. C.1, Author
Affiliations:
1Department of Physics and Astronomy, Division of Molecular and Condensed Matter Physics, Uppsala University, Box 516, S-751 20 Uppsala, Sweden, ou_persistent22              
2Inorganic Chemistry, Fritz Haber Institute, Max Planck Society, ou_24023              
3Helmholtz-Zentrum Berlin für Materialien und Energie, Albert-Einstein-Str. 15, D-12489 Berlin, Germany, ou_persistent22              
4Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, California 94720, USA, ou_persistent22              

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Free keywords: Silver; Cell membranes;Powders;Catalysis;X-ray absorption spectroscopy;X-ray spectroscopy;Photochemical reactions;Membrane biochemistry;Sample handling;Heterogeneous catalysis
 Abstract: We present a novel in situ reaction cell for heterogeneous catalysis monitored in situ by x-ray absorption spectroscopy (XAS) and resonant inelastic x-ray scattering (RIXS). The reaction can be carried out at a total pressure up to 1 atm, a regime that has not been accessible to comparable in situ techniques and thus closes the pressure gap to many industrial standard conditions. Two alternate catalyst geometries were tested: (A) a thin film evaporated directly onto an x-ray transparent membrane with a flowing reaction gas mixture behind it or (B) a powder placed behind both the membrane and a gap of flowing reaction gas mixture. To illustrate the working principle and feasibility of our reaction cell setup we have chosen ethylene epoxidation over a silver catalyst as a test case. The evolution of incorporated oxygen species was monitored by total electron/fluorescence yield O K-XAS as well as O K-RIXS, which is a powerful method to separate contributions from inequivalent sites. We find that our method can reliably detect transient species that exist during catalytic reaction conditions that are hardly accessible using other spectroscopic methods.

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Language(s): eng - English
 Dates: 2013-09-222013-10-262013-11-192013
 Publication Status: Issued
 Pages: 12
 Publishing info: -
 Table of Contents: -
 Rev. Type: Peer
 Identifiers: DOI: 10.1063/1.4829630
 Degree: -

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Title: Review of Scientific Instruments
Source Genre: Journal
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Publ. Info: Woodbury, N.Y. [etc.] : American Institute of Physics
Pages: - Volume / Issue: 84 (11) Sequence Number: 113107 Start / End Page: - Identifier: ISSN: 0034-6748
CoNE: https://pure.mpg.de/cone/journals/resource/991042742033452