Versatile and high temperature spectroscopic cell for operando fluorescence and transmission x-ray absorption spectroscopic studies of heterogeneous catalysts

A modular high-temperature cell consisting of a plug-flow microreactor with a fixed catalyst bed and long heating zone has been established for operando x-ray absorption/fluorescence spectroscopic and diffraction studies. The functionality of the cell is demonstrated for two important areas: emissio...

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Bibliographic Details
Published in:Review of scientific instruments 2021-02, Vol.92 (2), p.023106-023106
Main Authors: Eggart, Daniel, Zimina, Anna, Cavusoglu, Gülperi, Casapu, Maria, Doronkin, Dmitry E., Lomachenko, Kirill A., Grunwaldt, Jan-Dierk
Format: Article
Language:English
Subjects:
Alkenes
Aluminum oxide
Catalysts
Control systems design
Cooling rate
Cooling systems
Direct conversion
Emissions control
Fluorescence
Heating
High temperature
Iron
Liquid cooling
Mass spectrometry
Plug flow
Raman spectroscopy
Scientific apparatus & instruments
Silicon dioxide
Spectroscopic analysis
Synchrotrons
X ray absorption
X-ray spectroscopy
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Summary:A modular high-temperature cell consisting of a plug-flow microreactor with a fixed catalyst bed and long heating zone has been established for operando x-ray absorption/fluorescence spectroscopic and diffraction studies. The functionality of the cell is demonstrated for two important areas: emission control using 2 wt. % Pd/Al2O3 acting as a three-way catalyst and direct conversion of methane to olefins and aromatics on a 0.5% Fe/SiO2 catalyst. The performance has been determined by online infrared spectroscopy and mass spectrometry, respectively. In addition, the cell can be combined with optical spectroscopy, such as Raman spectroscopy. The catalyst, present as powdered/sieved samples, can be measured under reaction conditions at temperatures of up to 1050 °C. Another key aspect is a long isothermal heating zone with a small temperature gradient (
ISSN:0034-6748
1089-7623
DOI:10.1063/5.0038428