Development of a cell for in-situ/operando Mössbauer spectroscopy studies of Catalysts: Application to the characterization of iron nanoparticles used in Fischer–Tropsch reaction

In this paper, we report the design of a stainless-steel cell with polyimide film windows for carrying out in situ Mossbauer spectroscopy studies with a horizontal x-ray beam. It allows recording spectra at pressures up to 0.2–0.3 MPa and temperatures up to 500 °C under a gas flow rate of up to 100...

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Bibliographic Details
Published in:Review of scientific instruments 2023-09, Vol.94 (9)
Main Authors: Huve, J., Bourgain, F., Farrusseng, D., Millet, J. M. M.
Format: Article
Language:English
Subjects:
Catalysis
Catalysts
Chemical Sciences
Cooling rate
Environment and Society
Environmental Sciences
Gas flow
Heating
Mossbauer spectroscopy
Nanoparticles
Scientific apparatus & instruments
Silicalite
Spectroscopic analysis
Stainless steels
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Summary:In this paper, we report the design of a stainless-steel cell with polyimide film windows for carrying out in situ Mossbauer spectroscopy studies with a horizontal x-ray beam. It allows recording spectra at pressures up to 0.2–0.3 MPa and temperatures up to 500 °C under a gas flow rate of up to 100 ml min−1. The catalyst is either directly deposited on the heating element or pressed into the form of a pellet for larger quantities. A wide range of heating or cooling rates can be used, and a very accurate sample temperature can be monitored for several days. An example of application to the study of a catalyst based on iron nanoparticles entrapped in silicalite-1 used for the Fischer–Tropsch reaction is presented to illustrate the use of the cell.
ISSN:0034-6748
1089-7623
DOI:10.1063/5.0160107