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Operando laboratory XAS of Ni nanoparticles in CO2 methanation using a plug-flow fixed-bed cell with von Hámos spectrometer.

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Title: Operando laboratory XAS of Ni nanoparticles in CO2 methanation using a plug-flow fixed-bed cell with von Hámos spectrometer.
Authors: Praetz, Sebastian1 (AUTHOR) sebastian.praetz@tu-berlin.de, Dal Molin, Emiliano2 (AUTHOR), Kober, Delf2 (AUTHOR), Tesic, Marko1 (AUTHOR), Schlesiger, Christopher1 (AUTHOR), Kraus, Peter3 (AUTHOR), Müller, Julian T.2 (AUTHOR), Aswin, Jyothilakshmi Ravi4 (AUTHOR), Grötzsch, Daniel1 (AUTHOR), Bekheet, Maged F.2 (AUTHOR), Gili, Albert5 (AUTHOR), Gurlo, Aleksander2 (AUTHOR), Kanngießer, Birgit1 (AUTHOR)
Source: JAAS (Journal of Analytical Atomic Spectrometry). Apr2026, Vol. 41 Issue 4, p1208-1211. 4p.
Subjects: X-ray absorption spectra, Fixed bed reactors, Catalysts, Heterogeneous catalysis, Carbon dioxide, Nanoparticles, X-ray spectrometers, Time-resolved spectroscopy
Abstract: A plug-flow fixed-bed cell for operando laboratory X-ray absorption spectroscopy (XAS) using a von Hámos spectrometer is presented for heterogeneous catalysis studies. The cell operates up to 1000 °C and 10 bar with controlled gas atmospheres provided by three mass flow controllers and rapid infrared heating. The performance of the setup is demonstrated across a broad usable energy range of the spectrometer, and as a proof of principle, operando Ni K-edge XAS was used to monitor the activation of a 20 wt% NiO/COK-12 catalyst under CO2 methanation conditions (CO2 : H2 = 1 : 4, 350 °C). Time-resolved spectra acquired on a 5 min timescale reveal the reduction of NiO nanoparticles to metallic Ni during activation, directly correlating with increasing catalytic activity quantified by online gas chromatography. This setup enables minute-scale, time-resolved structural analysis of working catalysts under industrially relevant conditions, providing a practical laboratory-based alternative complementary to synchrotron studies. [ABSTRACT FROM AUTHOR]
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Database: Engineering Source
Description
Abstract:A plug-flow fixed-bed cell for operando laboratory X-ray absorption spectroscopy (XAS) using a von Hámos spectrometer is presented for heterogeneous catalysis studies. The cell operates up to 1000 °C and 10 bar with controlled gas atmospheres provided by three mass flow controllers and rapid infrared heating. The performance of the setup is demonstrated across a broad usable energy range of the spectrometer, and as a proof of principle, operando Ni K-edge XAS was used to monitor the activation of a 20 wt% NiO/COK-12 catalyst under CO2 methanation conditions (CO2 : H2 = 1 : 4, 350 °C). Time-resolved spectra acquired on a 5 min timescale reveal the reduction of NiO nanoparticles to metallic Ni during activation, directly correlating with increasing catalytic activity quantified by online gas chromatography. This setup enables minute-scale, time-resolved structural analysis of working catalysts under industrially relevant conditions, providing a practical laboratory-based alternative complementary to synchrotron studies. [ABSTRACT FROM AUTHOR]
ISSN:02679477
DOI:10.1039/d6ja00027d