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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]
Copyright of JAAS (Journal of Analytical Atomic Spectrometry) is the property of Royal Society of Chemistry and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
Database: Engineering Source
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Header DbId: egs
DbLabel: Engineering Source
An: 193065231
AccessLevel: 6
PubType: Academic Journal
PubTypeId: academicJournal
PreciseRelevancyScore: 0
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  Data: <searchLink fieldCode="AR" term="%22Praetz%2C+Sebastian%22">Praetz, Sebastian</searchLink><relatesTo>1</relatesTo> (AUTHOR)<i> sebastian.praetz@tu-berlin.de</i><br /><searchLink fieldCode="AR" term="%22Dal+Molin%2C+Emiliano%22">Dal Molin, Emiliano</searchLink><relatesTo>2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Kober%2C+Delf%22">Kober, Delf</searchLink><relatesTo>2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Tesic%2C+Marko%22">Tesic, Marko</searchLink><relatesTo>1</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Schlesiger%2C+Christopher%22">Schlesiger, Christopher</searchLink><relatesTo>1</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Kraus%2C+Peter%22">Kraus, Peter</searchLink><relatesTo>3</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Müller%2C+Julian+T%2E%22">Müller, Julian T.</searchLink><relatesTo>2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Aswin%2C+Jyothilakshmi+Ravi%22">Aswin, Jyothilakshmi Ravi</searchLink><relatesTo>4</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Grötzsch%2C+Daniel%22">Grötzsch, Daniel</searchLink><relatesTo>1</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Bekheet%2C+Maged+F%2E%22">Bekheet, Maged F.</searchLink><relatesTo>2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Gili%2C+Albert%22">Gili, Albert</searchLink><relatesTo>5</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Gurlo%2C+Aleksander%22">Gurlo, Aleksander</searchLink><relatesTo>2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Kanngießer%2C+Birgit%22">Kanngießer, Birgit</searchLink><relatesTo>1</relatesTo> (AUTHOR)
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  Data: <searchLink fieldCode="DE" term="%22X-ray+absorption+spectra%22">X-ray absorption spectra</searchLink><br /><searchLink fieldCode="DE" term="%22Fixed+bed+reactors%22">Fixed bed reactors</searchLink><br /><searchLink fieldCode="DE" term="%22Catalysts%22">Catalysts</searchLink><br /><searchLink fieldCode="DE" term="%22Heterogeneous+catalysis%22">Heterogeneous catalysis</searchLink><br /><searchLink fieldCode="DE" term="%22Carbon+dioxide%22">Carbon dioxide</searchLink><br /><searchLink fieldCode="DE" term="%22Nanoparticles%22">Nanoparticles</searchLink><br /><searchLink fieldCode="DE" term="%22X-ray+spectrometers%22">X-ray spectrometers</searchLink><br /><searchLink fieldCode="DE" term="%22Time-resolved+spectroscopy%22">Time-resolved spectroscopy</searchLink>
– Name: Abstract
  Label: Abstract
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  Data: 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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  Data: <i>Copyright of JAAS (Journal of Analytical Atomic Spectrometry) is the property of Royal Society of Chemistry and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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      – Type: doi
        Value: 10.1039/d6ja00027d
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      – Code: eng
        Text: English
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        PageCount: 4
        StartPage: 1208
    Subjects:
      – SubjectFull: X-ray absorption spectra
        Type: general
      – SubjectFull: Fixed bed reactors
        Type: general
      – SubjectFull: Catalysts
        Type: general
      – SubjectFull: Heterogeneous catalysis
        Type: general
      – SubjectFull: Carbon dioxide
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      – SubjectFull: Nanoparticles
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      – SubjectFull: X-ray spectrometers
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      – SubjectFull: Time-resolved spectroscopy
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              M: 04
              Text: Apr2026
              Type: published
              Y: 2026
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