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Selectively monitoring the operando temperature of active metal nanoparticles during catalytic reactions by X-ray absorption nanothermometry

Nature Catalysis volume 8, pages 187–195 (2025)Cite this article

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Abstract

Heat involved in catalytic reactions can influence the local temperature and performance of the active site, potentially causing catalyst degradation and runaway scenarios. Yet, broadly applicable thermometry methods to selectively probe the temperature of the catalytically active phase—where reactions take place—are generally lacking. Here we explore extended X-ray absorption fine-structure thermometry to monitor the operando temperature of active Ni nanoparticles, fully deconvoluted from their metal-oxide support. During dry reforming of methane, the reaction’s endothermicity causes Ni nanoparticles to become local heat sinks with their temperature deviating 90 °C from the reactor temperature. By thermometry at the single nanoparticle level, we chart the energy balance of nanoparticles and relate their temperature to reaction kinetics. Covering the full temperature range relevant to catalysis, this broadly applicable method enables temperature monitoring of individual catalyst components separately. Applying extended X-ray absorption fine-structure thermometry to existing datasets worldwide can generate enhanced understanding on reaction-induced temperature phenomena in heterogeneous catalysis.

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Fig. 1: Schematic illustration of the concept of this study.
Fig. 2: Establishing a relation between EXAFS and temperature.
Fig. 3: Operando EXAFS thermometry to extract the Ni nanoparticle temperature during the DRM and RWGS reactions.
Fig. 4: Rationalizing the oscillatory temperature and energy balance in Ni nanoparticles during DRM.

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Data availability

All data are available from the corresponding authors upon reasonable request.

Code availability

Code to perform EXAFS thermometry is available via GitHub at https://github.com/matthiasfilez/EXAFS-thermometry.

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Acknowledgements

M.F. acknowledges the FWO for a senior postdoctoral research fellowship (1280621N). This work was supported by the Fund for Scientific Research Flanders (grant no. G0A5923N (M.B.J.R. and C.D.), 3G021220 (V.G. and C.D.), G093823N (M.F. and J.D.)) and the Special Research Fund BOF of Ghent University (grant no. GOA-01G02124 (M.F., J.D. and C.D.)). The research leading to these results is supported by the project CALIPSOplus under grant agreement 730872 from the EU Framework Programme for Research and Innovation HORIZON 2020, in supplying financing of subsistence costs for the synchrotron campaign (SOLEIL, proposal 20200555 (V.D.C., H.P. and V.G.). We acknowledge the assistance from the ROCK staff for a smooth beamtime.

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Authors and Affiliations

  1. Conformal Coating of Nanomaterials, Department of Solid State Sciences, Ghent University, Ghent, Belgium

    Matthias Filez, Jolien Dendooven & Christophe Detavernier

  2. Centre for Membrane Separations, Adsorption, Catalysis and Spectroscopy for Sustainable Solutions, KU Leuven, Leuven, Belgium

    Matthias Filez & Maarten B. J. Roeffaers

  3. Laboratory for Chemical Technology, Ghent University, Ghent, Belgium

    Valentijn De Coster, Hilde Poelman & Vladimir Galvita

  4. SOLEIL Synchrotron, L’Orme des Merisiers, Saint Aubin, France

    Valerie Briois & Anthony Beauvois

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Contributions

M.F., J.D., M.B.J.R. and C.D. conceived the research idea and project. V.D.C., H.P. and V.G. produced the samples and collected the XAS data together with V.B. and A.B. M.F., V.D.C. and A.B. preprocessed the data. M.F. developed the thermometry workflow and data analysis with the support of V.D.C. M.F. and V.G. collected the transmission electron microscopy data. M.F. analysed the transmission electron microscopy data and wrote the paper. All authors contributed to revising and optimizing the paper.

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Correspondence to Matthias Filez or Christophe Detavernier.

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Nature Catalysis thanks Ken Motokura and the other, anonymous, reviewer(s) for their contribution to the peer review of this work.

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Supplementary Figs. 1–11, Tables 1–4 and Notes 1–8.

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Filez, M., De Coster, V., Poelman, H. et al. Selectively monitoring the operando temperature of active metal nanoparticles during catalytic reactions by X-ray absorption nanothermometry. Nat Catal 8, 187–195 (2025). https://doi.org/10.1038/s41929-025-01295-9

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