Redistribution of Ru in Fe2O3–Ru Nanocatalysts through an Oxidative Pretreatment Improves Reverse Water–Gas Shift Activity

Alexandre C. Foucher; Kai Shen; Robert J. Macfarlane; John M. Vohs; Frances M. Ross

doi:10.1021/acsanm.5c02330

Redistribution of Ru in Fe₂O₃–Ru Nanocatalysts through an Oxidative Pretreatment Improves Reverse Water–Gas Shift Activity

Alexandre C. Foucher
, Kai Shen
, Robert J. Macfarlane
, John M. Vohs
, Frances M. Ross

Research output: Contribution to journal › Article › peer-review

1 Scopus citations

Abstract

We have synthesized Fe–Ru nanoparticles via a solvothermal method to create catalysts for the reverse water–gas shift reaction and demonstrated the impact of reductive and oxidative pretreatments on both catalytic performance and structure. Catalytic testing showed improved activity after exposure to O₂at 600 °C. In contrast, the activity became lower if then exposed to H₂at 600 °C. Environmental scanning transmission electron microscopy and scanning electron microscopy showed that exposure to O₂at 600 °C changes the morphology and completely oxidizes Fe into Fe₂O₃. Exposure to H₂at elevated temperature caused Ru coalescence at the surface of the nanoparticle, forming clusters which decreased the optimization of Ru. Reoxidation of the particles exposed to H₂, however, caused a redistribution of Ru that appears beneficial in maximizing Ru exposure and synergy with Fe oxide, with no major changes in the morphology and oxide structure. Our diagnostics demonstrate the complex and reversible rearrangements possible in these multicomponent particles and the benefits of oxidative pretreatment to enhance or regenerate Fe–Ru catalysts in other important catalytic reactions such as Fischer–Tropsch synthesis.

Original language	English
Pages (from-to)	15131-15139
Number of pages	9
Journal	ACS Applied Nano Materials
Volume	8
Issue number	30
DOIs	https://doi.org/10.1021/acsanm.5c02330
State	Published - Aug 1 2025
Externally published	Yes

Funding

This work was funded in part by Semiconductor Research Corporation (SRC) under contract number 2021-NM-3027. This work was supported by the Office of Naval Research (ONR) MURI through Grant No. N00014-17-1-2661. This project was carried out in part through the use of MIT.nano’s facilities. This work was also supported as part of the Integrated Mesoscale Architectures for Sustainable Catalysis (IMASC), an Energy Frontier Research Center funded by the U.S. Department of Energy, Office of Science, Basic Energy Sciences under Award #DE-SC0012573. This work was also supported by the National Science Foundation Grant No. DMREF-2323701.

Keywords

Fe−Ru nanoparticles
heterogeneous catalysis
in situtransmission electron microscopy
optimization of catalytic properties
reverse water−gas shift

Access to Document

10.1021/acsanm.5c02330

Cite this

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title = "Redistribution of Ru in Fe2O3–Ru Nanocatalysts through an Oxidative Pretreatment Improves Reverse Water–Gas Shift Activity",

abstract = "We have synthesized Fe–Ru nanoparticles via a solvothermal method to create catalysts for the reverse water–gas shift reaction and demonstrated the impact of reductive and oxidative pretreatments on both catalytic performance and structure. Catalytic testing showed improved activity after exposure to O2at 600 °C. In contrast, the activity became lower if then exposed to H2at 600 °C. Environmental scanning transmission electron microscopy and scanning electron microscopy showed that exposure to O2at 600 °C changes the morphology and completely oxidizes Fe into Fe2O3. Exposure to H2at elevated temperature caused Ru coalescence at the surface of the nanoparticle, forming clusters which decreased the optimization of Ru. Reoxidation of the particles exposed to H2, however, caused a redistribution of Ru that appears beneficial in maximizing Ru exposure and synergy with Fe oxide, with no major changes in the morphology and oxide structure. Our diagnostics demonstrate the complex and reversible rearrangements possible in these multicomponent particles and the benefits of oxidative pretreatment to enhance or regenerate Fe–Ru catalysts in other important catalytic reactions such as Fischer–Tropsch synthesis.",

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AU - Shen, Kai

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AU - Vohs, John M.

AU - Ross, Frances M.

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N2 - We have synthesized Fe–Ru nanoparticles via a solvothermal method to create catalysts for the reverse water–gas shift reaction and demonstrated the impact of reductive and oxidative pretreatments on both catalytic performance and structure. Catalytic testing showed improved activity after exposure to O2at 600 °C. In contrast, the activity became lower if then exposed to H2at 600 °C. Environmental scanning transmission electron microscopy and scanning electron microscopy showed that exposure to O2at 600 °C changes the morphology and completely oxidizes Fe into Fe2O3. Exposure to H2at elevated temperature caused Ru coalescence at the surface of the nanoparticle, forming clusters which decreased the optimization of Ru. Reoxidation of the particles exposed to H2, however, caused a redistribution of Ru that appears beneficial in maximizing Ru exposure and synergy with Fe oxide, with no major changes in the morphology and oxide structure. Our diagnostics demonstrate the complex and reversible rearrangements possible in these multicomponent particles and the benefits of oxidative pretreatment to enhance or regenerate Fe–Ru catalysts in other important catalytic reactions such as Fischer–Tropsch synthesis.

AB - We have synthesized Fe–Ru nanoparticles via a solvothermal method to create catalysts for the reverse water–gas shift reaction and demonstrated the impact of reductive and oxidative pretreatments on both catalytic performance and structure. Catalytic testing showed improved activity after exposure to O2at 600 °C. In contrast, the activity became lower if then exposed to H2at 600 °C. Environmental scanning transmission electron microscopy and scanning electron microscopy showed that exposure to O2at 600 °C changes the morphology and completely oxidizes Fe into Fe2O3. Exposure to H2at elevated temperature caused Ru coalescence at the surface of the nanoparticle, forming clusters which decreased the optimization of Ru. Reoxidation of the particles exposed to H2, however, caused a redistribution of Ru that appears beneficial in maximizing Ru exposure and synergy with Fe oxide, with no major changes in the morphology and oxide structure. Our diagnostics demonstrate the complex and reversible rearrangements possible in these multicomponent particles and the benefits of oxidative pretreatment to enhance or regenerate Fe–Ru catalysts in other important catalytic reactions such as Fischer–Tropsch synthesis.

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