Visualizing defects and pore connectivity within metal-organic frameworks by X-ray transmission tomography

Rafael Mayorga-González, Miguel Rivera-Torrente, Nikolaos Nikolopoulos, Koen W. Bossers, Roozbeh Valadian, Joaquín Yus, Beatriz Seoane, Bert M. Weckhuysen*, Florian Meirer

*Corresponding author for this work

    Research output: Contribution to journalArticleAcademicpeer-review

    Abstract

    Metal-Organic Frameworks (MOFs) have the potential to change the landscape of molecular separations in chemical processes owing to their ability of selectively binding molecules. Their molecular sorting properties generally rely on the micro- and meso-pore structure, as well as on the presence of coordinatively unsaturated sites that interact with the different chemical species present in the feed. In this work, we show a first-of-its-kind tomographic imaging of the crystal morphology of a metal-organic framework by means of transmission X-ray microscopy (TXM), including a detailed data reconstruction and processing approach. Corroboration with Focused Ion Beam-Scanning Electron Microscopy (FIB-SEM) images shows the potential of this strategy for further (non-destructively) assessing the inner architecture of MOF crystals. By doing this, we have unraveled the presence of large voids in the internal structure of a MIL-47(V) crystal, which are typically thought of as rather homogeneous lattices. This challenges the established opinion that hydrothermal syntheses yield relatively defect-free material and sheds further light on the internal morphology of crystals.

    Original languageEnglish
    Article number8458
    Pages (from-to)8458-8467
    Number of pages10
    JournalChemical Science
    Volume12
    Issue number24
    DOIs
    Publication statusPublished - 28 Jun 2021

    Bibliographical note

    Funding Information:
    This work was supported by the Netherlands Center for Multiscale Catalytic Energy Conversion (MCEC), an NWO Gravitation programme funded by the Ministry of Education, Culture and Science of the government of the Netherlands. This project has received funding from the European Union?s Horizon 2020 research and innovation programme under the Marie Sk?odowska-Curie grant agreement No 801359. J. Ag?ndez (Institute for Catalysis and Petrochemistry, ICP-CSIC) and S. P?rez (ICP-CSIC) are gratefully acknowledged for their help with Hg-porosimetry experiments. We thank I. K. Van Ravenhorst (Utrecht University, UU) and S. Kalirai for their assistance during TXM data collection. Y. Liu and J. Nelson-Weker also assisted during TXM data collection at beamline 6-2c of the Stanford Synchrotron Radiation Lightsource (SSRL). SSRL is a directorate of SLAC National Accelerator Laboratory and an Office of Science User Facility operated for the U.S. Department of Energy Office of Science by Stanford University.

    Funding Information:
    This work was supported by the Netherlands Center for Multiscale Catalytic Energy Conversion (MCEC), an NWO Gravitation programme funded by the Ministry of Education, Culture and Science of the government of the Netherlands. This project has received funding from the European Union’s Horizon 2020 research and innovation programme under the Marie Skłodowska-Curie grant agreement No 801359. J. Agúndez (Institute for Catalysis and Petrochemistry, ICP-CSIC) and S. Pérez (ICP-CSIC) are gratefully acknowledged for their help with Hg-porosimetry experiments. We thank I. K. Van Ravenhorst (Utrecht University, UU) and S. Kalirai for their assistance during TXM data collection. Y. Liu and J. Nelson-Weker also assisted during TXM data collection at beamline 6-2c of the Stanford Synchrotron Radiation Light-source (SSRL). SSRL is a directorate of SLAC National Accelerator Laboratory and an Office of Science User Facility operated for the U.S. Department of Energy Office of Science by Stanford University.

    Publisher Copyright:
    © The Royal Society of Chemistry 2021.

    Funding

    This work was supported by the Netherlands Center for Multiscale Catalytic Energy Conversion (MCEC), an NWO Gravitation programme funded by the Ministry of Education, Culture and Science of the government of the Netherlands. This project has received funding from the European Union?s Horizon 2020 research and innovation programme under the Marie Sk?odowska-Curie grant agreement No 801359. J. Ag?ndez (Institute for Catalysis and Petrochemistry, ICP-CSIC) and S. P?rez (ICP-CSIC) are gratefully acknowledged for their help with Hg-porosimetry experiments. We thank I. K. Van Ravenhorst (Utrecht University, UU) and S. Kalirai for their assistance during TXM data collection. Y. Liu and J. Nelson-Weker also assisted during TXM data collection at beamline 6-2c of the Stanford Synchrotron Radiation Lightsource (SSRL). SSRL is a directorate of SLAC National Accelerator Laboratory and an Office of Science User Facility operated for the U.S. Department of Energy Office of Science by Stanford University. This work was supported by the Netherlands Center for Multiscale Catalytic Energy Conversion (MCEC), an NWO Gravitation programme funded by the Ministry of Education, Culture and Science of the government of the Netherlands. This project has received funding from the European Union’s Horizon 2020 research and innovation programme under the Marie Skłodowska-Curie grant agreement No 801359. J. Agúndez (Institute for Catalysis and Petrochemistry, ICP-CSIC) and S. Pérez (ICP-CSIC) are gratefully acknowledged for their help with Hg-porosimetry experiments. We thank I. K. Van Ravenhorst (Utrecht University, UU) and S. Kalirai for their assistance during TXM data collection. Y. Liu and J. Nelson-Weker also assisted during TXM data collection at beamline 6-2c of the Stanford Synchrotron Radiation Light-source (SSRL). SSRL is a directorate of SLAC National Accelerator Laboratory and an Office of Science User Facility operated for the U.S. Department of Energy Office of Science by Stanford University.

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