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Synthesis of Mixed-Metal MIL-68 under Mild Conditions by Controlling Nucleation Using a Microfluidic System

  • Saki Yamada
    Saki Yamada
    Department of Chemistry, School of Science, Kwansei Gakuin University, 2-1 Gakuen, Sanda, Hyogo 669-1337, Japan
    More by Saki Yamada
  • Ayumi Hirano
    Ayumi Hirano
    Department of Chemistry, School of Science, Kwansei Gakuin University, 2-1 Gakuen, Sanda, Hyogo 669-1337, Japan
    More by Ayumi Hirano
  • Yoko Tanaka
    Yoko Tanaka
    Department of Chemistry, School of Science, Kwansei Gakuin University, 2-1 Gakuen, Sanda, Hyogo 669-1337, Japan
    More by Yoko Tanaka
  • Ryohei Akiyoshi
    Ryohei Akiyoshi
    Department of Chemistry, School of Science, Kwansei Gakuin University, 2-1 Gakuen, Sanda, Hyogo 669-1337, Japan
  • Hirofumi Yoshikawa
    Hirofumi Yoshikawa
    Program of Material Science, School of Technology, Kwansei Gakuin University, Sanda, Hyogo 669-1337, Japan
  • , and 
  • Daisuke Tanaka*
    Daisuke Tanaka
    Department of Chemistry, School of Science, Kwansei Gakuin University, 2-1 Gakuen, Sanda, Hyogo 669-1337, Japan
    *Email: [email protected]
Cite this: Cryst. Growth Des. 2022, 22, 7, 4139–4145
Publication Date (Web):June 17, 2022
https://doi.org/10.1021/acs.cgd.2c00140
Copyright © 2022 American Chemical Society

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    Abstract

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    Metal–organic frameworks that contain trivalent metal ions as nodes (M3+–MOFs) exhibit potential for various applications due to their exceptional thermal and chemical stability; however, M3+–MOF synthesis requires extreme reaction conditions such as high temperatures, long reaction times, and hydrogen fluoride (HF) addition. Here, we rapidly synthesized MIL-68 containing trivalent metal ions without any HF addition by controlling nucleation using microfluidic synthesis and metal mixing. Al3+ addition during the initial reaction between Fe3+ and the ligand yielded 1D chain-based secondary building units, consequently forming MIL-68. Compared to the products obtained using bulk and microwave-assisted syntheses, the product obtained via microfluidic synthesis exhibited high crystallinity. Thus, the combination of microfluidic systems and metal mixing is a novel approach in synthesizing industrially applicable M3+–MOFs.

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    The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.cgd.2c00140.

    • Experimental details, including PXRD patterns, SEM images, and N2 sorption isotherms (PDF)

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