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<p>By employing a room temperature batch method, we successfully synthesized single crystals of Na<sup>+</sup> ion-exchanged, binary ion (Mn<sup>2+</sup> and Na<sup>+</sup>) exchanged, and Mn<sup>2+</sup> ion exchanged zeolite A, enabling detailed structural analysis via single-crystal synchrotron X-ray diffraction. The structures of these fully dehydrated crystals: Na<sup>+</sup> ion exchanged zeolite A (Crystal 1), 0.08&#xa0;M Na<sup>+</sup>:0.02&#xa0;M Mn<sup>2+</sup> ion exchanged zeolite A (Crystal 2), 0.05&#xa0;M Mn<sup>2+</sup>: 0.05&#xa0;M Na<sup>+</sup> ion exchanged zeolite A (Crystal 3), and Mn<sup>2+</sup> ion exchanged zeolite A (Crystal 4) were determined by single-crystal synchrotron X-ray diffraction techniques. Measurements were conducted in the cubic space group <i>Pm</i>-<InlineEquation ID="IEq1"> <InlineMediaObject> <ImageObject Color="BlackWhite" FileRef="10934_2025_1811_Article_IEq1.gif" Format="GIF" Height="16" Rendition="HTML" Resolution="72" Type="Linedraw" Width="10" /> </InlineMediaObject> <EquationSource Format="TEX">\(\bar{3}\)</EquationSource> </InlineEquation><i>m</i> at 100(1) K, with the structures refined to the final error indices R<sub>1</sub>/<i>w</i>R<sub>2</sub> of 0.0486/0.1565, 0.0600/0.1625, 0.0549/0.1443, and 0.0768/0.2077 (for F<sub>o</sub> &gt; 4σ(F<sub>o</sub>)) for crystals 1, 2, 3, and 4, respectively. No dealumination was observed in these structures. In the fully Na<sup>+</sup> ion-exchanged structure (Crystal 1), Na<sup>+</sup> ions fully occupy the 6-ring positions, which, while demonstrating complete ion occupancy, potentially limits functionality due to blocked 8-ring windows. In contrast, the 0.08&#xa0;M Na<sup>+</sup>:0.02&#xa0;M Mn<sup>2+</sup> ion-exchanged crystal (Crystal 2) showed an ideal distribution of ions, with evenly filled 6-rings and open 8-ring windows. The structural analysis emphasizes the critical role of ion distribution within zeolite A, suggesting structural implications that may inform future material design for ion exchange or separation application.</p>

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Ion distribution and structural modification in zeolite LTA via Na+ and Mn2+ ion exchange

  • 期刊论文

  • 发表日期：

    2025年5月6日

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  • Sayantika Nath,
  • Hyeon Seung Lim,
  • Hu Sik Kim,
  • Woo Taik Lim

摘要

By employing a room temperature batch method, we successfully synthesized single crystals of Na+ ion-exchanged, binary ion (Mn2+ and Na+) exchanged, and Mn2+ ion exchanged zeolite A, enabling detailed structural analysis via single-crystal synchrotron X-ray diffraction. The structures of these fully dehydrated crystals: Na+ ion exchanged zeolite A (Crystal 1), 0.08 M Na+:0.02 M Mn2+ ion exchanged zeolite A (Crystal 2), 0.05 M Mn2+: 0.05 M Na+ ion exchanged zeolite A (Crystal 3), and Mn2+ ion exchanged zeolite A (Crystal 4) were determined by single-crystal synchrotron X-ray diffraction techniques. Measurements were conducted in the cubic space group Pm- \(\bar{3}\) m at 100(1) K, with the structures refined to the final error indices R1/wR2 of 0.0486/0.1565, 0.0600/0.1625, 0.0549/0.1443, and 0.0768/0.2077 (for Fo > 4σ(Fo)) for crystals 1, 2, 3, and 4, respectively. No dealumination was observed in these structures. In the fully Na+ ion-exchanged structure (Crystal 1), Na+ ions fully occupy the 6-ring positions, which, while demonstrating complete ion occupancy, potentially limits functionality due to blocked 8-ring windows. In contrast, the 0.08 M Na+:0.02 M Mn2+ ion-exchanged crystal (Crystal 2) showed an ideal distribution of ions, with evenly filled 6-rings and open 8-ring windows. The structural analysis emphasizes the critical role of ion distribution within zeolite A, suggesting structural implications that may inform future material design for ion exchange or separation application.