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Direct Detection of Al–O–Al Structure in Aluminosilicate Specimens: A Use of Homo-Nuclear DQMAS NMR

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Abstract

A general strategy of Al–O–Al structure in various aluminosilicate was evaluated by combining triple-quantum magic angle spinning (3QMAS) and double-quantum homo-nuclear correlation under magic angle spinning (DQMAS) solid-state nuclear magnetic resonance (NMR) measurements with the aid of high magnetic field NMR (800 MHz for 1H Larmor frequency). The results show that in many cases the direct detection of Al–O–Al sites in aluminosilicate crystals and glasses is possible; hence the extent of aluminum avoidance can be directly elucidated. Specifically, experimental evidence of Al–O–Al linkages in several aluminosilicate materials with Si/Al >1 was straightforwardly confirmed; and the existence of Al–O–Al is considered to have little correlation with the Si/Al ratio, but it may be strongly related to the cation and local structural arrangement. In addition, the presence of tri-clusters of (Si, Al)O4-tetrahedra in aluminosilicate framework was proposed, which was thought to act as nuclei for formation and incorporation of cations to achieve charge neutrality.

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Acknowledgments

We gratefully acknowledge the financial support provided by the Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Ministry; and the New Energy and Industrial Technology Development Organization (NEDO) of Japan.

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Authors and Affiliations

  1. School of Chemical and Environmental Engineering, China University of Mining and Technology (Beijing), D11 Xueyuan Road, Haidian District, Beijing, 100083, People’s Republic of China

    Xiongchao Lin & Yonggang Wang

  2. Institute for Materials Chemistry and Engineering, Kyushu University, Fukuoka, 816-8580, Japan

    Keiko Ideta, Jin Miyawaki, Seongho Yoon & Isao Mochida

  3. JEOL Resonance Inc., 3-1-2 Musashino, Akishima, Tokyo, 196-8558, Japan

    Yusuke Nishiyama

Authors
  1. Xiongchao Lin
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  2. Keiko Ideta
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  3. Jin Miyawaki
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  4. Yonggang Wang
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  5. Yusuke Nishiyama
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  6. Seongho Yoon
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  7. Isao Mochida
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Correspondence to Xiongchao Lin or Yusuke Nishiyama.

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Lin, X., Ideta, K., Miyawaki, J. et al. Direct Detection of Al–O–Al Structure in Aluminosilicate Specimens: A Use of Homo-Nuclear DQMAS NMR. Appl Magn Reson 45, 111–123 (2014). https://doi.org/10.1007/s00723-013-0504-4

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  • DOI: https://doi.org/10.1007/s00723-013-0504-4

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