7 Li{ 19 F} TEDOR NMR to observe the lithium migration in heated montmorillonite

Abstract : The distribution of lithium ions in heated synthetic montmorillonites was studied by using F-19, Li-7 MAS and Li-7{F-19} TEDOR nuclear magnetic resonance technics. To get the best of NMR spectroscopy, Na-montmorillonites, free of paramagnetic centres (Fe2+, Fe3+), were synthesized in fluoride medium, in order to have substitution of some hydroxyl groups by fluorine in the octahedral layer (Na-0.35[(Al1.69Mg0.36)vi(Si3.86Al0.14)(IV)O-10(OH0.95F0.05)(2)]). After Li+ exchange, mild heat treatments (from 110 to 250 degrees C during 24 h) were applied to follow the lithium migration. Both F-19 and Li-7 MAS spectra indicate that the lithium migration operates in two steps: at 110 degrees C, 86% of the lithium ions have moved to the hexagonal site. The remaining interlayer ions move progressively to this site when the heating temperature is in the range (170-250 degrees C]. For the first time a direct fluorine-lithium distance of 2.23 angstrom was measured by Li-7{F-19} TEDOR, which uses fluorine as a highly selective and NMR-sensitive witness of atomic-scale motions inside porous media, and which agrees with the preferred hexagonal site for Li+ migration.
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https://hal-univ-bourgogne.archives-ouvertes.fr/hal-01896048
Contributeur : Pam - Université de Bourgogne <>
Soumis le : lundi 15 octobre 2018 - 17:27:21
Dernière modification le : jeudi 21 février 2019 - 10:34:07

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Philippe Bodart, L. Delmotte, S. Rigolet, J. Brendle, Régis Gougeon. 7 Li{ 19 F} TEDOR NMR to observe the lithium migration in heated montmorillonite. Applied Clay Science, Elsevier, 2018, 157, pp.204 - 211. ⟨10.1016/j.clay.2018.03.007⟩. ⟨hal-01896048⟩

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