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Hydrothermal synthesis, between 75 and 150°C, of High-charge, ferric nontronites

Published online by Cambridge University Press:  01 January 2024

Alain Decarreau*
Affiliation:
Université de Poitiers, UMR 6532 HydrASA CNRS/INSU, 40 Av. Recteur Pineau, F86022 Poitiers cedex, France
Sabine Petit
Affiliation:
Université de Poitiers, UMR 6532 HydrASA CNRS/INSU, 40 Av. Recteur Pineau, F86022 Poitiers cedex, France
François Martin
Affiliation:
ERT 1074 CNRS Géomatériaux, LMTG-OMP-UPS-IRD-CNRS, 14 Avenue Edouard Belin, F31400 Toulouse, France
François Farges
Affiliation:
USM 201 - UMR.CNRS 7160, Muséum National d’Histoire Naturelle, 61 rue Buffon, F75005 Paris, France
Philippe Vieillard
Affiliation:
Université de Poitiers, UMR 6532 HydrASA CNRS/INSU, 40 Av. Recteur Pineau, F86022 Poitiers cedex, France
Emmanuel Joussein
Affiliation:
Université de Limoges, UMR 6532 HydrASA CNRS/INSU, 123 Av. A. Thomas, F87060 Limoges cedex, France
*
* E-mail address of corresponding author: [email protected]
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Abstract

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High-charge nontronites were synthesized at 75, 90, 100, 110, 125, and 150°C from a silicoferrous starting gel with Si2FeNa2O6.nH2O composition. This gel was oxidized in contact with air and then hydrothermally treated, for a period of 4 weeks, under equilibrium water pressure. The synthesized nontronites were similar to each other, regardless of the synthesis temperature. Their structural formula, obtained from chemical analysis, X-ray diffraction (XRD), and Fourier transform infrared (FTIR), Mössbauer, and X-ray absorption fine structure spectroscopies is: (Si3.25Fe0.753+)Fe23+O10(OH)2Na0.75$\left( {{\rm{S}}{{\rm{i}}_{3.25}}{\rm{Fe}}_{0.75}^{3 + }} \right){\rm{Fe}}_2^{3 + }{{\rm{O}}_{10}}{\left( {{\rm{OH}}} \right)_2}{\rm{N}}{{\rm{a}}_{0.75}}$. A strictly ferric end-member of the nontronite series was therefore synthesized for the first time. The uncommon chemistry of the synthesized nontronites, notably the high level of Fe-for-Si substitution, induced particular XRD, FTIR, and differential thermal analysis-thermogravimetric analysis data. The ethylene glycol expandability of the synthetic nontronites was linked to their crystallinity and depended on the nature of the interlayer cation, moving from smectite to vermiculite-like behavior. As the synthesis temperature increased, the crystallinity of the synthesized clays increased. The nontronite obtained at 150°C had the ‘best crystallinity’, which cannot be improved by increasing synthesis time or temperature.

Type
Article
Copyright
Copyright © 2008, The Clay Minerals Society

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