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Clay Minerals; June 2005; v. 40; no. 2; p. 177-190; DOI: 10.1180/0009855054020164
© 2005 Mineralogical Society of Great Britain and Ireland
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Synthesis and characterization of montmorillonite-type phyllosilicates in a fluoride medium

M. REINHOLDT1, J. MIEHÉ-BRENDLÉ1,*, L. DELMOTTE1, R. LE DRED1 and M.-H. TUILIER2

1 Laboratoire deMatériaux Minéraux,UMR 7016, Ecole Nationale Supérieure de Chimie, Université de Haute Alsace, 3 rue Alfred Werner, F-68093 Mulhouse Cedex, and 2 Equipe de Recherche Mécanique Matériaux et Procédés de Fabrication, Université de Haute Alsace, 61 rue Albert Camus, F-68093 Mulhouse Cedex, France

* E-mail: J.Brendle{at}uha.fr

(Received 5 February 2004; revised 21 September 2004)

The fluorine route is thoroughly investigated for the hydrothermal synthesis of montmorillonite in the Na2O-MgO-Al2O3-SiO2-H2O system. Using the optimal conditions suggested by Reinholdt et al. (2001) for the crystallization of pure montmorillonites with the formula Na2x(Al2(1–x)Mg2x{square})Si4O10(OH)2, several parameters (x, Mg content, duration of crystallization, F/Si atomic ratio, pH, nature of counterbalance cation) are varied independently from their ideal values. The products are analysed by various techniques (X-ray diffraction, thermogravimetric analysis-differential thermal analysis, 29Si, 27Al and 19F magic angle spinning-nuclear magnetic resonance). It appears that a pure montmorillonite can only be obtained within a narrow x range (0.10 ≤ x ≤ 0.20). The presence of F in the starting hydrogel and the crystallization time also have significant effects on the purity of the final products. It is shown that a small amount of fluorine is needed for the crystallization of pure montmorillonite phyllosilicates.

KEYWORDS: clay minerals, montmorillonite, synthesis, fluorine, solid-state NMR






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