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Key Steps Influencing the Formation of Aluminosilicate Nanotubes by the Fluoride Route

Published online by Cambridge University Press:  01 January 2024

Atika Chemmi ,
Jocelyne Brendle ,
Claire Marichal  and
Benedicte Lebeau
Atika Chemmi
Affiliation:
Pôle Matériaux à Porosité Contrôlée (MPC), Institut de Science des Matériaux de Mulhouse (IS2M), CNRS UMR 7361, Universitéde Haute Alsace (UHA), ENSCMu, 3b rue Alfred Werner 68093 Mulhouse Cedex, France
Jocelyne Brendle*
Affiliation:
Pôle Matériaux à Porosité Contrôlée (MPC), Institut de Science des Matériaux de Mulhouse (IS2M), CNRS UMR 7361, Universitéde Haute Alsace (UHA), ENSCMu, 3b rue Alfred Werner 68093 Mulhouse Cedex, France
Claire Marichal
Affiliation:
Pôle Matériaux à Porosité Contrôlée (MPC), Institut de Science des Matériaux de Mulhouse (IS2M), CNRS UMR 7361, Universitéde Haute Alsace (UHA), ENSCMu, 3b rue Alfred Werner 68093 Mulhouse Cedex, France
Benedicte Lebeau
Affiliation:
Pôle Matériaux à Porosité Contrôlée (MPC), Institut de Science des Matériaux de Mulhouse (IS2M), CNRS UMR 7361, Universitéde Haute Alsace (UHA), ENSCMu, 3b rue Alfred Werner 68093 Mulhouse Cedex, France
*
*E-mail address of corresponding author: jocelyne.brendle@uha.fr
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Abstract

Imogolite is usually formed by means of a three-step process involving the use of large amounts of water with long crystallization times and low yields, preventing large-scale synthesis. These drawbacks can be overcome by synthesis in the presence of fluoride, an approach which has been demonstrated to be suitable for the synthesis of other phyllosilicates. In the present study, the nature of the Al and Si sources, the Al/Si molar ratio, the volume of H2O for the redispersion of the gel after desalination, the F/Si molar ratio, as well as the crystallization temperature and time have been varied to investigate their role in the crystallization of imogolite. The structural properties of the as-synthesized samples were characterized by X-ray diffraction, infrared spectroscopy, and 29Si, 27Al, and 19F magic angle spinning nuclear magnetic resonance spectroscopy. The results show that the imogolite nanotubes can be prepared with high yields (>55%) from AlCl3·6H2O and Na4SiO4 aqueous solutions with an Al/Si molar ratio of 2.5, addition of HF for a F/Si molar ratio of 0.1–0.2, and 4 days of crystallization at 98°C.

Keywords

Aluminosilicate NanotubeFluoride RouteImogolite
Type
Research Article
Information
Clays and Clay Minerals , Volume 63 , Issue 2 , April 2015 , pp. 132 - 143
Copyright
Copyright © Clay Minerals Society 2015

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