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Nanomaterials 2013, 3(1), 48-69; doi:10.3390/nano3010048

Hydrothermal Synthesis and Characterization of Ni-Al Montmorillonite-Like Phyllosilicates

1,* , 2
1 Université de Poitiers, CNRS UMR 7285 IC2MP, ENSIP-Bât. B1, 1 Rue Marcel Doré, F-86022 Poitiers cedex, France 2 Université de Haute Alsace (UHA), CNRS, Equipe Matériaux à Porosité Contrôlée (MPC), Institut de Science des Matériaux de Mulhouse (IS2M), LRC 7228, F-68093 Mulhouse, France 3 Université de Haute Alsace (UHA), Laboratoire Physique et Mécanique Textile (LPMT), EA 4365 (conventionnée au CNRS), F-68093 Mulhouse, France 4 Chimique, Université Laval, 1065 ave. de la Médecine, Québec, QC G1V 0A6, Canada
* Author to whom correspondence should be addressed.
Received: 4 December 2012 / Revised: 3 January 2013 / Accepted: 14 January 2013 / Published: 21 January 2013
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This work describes the first hydrothermal synthesis in fluoride medium of Ni-Al montmorillonite-like phyllosilicates, in which the only metallic elements in the octahedral sheet are Ni and Al. X-ray diffraction, chemical analysis, thermogravimetric and differential thermal analysis, scanning electron microscopy and transmission electron microscopy confirm that the synthesized samples are montmorillonite-like phyllosilicates having the expected chemical composition. The specific surface areas of the samples are relatively large (>100 m2 g1) compared to naturally occurring montmorillonites. 29Si and 27Al nuclear magnetic resonance (NMR) indicate substitutions of Al for Si in the tetrahedral sheet. 19F NMR and Ni K-edge extended X-ray absorption fine structure (EXAFS) local probes highlight a clustering of the metal elements and of the vacancies in the octahedral sheet of the samples. These Ni-Al phyllosilicates exhibit a higher local order than in previously synthesized Zn-Al phyllosilicates. Unlike natural montmorillonites, where the distribution of transition metal cations ensures a charge equilibrium allowing a stability of the framework, synthetic montmorillonites entail clustering and instability of the lattice when the content of divalent element in the octahedral sheet exceeds ca. 20%. Synthesis of Ni-Al montmorillonite-like phyllosilicates, was successfully achieved for the first time. These new synthetic materials may find potential applications as catalysts or as materials with magnetic, optical or staining properties.
Keywords: clay; montmorillonite; synthesis; fluoride medium; solid-state NMR; EXAFS clay; montmorillonite; synthesis; fluoride medium; solid-state NMR; EXAFS
This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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Reinholdt, M.X.; Brendlé, J.; Tuilier, M.-H.; Kaliaguine, S.; Ambroise, E. Hydrothermal Synthesis and Characterization of Ni-Al Montmorillonite-Like Phyllosilicates. Nanomaterials 2013, 3, 48-69.

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