Structural Investigation of Zn(II) Insertion in Bayerite, an Aluminum Hydroxide. - Archive ouverte HAL Accéder directement au contenu
Article Dans Une Revue Inorganic Chemistry Année : 2016

Structural Investigation of Zn(II) Insertion in Bayerite, an Aluminum Hydroxide.

Résumé

Bayerite was treated under hydrothermal conditions (120, 130, 140, and 150 °C) to prepare a series of layered double hydroxides (LDHs) with an ideal composition of ZnAl4(OH)12(SO4)0.5·nH2O (ZnAl4-LDHs). These products were investigated by both bulk techniques (powder X-ray diffraction (PXRD), transmission electron microscopy, and elemental analysis) and atomic-level techniques (1H and 27Al solid-state NMR, IR, and Raman spectroscopy) to gain a detailed insight into the structure of ZnAl4-LDHs and sample composition. Four structural models (one stoichiometric and three different defect models) were investigated by Rietveld refinement of the PXRD data. These were assessed using the information obtained from other characterization techniques, which favored the ideal (nondefect) structural model for ZnAl4-LDH, as, for example, 27Al magic-angle spinning NMR showed that excess Al was present as amorphous bayerite (Al(OH)3) and pseudoboehmite (AlOOH). Moreover, no evidence of cation mixing, that is, partial substitution of Zn(II) onto any of four Al sites, was observed. Altogether this study highlights the challenges involved to synthesize pure ZnAl4-LDHs and the necessity to use complementary techniques such as PXRD, elemental analysis, and solid-state NMR for the characterization of the local and extended structure of ZnAl4-LDHs.

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Chimie
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Dates et versions

hal-01384759 , version 1 (20-10-2016)

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Citer

Suraj Shiv Charan Pushparaj, Nicholai Daugaard Jensen, Claude Forano, Gregory J. Rees, Vanessa Prevot, et al.. Structural Investigation of Zn(II) Insertion in Bayerite, an Aluminum Hydroxide. . Inorganic Chemistry, 2016, 55, pp.9306-9315. ⟨10.1021/acs.inorgchem.6b01436⟩. ⟨hal-01384759⟩
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