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Issue 9, 2004
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A time resolved, in-situ X-ray diffraction study of the de-intercalation of anions and lithium cations from [LiAl2(OH)6]nqH2O (X = Cl, Br, NO3, SO42−)

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Abstract

The layered double hydroxides (LDHs), [LiAl2(OH)6]nqH2O (Xn = Cl, Br, NO3, SO42−) spontaneously lose both Li+ cations and Xn anions to give crystalline Al(OH)3 on stirring in water. The kinetics of this topochemical de-intercalation reaction have been studied using time-resolved, in-situ energy dispersive X-ray powder diffraction. The temperature dependence of the rate of the de-intercalation reaction yields activation energies of 94 ± 15 kJ mol−1 for mono-dispersed [LiAl2(OH)6]Cl·1.5H2O crystallites (particle size 5–10 µm) and 117 ± 15 kJ mol−1 for poly-dispersed [LiAl2(OH)6]Cl·1.5H2O crystallites (particle size 1–30 µm). The rate of ion de-intercalation was found to decrease as the H2O/LDH ratio decreased. The rate of the de-intercalation has also been shown to be dependent on the interlayer anion, with the reaction rates NO3 > Cl > Br. In the case of SO42− rapid de-intercalation only goes to 40% completion.

Graphical abstract: A time resolved, in-situ X-ray diffraction study of the de-intercalation of anions and lithium cations from [LiAl2(OH)6]nX·qH2O (X = Cl−, Br−, NO3−, SO42−)

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Publication details

The article was received on 11 Nov 2003, accepted on 25 Feb 2004 and first published on 24 Mar 2004


Article type: Paper
DOI: 10.1039/B314473A
Citation: J. Mater. Chem., 2004,14, 1443-1447
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    A time resolved, in-situ X-ray diffraction study of the de-intercalation of anions and lithium cations from [LiAl2(OH)6]nqH2O (X = Cl, Br, NO3, SO42−)

    K. A. Tarasov, V. P. Isupov, L. E. Chupakhina and D. O'Hare, J. Mater. Chem., 2004, 14, 1443
    DOI: 10.1039/B314473A

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