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Thermogravimetric analysis of selected layered double hydroxides

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Abstract

Thermogravimetric analysis (TG) and powder X-ray diffraction (PXRD) were used to study some selected Mg/Al and Zn/Al layered double hydroxides (LDHs) prepared by co-precipitation. A Mg/Al hydrotalcite was investigated before and after reformation in fluoride and nitrate solutions. Little change in the TG or PXRD patterns was observed. It was proposed that successful intercalation of nitrate anions has occurred. However, the absence of any change in the d (003) interlayer spacing suggests that fluoride anions were not intercalated between the LDH layers. Any fluoride anions that were removed from solution are most likely adsorbed onto the outer surfaces of the hydrotalcite. As fluoride removal was not quantified it is not possible to confirm that this has happened without further experimentation. Carbonate is probably intercalated into the interlayer of these hydrotalcites, as well as fluoride or nitrate. The carbonate most likely originates from either incomplete decarbonation during thermal activation or adsorption from the atmosphere or dissolved in the deionised water. Small and large scale co-precipitation syntheses of a Zn/Al LDH were also investigated to determine if there was any change in the product. While the small scale experiment produced a good quality LDH of reasonable purity; the large scale synthesis resulted in several additional phases. Imprecise measurement and difficulty in handling the large quantities of reagents appeared to be sufficient to alter the reaction conditions causing a mixture of phases to be formed.

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Acknowledgements

The financial and infra-structure support of the Discipline of Nanotechnology and Molecular Science of the Faculty of Science and Engineering, Queensland University of Technology is gratefully acknowledged. The Australian Research Council (ARC) is thanked for funding the instrumentation.

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  1. School of Chemistry, Physics and Mechanical Engineering, Science and Engineering Faculty, Queensland University of Technology, Brisbane, QLD, 4001, Australia

    Frederick L. Theiss, Godwin A. Ayoko & Ray L. Frost

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  1. Frederick L. Theiss
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Correspondence to Ray L. Frost.

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Theiss, F.L., Ayoko, G.A. & Frost, R.L. Thermogravimetric analysis of selected layered double hydroxides. J Therm Anal Calorim 112, 649–657 (2013). https://doi.org/10.1007/s10973-012-2584-z

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  • DOI: https://doi.org/10.1007/s10973-012-2584-z

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