Abstract
Lithium aluminosilicate inorganic polymers were synthesised from dehydroxylated kaolin-type clay (halloysite) by the conventional method under highly alkaline conditions with lithium hydroxide or lithium silicate solutions of two different Li2O/SiO2 molar ratios. Variants were also developed of a solid-state synthesis method involving the thermal reaction of dehydroxylated halloysite with LiOH followed by hydration of the product. The molar compositions of the materials prepared by all three methods (SiO2/Al2O3 = 2.41–3.27, Li2O/SiO2 = 0.30–0.61, and H2O/Li2O = 9.33–10.40) fall within the range of compositions previously reported to produce viable geopolymers. Curing at 40 °C produces solid samples of varying viability depending on the amount of synthesis water. The cured materials are not characteristically X-ray amorphous, but contain the lithium zeolites Li-ABW and fibrous Li-EDI, the latter in the materials synthesised by solid-state reaction. The 27Al and 29Si MAS NMR spectra of the cured materials contain narrow resonances more characteristic of zeolites than of inorganic polymers. Heating the synthesised products at <800 °C produces β-eucryptite, LiAlSiO4. In a further series of thermal reactions, β-spodumene, LiAlSi2O6 is formed at 900 °C, decomposing at 1100 °C to form additional β-eucryptite. At 1275 °C, β-spodumene reappears in the samples of higher silica content. Judicious manipulation of the composition and thermal treatment of the Li-zeolites formed in these lithium aluminosilicate syntheses could make them useful precursors to β-eucryptite and β-spodumene ceramics.
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Acknowledgements
We are indebted to M. J. Ryan for assistance with the interpretation of the XRD data and to D. Flynn for assistance with the electron microscopy. This study was partly funded by a subcontract from Industrial Research Ltd. of the Foundation for Research Science and Technology contract CO8X0302 and partly by the MacDiarmid Institute for Advanced Materials and Nanotechnology.
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O’Connor, S.J., MacKenzie, K.J.D. Synthesis, characterisation and thermal behaviour of lithium aluminosilicate inorganic polymers. J Mater Sci 45, 3707–3713 (2010). https://doi.org/10.1007/s10853-010-4383-x
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DOI: https://doi.org/10.1007/s10853-010-4383-x