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Low-temperature synthesis of CaZrTi2O7 zirconolite-type materials using coprecipitation and sol-gel methods

Abstract

The effects of solution-based synthesis methods (coprecipitation and sol-gel) on the long- and short-range structures of zirconolite-type oxides annealed at various temperatures was investigated. Powder X-ray diffraction (XRD) was used to study the formation of the zirconolite phase at all temperatures studied (700 to 1400 °C). While the zirconolite structure was observed to be formed over the temperature range of 900 to 1400 oC, a mixture of zirconolite and defect fluorite phases were observed when the annealing temperature was 800 oC and only the defect fluorite structure was observed when the annealing temperature was 700 oC. Changes in the long-range structure of the zirconolite-type materials were evaluated by Rietveld refinement of the diffraction patterns. X-ray absorption near edge spectroscopy (XANES) was used to probe the local structure of Ti and Zr within the materials. Examination of the Ti K- and Zr K-edge XANES spectra showed no change in the local structure of the zirconolite-type materials annealed at temperatures as low as 900 °C while changes were observed when lower annealing temperatures were used owing to the presence of both the zirconolite and defect fluorite phases. It has been shown in this study that zirconolite-type materials can be synthesized at temperatures as low as 900 °C using coprecipitation or sol-gel methods due to the atomic scale mixing of reactants which occurs in solution. Both the long-range and local structures of the zirconolite materials formed by the sol-gel and coprecipitation methods compared well to equivalent materials formed at high temperature using the traditional ceramic method. The reduction of the annealing temperatures required to form zirconolite-type materials results in more cost-efficient processing which is ideal for industrial scaling.

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Publication details

The article was received on 09 Sep 2018, accepted on 03 Dec 2018 and first published on 04 Dec 2018


Article type: Paper
DOI: 10.1039/C8TC04560G
Citation: J. Mater. Chem. C, 2018, Accepted Manuscript
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    Low-temperature synthesis of CaZrTi2O7 zirconolite-type materials using coprecipitation and sol-gel methods

    S. McCaugherty and A. P. Grosvenor, J. Mater. Chem. C, 2018, Accepted Manuscript , DOI: 10.1039/C8TC04560G

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