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New approach of synthesis of phosphate–sulfates with NZP-type structure

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Abstract

New approach of phosphate–sulfate synthesis, preventing sulfur elimination was proposed. It implies sulfur encasement into intermediate with heightened thermal resistance, thus the synthesis temperature of phosphate–sulfate could be increased, and crystallization can be performed. This method is considered to be capable by example of obtaining of Pb2/3FeZr(PO4)7/3(SO4)2/3 ceramic. It was synthesized by means of sol–gel method via formation of intermediate PbSO4, which encased sulfur and eventually led to formation of mentioned before phosphate–sulfate. Obtained sample was characterized via X-ray, IR, combined DTA–TG, SEM and microprobe electron analysis. Crystal structure and unit cell parameters were derived from least-squares refinement of powder X-ray diffraction data (NZP-type, sp. gr.\({\text{R}}\bar{3}{\text{c}}\), a = 8.6339 Å, c = 23.2991 Å, V = 1504.1 Å3). Thermal expansion (α a = 0.96·10−6, α c = 3.24·10−6, α av = 1.76·10−6 K−1) of compound also has been studied. There is a wide area of interest, due to development of ceramics with low thermal expansion.

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Acknowledgements

The present work was performed at the Lobachevsky State University of Nizhni Novgorod with the financial support of the Russian Foundation for Basic Research (Project No. 15-03-00716 a).

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Authors and Affiliations

  1. Lobachevsky State University of Nizhni Novgorod, Gagarin Av. 23, Nizhni Novgorod, Russia, 603950

    V. I. Pet’kov, A. S. Dmitrienko & M. V. Sukhanov

  2. National University of Science and Technology “MISIS”, Leninskii Av. 4, Moscow, Russia, 119049

    A. M. Kovalskii

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  1. V. I. Pet’kov
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  2. A. S. Dmitrienko
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  3. M. V. Sukhanov
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  4. A. M. Kovalskii
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Correspondence to V. I. Pet’kov.

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Pet’kov, V.I., Dmitrienko, A.S., Sukhanov, M.V. et al. New approach of synthesis of phosphate–sulfates with NZP-type structure. J Therm Anal Calorim 127, 2093–2099 (2017). https://doi.org/10.1007/s10973-016-5724-z

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  • DOI: https://doi.org/10.1007/s10973-016-5724-z

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