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DTA-TG and XRD study on the reaction between ZrOCl2·8H2O and (NH4)2HPO4 for synthesis of ZrP2O7

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Abstract

In this paper, we report results of thermoanalytical investigation on the reaction between ZrOCl2·8H2O and (NH4)2HPO4 in molar ratio 1:2. Differential thermal-thermogravimetric and X-ray diffraction analyses were performed in order to reveal the chemical transformations, which took place during heating of the individual compounds ZrOCl2·8H2O, (NH4)2HPO4 and the mixture ZrOCl2·8H2O:2(NH4)2HPO4. It was shown that the transformations in the mixture below 160 °C were connected with dehydration of ZrOCl2·8H2O and interaction between the components of the mixture, which resulted in the formation of NH4Cl, NH4H2PO4 and a mainly amorphous zirconium phase, most likely t-ZrO2. The zirconium component subsequently reacted with ammonium dihydrophosphate (below 200 °C) or with dehydrated phosphate derivatives (above 200 °C), which in both cases yielded an amorphous product. The interaction between the components of the mixture resulting in the formation of ZrP2O7 was completed by its crystallisation at 610 °C. Our study indicates an alternative low-temperature approach for the synthesis of the technologically important ZrP2O7 material.

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Acknowledgements

The Ministry of Education, Youth and Sports of the Czech Republic, Project CZ.1.07/2.3.00/30.0021 “Enhancement of R&D Pools of Excellence at the University of Pardubice”, financially supported this work.

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Authors and Affiliations

  1. Department of Inorganic Technology, Faculty of Chemical Technology, University of Pardubice, Doubravice 41, 532 10, Pardubice, Czech Republic

    Nataliia Gorodylova & Petra Šulcová

  2. Department of Inorganic and Analytical Chemistry, Faculty of Chemical Technology and Engineering, West-Pomeranian University of Technology, Szczecin, Al. Piastow 42, 71 065, Szczecin, Poland

    Monika Bosacka & Elżbieta Filipek

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  1. Nataliia Gorodylova
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Correspondence to Nataliia Gorodylova.

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Gorodylova, N., Šulcová, P., Bosacka, M. et al. DTA-TG and XRD study on the reaction between ZrOCl2·8H2O and (NH4)2HPO4 for synthesis of ZrP2O7 . J Therm Anal Calorim 118, 1095–1100 (2014). https://doi.org/10.1007/s10973-014-3890-4

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