Abstract
Nanocrystalline NH4ZrH(PO4)2·H2O was synthesized by solid-state reaction at low heat using ZrOCl2·8H2O and (NH4)2HPO4 as raw materials. X-ray powder diffraction analysis showed that NH4ZrH(PO4)2·H2O was a layered compound with an interlayer distance of 1.148 nm. The thermal decomposition of NH4ZrH(PO4)2·H2O experienced four steps, which involves the dehydration of the crystal water molecule, deamination, intramolecular dehydration of the protonated phosphate groups, and the formation of orthorhombic ZrP2O7. In the DTA curve, the three endothermic peaks and an exothermic peak, respectively, corresponding to the first three steps' mass losses of NH4ZrH(PO4)2·H2O and crystallization of ZrP2O7 were observed. Based on Flynn–Wall–Ozawa equation and Kissinger equation, the average values of the activation energies associated with the NH4ZrH(PO4)2·H2O thermal decomposition and crystallization of ZrP2O7 were determined to be 56.720 ± 13.1, 106.55 ± 6.28, 129.25 ± 4.32, and 521.90 kJ mol−1, respectively. Dehydration of the crystal water of NH4ZrH(PO4)2·H2O could be due to multi-step reaction mechanisms: deamination of NH4ZrH(PO4)2 and intramolecular dehydration of the protonated phosphate groups from Zr(HPO4)2 are simple reaction mechanisms.
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Acknowledgements
This study was financially supported by the Guangxi Natural Scientific Foundation of China (Grant No. 0991108), and the Guangxi Science and Technology Agency Research Item of China (Grant No. 0992001-5).
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Wu, W., Wu, X., Lai, S. et al. Non-isothermal kinetics of thermal decomposition of NH4ZrH(PO4)2·H2O. J Therm Anal Calorim 104, 685–691 (2011). https://doi.org/10.1007/s10973-010-0986-3
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DOI: https://doi.org/10.1007/s10973-010-0986-3