Abstract
The solid-state synthesis of undoped K0.5Na0.5NbO3 (KNN) and KNN doped with 1, 2 and 6 mol% Sr, from potassium, sodium and strontium carbonates with niobium pentoxide, was studied using thermal analysis and in situ high-temperature X-ray diffraction (HT-XRD). The thermogravimetry and the differential thermal analyses with evolved-gas analyses showed that the carbonates, which were previously reacted with the moisture in the air to form hydrogen carbonates, partly decomposed when heated to 200 °C. In the temperature interval where the reaction was observed, i.e., between 200 and 750 °C, all the samples exhibited the main mass loss in two steps. The first step starts at around 400 °C and finishes at 540 °C, and the second step has an onset at 540 °C and finishes with the end of the reaction between 630 and 675 °C, depending on the particle size distribution of the Nb2O5 precursor. According to the HT-XRD analysis, the perovskite phase is formed at 450 °C for all the samples, regardless of the Sr content. The formation of a polyniobate phase with a tetragonal tungsten bronze structure was detected by HT-XRD in the KNN with the largest amount of Sr dopant, i.e., 6 mol% of Sr, at 600 °C.
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Acknowledgements
This work was supported by the Slovenian Research Agency, under Grants P2-0105 and PR-03727. The authors would like to thank Edi Kranjc for measuring the HT-XRD of the samples.
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Hreščak, J., Malič, B., Cilenšek, J. et al. Solid-state synthesis of undoped and Sr-doped K0.5Na0.5NbO3 . J Therm Anal Calorim 127, 129–136 (2017). https://doi.org/10.1007/s10973-016-5615-3
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DOI: https://doi.org/10.1007/s10973-016-5615-3