Affiliation:
1. Yuriy Fedkovych Chernivtsi National University
Abstract
The crystalline CsPbBr3 was synthesized from CsBr (6N) and PbBr2 (5N) by the mechanochemical method with further fusion in quartz ampoule at 640-650 °С. After synthesis, the structure and chemical composition of the obtained material was confirmed by energy-dispersive X-ray spectroscopy (EDX) and X-ray diffraction analysis. The melting and crystallization of the obtained perovskite were investigated by the differential thermal analysis (DTA) with heating/cooling rates of 1, 5 and 10 °C/min. Measurements were carried on the self-constructed DTA-setup with S-type thermocouples in the range of 450-590 °C. Each cycle of heating/cooling was repeated three times to confirm the accuracy of the results obtained. A decrease in the melting point from ~ 568.1 °C to ~ 566.2 °C was demonstrated with an increase in the heating rate from 1 °C/min. up to 10 °C/min. respectively. Probably, it's due to the approach to equilibrium conditions of phase transformations at lower heating rates. We recorded an additional-endothermic effect during CsPbBr3 melting. This may indicate a complex process of melting the compound. The thesis of a two-stage melting mechanism of CsPbBr3 perovskite with an initial stage of fragmentation of the crystalline structure and subsequent dissolution of crystalline phase residues is proposed. It is reported that with increasing of the melt heating above a certain "critical" temperature (579-585 °C), its homogenization occurs, and the crystallization temperature is set at 540-550 °C for the heating/cooling rate of 1 ° C/min. and 538-543 °C for the rate of 5-10° C/min. All obtained data confirm the assumption of a two-step melting process of CsPbBr3 perovskite, and the relatively constant crystallization temperature after a critical point of overheating may also indicate a certain structure of the melt of the compound with short-range order in the arrangement of the structural units of the compound in the liquid phase.
Publisher
Yuriy Fedkovych Chernivtsi National University
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