Abstract
In this article, a consistent study of phase transformations during the crystallization of YBa2Cu3O7-δ compound was carried out using XRD, thermogravimetric and differential thermal analyzes, as well as optical microscopy. When studying the microstructure and elemental composition in the reaction zone in the process of obtaining single crystals by the crucible-less method, the products of chemical reactions were identified depending on the composition of the reacting components and synthesis conditions. It has been established that the use of precursors Y2BaCuO5, YBa4Cu3O9-δ and ВаCu2O2 as initial reagents has made it possible to carry out the direct synthesis of YBa2Cu3O7-δ single crystals without the formation of intermediate phases. The superconductor has been synthesized at 1270 K on single-crystal MgO substrates with the (001) orientation, since their surface is poorly wetted by the melt solution and stimulates the YBa2Cu3O7-δ nucleation process. This ensures the minimum loss of the liquid fraction formed in the sample. The growth conditions for YBa2Cu3O7-δ single crystals have been studied and optimized. It has been experimentally revealed that the use of combined cooling conditions leads to an increase in the size of single crystals and a reduction in the time of their growth without changing the quality and crystal structure. The investigation showed that the largest volume (50 mm3) was achieved for single-phase YBa2Cu3O7-δ single crystals grown at a cooling rate of 0.5 deg/h in the temperature range 1260–1240 K and at a rate of 1.2 deg/h in the range 1240–1210 K. An analysis of the Laue rotation lines obtained in this work indicates the presence of blocks in single crystals cooled in the temperature range 1243–1193 K at a cooling rate of 1.5 deg/h and their absence in crystals cooled at 1.2 deg/h. An assessment of the degree of perfection of the structure by the width of the rocking curves at half-height of the X-ray reflection (006) showed that the width of the rocking curves of 0.36 deg indicates the absence of structural defects, such as twins, blockiness, and shear defects.