In this manuscript, the effect of substituting strontium with barium on the structural properties of Tl0.8Ni0.2Sr2-xBrxCa2Cu3O9-δcompound with x= 0, 0.2, 0.4, have been studied. Samples were prepared using solid state reaction technique, suitable oxides alternatives of Pb2O3, CaO, BaO and CuO with 99.99% purity as raw materials and then mixed. They were prepared in the form of discs with a diameter of 1.5 cm and a thickness of (0.2-0.3) cm under pressures 7 tons / cm2, and the samples were sintered at a constant temperature of 860 ° C. The structural properties were studied using X-ray diffraction for all samples, and the results showed that the samples have tetragonal structure and the change of the parameters structure with the change of the barium concentration. Full Width Half Maximum (FWHM) was calculated by Orange Pro using X-RAY data. The crystal size was calculated using Scherrer and Willeamson-Heall methods, where the results showed that the crystal size, compliance and degree of crystallinity changed with the change of barium concentration, and the highest average for the crystal size was 70.0271nm at x=0, and crystallization at 61.46% at x=0.6, and the strain decreased to 0.0037 when barium concentration equals 0.4.
