Effects of calcination temperature on phase and microstructure evolution of BaTi₄O₉ powders

Abstract.

Calcining of the mixture of BaCO₃ and TiO₂ with a ratio 1:4 at different temperatures was carried out to synthesize BaTi₄O₉ powders. Phase evolution of the samples was studied using the differential thermal analysis (DTA) and X-ray diffractometry (XRD). Both techniques confirmed that the formation of BaTi₄O₉ started around 1000 °C. The XRD peaks showed that BaTi₄O₉ was most pronounced at 1250 °C. X-ray line broadening methods were employed to study the variation of particle size and microstrain of the BaTi₄O₉ powders. The Voigt function in a single line and the pseudo-Voigt function in the variance methods were used in our case. We found that both functions resulted in the same trends, i.e., the particle size increased with the temperature with the biggest size of 180 and 160 nm, whilst the microstrain yielded the opposite trend with the lowest values of 6.2 × 10^–3 and 1.1 × 10^–3. The scanning electron microscopy (SEM) study revealed the size of the large particles formed, due to agglomeration, to be about 0.5–1.9 μm. Furthermore, it was shown that irregular shapes of BaTi₄O₉ powders necked to each other appeared at 1000 °C and grew into ellipse and rod shapes at 1250 °C.