Analysis and Characterization of Phase Evolution of Nanosized BaTiO3 Powder Synthesized Through a Chemically Modified Sol-Gel Process

Abstract

In the current research, a cost-effective and modified method with a high degree of reproducibility was proposed for the preparation of fine nanoscale and high-purity BaTiO3. In contrast to the other established methods, in this research, carbonate-free BaTiO3 nanopowders were prepared at a lower temperature and in a shorter time span. To reach an in-depth understanding of the scientific basis of the proposed process, an in-detail analysis was carried out for characterization of nanoscale BaTiO3 particles via differential thermal analysis (DTA)/thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) techniques aided by theoretical calculations. The effects of the temperature and time of calcination process on the preparation mechanism, phase transformation, tetragonality, and particle size of BaTiO3 were examined. The reaction that results in the formation of barium titanate initiated at approximately 873 K (600 °C) and seemed to be completed at approximately 1073 K (800 °C) and the polymorphic transformation of cubic to tetragonal initiated at approximately 1173 K (900 °C). It seemed to be completed at approximately 1373 K (1100 °C). According to the reaction mechanism, the formation of BaTiO3 in the initial stage of the interfacial reaction between BaCO3 and TiO2 depends on the BaCO3 decomposition. In the second stage, the BaTiO3 formation is controlled by barium diffusion through the barium titanate layer. In this stage, in contrast to the literature, no secondary phase was detected. The overall characterizations showed the temperature is more effective than time on the progress in process of preparation because of its diffusion-controlled nature.