| Summary: | Despite considerable efforts undertaken in a rapidly developing area of multiferroic research, synthesis of phase pure BiFeO<sub>3</sub> is still a matter of intensive research. In this work, we report the shape-controlled synthesis of pure BiFeO<sub>3</sub> microspheres via a facile hydrothermal route. The prepared BiFeO<sub>3</sub> powder has been characterized using powder X-ray Diffraction (XRD), Differential Thermal analysis (DTA), Scanning Electron microscopy (SEM), and impedance spectroscopy. Powder XRD analysis confirms the formation of pure rhombohedrally distorted perovskite with <i>R</i>3<i>c</i> space group. Scanning electron micrograph revealed that the prepared BiFeO<sub>3</sub> microspheres are nearly spherical in shape with uniform size distribution. The BiFeO<sub>3</sub> microspheres exhibit a dielectric constant value of ~110 at 1000 KHz, which is higher than the BiFeO<sub>3</sub> prepared by conventional solid-state reaction and sol–gel method. Variation of dielectric constant with temperature at different frequencies shows that the BiFeO<sub>3</sub> has a dielectric anomaly of ferroelectric to paraelectric type at 1093 K and this phenomenon is well supported by TGA results.
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