Preparation and characterization of nanometer-sized (Pb 1− x,Ba x)TiO 3 powders using acetylacetone as a chelating agent in a non-aqueous sol–gel process

Abstract

Nanometer-sized lead barium titanate (Pb 1− x Ba x TiO 3, PB x T) powders were prepared by a non-aqueous sol–gel process using lead acetate, barium acetate, and titanium isopropoxide as precursors and ethylene glycol as the solvent. In this procedure, Ti-isopropoxide was chelated with acetylacetone. The samples were characterized by Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, thermogravimetric analysis/differential thermal analysis (TGA/DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM) and Brunauer–Emmett–Teller (BET) specific surface area analysis. The results indicate that perovskite PB x T phases were obtained by heat treatment at 450 °C for 5 h, and a pure perovskite was examined at 600 °C. The average particle sizes of perovskite PB x T powders calcined at 600 °C were approximately about 40–80 nm, and BET analysis showed that the surface areas of the powders obtained at 600 °C were approximately 6–16 m 2/g. In addition, the phase transition from the tetragonal ferroelectric phase to the cubic paraelectric phase occurred in a range of approximately 0.6 < x < 0.8.