Peroxide-based route free from halides for the synthesis of lead titanate powder

PbTiO3 has been successfully synthesized at reduced temperatures (500-700 degreesC) using neither organics (including alkoxides) nor undesirable halides. Water-soluble peroxytitanic complexes [Ti(OH)(3)O-2](-) were prepared by the reaction between titanium metal and hydrogen peroxide at pH = 11. A solution of lead nitrate was added to the peroxytitanic acid solution and an amorphous precipitate of lead and titanium was formed, which was filtered and washed to eliminate the nitrate ion. The precipitate was calcined between 200 and 700 degreesC in a closed alumina beat. The precipitate was characterized by ICP, TG, Raman spectroscopy, XRD, and SEM, and the calcined lead titanate was characterized by BET, Raman spectroscopy, XRD, and SEM. The amorphous precipitate showed a small. weight loss (11.45%). Powders calcined at temperatures higher than 500 degreesC showed pure tetragonal PbTiO3 perovskite phase on the XRD patterns and Raman spectra and a large surface area in the range of 6-22 m(2) g(-1). The average diameter of the particles was calculated from the SEM image as 100 nm.