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

PbTiO3 has been successfully synthesized at reduced temperatures (500-700 d egreesC) using neither organics (including alkoxides) nor undesirable halid es. Water-soluble peroxytitanic complexes [Ti(OH)(3)O-2](-) were prepared b y the reaction between titanium metal and hydrogen peroxide at pH = 11. A s olution 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 betwe en 200 and 700 degreesC in a closed alumina beat. The precipitate was chara cterized by ICP, TG, Raman spectroscopy, XRD, and SEM, and the calcined lea d titanate was characterized by BET, Raman spectroscopy, XRD, and SEM. The amorphous precipitate showed a small. weight loss (11.45%). Powders calcine d at temperatures higher than 500 degreesC showed pure tetragonal PbTiO3 pe rovskite phase on the XRD patterns and Raman spectra and a large surface ar ea in the range of 6-22 m(2) g(-1). The average diameter of the particles w as calculated from the SEM image as 100 nm.