Nonaqueous Synthesis of Amorphous Powder Precursors for Nanocrystalline PbTiO3, Pb(Zr,Ti)O3, and PbZrO3

Abstract

A novel, facile nonaqueous synthesis route to nanocrystalline lead zirconate titanate (PZT) powders is presented. Simple mixing of lead acetylacetonate with titanium and/or zirconium alkoxides in 2-butanone, followed by a solvothermal treatment at 200 °C, produced amorphous, nanosized precursor powders. According to X-ray diffraction and transmission electron microscopy investigations, calcination at comparably low temperatures yielded highly crystalline, phase-pure powders consisting of monocrystalline particles in the size range of about 10−30 nm. Thermogravimetric and infrared analyses of the as-prepared samples showed a content of organic species of about 10 wt %, which are decomposed between 200 and 330 °C. The lack of further weight loss above 400 °C proves the absence of PbO evaporation, a major drawback of previous PZT preparations. Crack-free thin films were obtained by simply casting a dispersion of precursor powders on a silicon substrate followed by thermal treatment. Scanning electron microsc...