The sonochemical preparation of PbTiO3 fine powders with lead acetate trihydrate and tetrabutyl titanate as precursors is reported in this paper. Narrow size distribution (40-60 nm) of gel-derived PbTiO3 nanocrystallites at 520degreesC was revealed by transmission electron microscopy. The preparation processings with ultrasonic irradiation and a control test without ultrasonic irradiation for comparison were investigated. Results of phase evolution, microstructure, and thermal analysis of gels were characterized and discussed between the control test and the ultrasonic preparations. Acoustic cavitation exerted an important influence on nucleation, gelation, and homogenization of as-prepared gel, which contributed to the evolution of the resulting gel on further heat treatment. The sonochemical gel was detected to crystallize at temperature, as low as about 410degreesC, which was confirmed by X-ray powder diffraction and thermogravimetric analysis and differential thermal analysis (TGA-DTA).