PZT nanocrystalline powder was prepared by a stearic acid gel method. The crystallization process from the precursor was monitored by infrared spectroscopy, differential thermal analysis, and thermogravimetric analysis. The nano-sized PZT powder was characterized by X-ray diffraction and transmission electron microscopy. It shows that pure single-phase PZT powder could be obtained at 450℃ for 1 h, and the particle size is about 20 nm. With an increase in the calcination temperature, the PZT crystallite size increased.