In recent years Sol-Gel processing provides an interesting alternative method for the fabrication of ferroelectric thin layers and powder. PZT powder was prepared from an alkoxide-based solution by a Sol-Gel method. Gelation of synthesized complex solutions, microstructure, thermal analysis and crystallization behaviors of the calcined powder were studied in accordance with a water content and a catalyst. Especially gelation and crystallization behavior were analysed with the change of pH. The gelation time decreased as the pH of the mixed solution increased. For PZT powder with 650.deg. C heat treatment, 100% perovskite phase was formed by using either acidic or basic catalyst. By using either acidic or basic catalyst, we were able to get very fine powders of uniform shape with an average particle size of 0.8-1.mu.m.