The sol-gel process is a technique which is applicable for forming ceramic materials. In this process, liquid precursor materials are reacted to form a sol which then polymerizes into an inorganic polymeric gel. Advantages of this process over standard powder preparation of ceramics are: purity, homogeneity, control of macro- and micro-structures, and low processing temperatures. In our laboratory the sol-gel process has been used to form lead titanate. We detail a procedure which has produced dried monolithic gels up to 1.5 cm in diameter. The as-dried gels have not been exposed to temperatures above 40‡ C and are X-ray amorphous. Samples of the gels were crushed into powder and heated at 8‡ C min−1 to various temperatures up to 500‡ C, held for a variety of times, and then cooled to room temperature. After certain annealing procedures crystalline phases were observed. The initial crystalline phase to emerge has not yet been identified. Upon further annealing this phase transforms to tetragonal PbTiO3.