In-situ X-ray studies of phase transformations in lead zirconate titanate thin films during annealing

Lead zirconate titanate (PZT) thin films were prepared by a sol-gel method on platinized Si and (100) MgO substrates. The evolution in the crystallinity was then studied in real time during annealing with an in-situ X-ray diffraction system using a Ruud-Barrett position-sensitive scintillation detector. Annealing rates of 50 °C min^-1 and 100 °C min^-1 were utilized to study the growth of an intermediate phase and the perovskite phase. This provided direct evidence on the structure evolution during heat treatment. It was observed that an intermediate phase, possibly the pyrochlore, existed over the temperature range 433-580 °C. The film transformed to the perovskite phase as soon as the temperature reached the range 595-600 °C and progressively grew as the temperature approached 650 °C. These results suggested that it may be difficult to bypass intermediate phase formation at this annealing rate. However, for a 100 °C min^-1 heat treatment, the amount of intermediate phase was suppressed from the 50 °C min^-1 case on both platinized Si and MgO substrates.