Stress development in thin layers of lead titanate prepared by sol-gel processing was monitored by in situ laser reflectance measurements. Layers were spin coated onto silicon substrates and thermally cycled to 500°C. The shrinkage normal to the rigid substrate was determined by in situ ellipsometry. Changes that occurred on drying and firing, which related to densification and stress development, are reported. The observed changes were explained in terms of evaporation and solvent/polymeric network interactions at lower temperatures, and thermal expansion mismatch between the substrate and the coating after formation of the dense oxide. Crystallization into the perovskite structure occurred only in thicker or multideposited coatings, altering the state of stress from tensile, to progressively more compressive, on cooling. The importance of the choice of substrate material, deposition method and heat treatment conditions, in relation to stress development and dependent electrical properties, are discussed.
We report on extended x-ray absorption fine structure (EXAFS) measurements for partially heat-treated gels in the lead zirconate titanate system (PZT). Self-consistent results obtained from the titanium and zirconium A"-edges and the lead Lm-edge were used to determine bonding pathways between cations. For lead titantate (PT) and PZT gels, separate networks of predominantly Ti-O-Ti, Zr-O-Zr, and Pb-O-Pb linkages were observed. For lead zirconate (PZ) gels, both Zr-O-Pb and Zr-O-Zr linkages were observed. The results indicate heterogeneity at the molecular level. These findings are discussed in terms of the evolution of structure for PZT materials prepared by our sol-gel method.
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