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Published online by Cambridge University Press: 10 February 2011
Stress development in thin layers of PbZr0.53Ti0.47O3 (PZT) and PbTiO3 (PT) prepared by sol-gel processing was monitored by in situ laser reflectance measurements. Layers were spin coated onto silicon substrates and thermally cycled to 600°C and 650°C. The shrinkage normal to the film plane was determined by in situ ellipsometry and scanning electron microscopy. Both PZT and PT multilayers showed a similar stress behavior on heating, but quite different behavior on cooling. As the film became dense at high temperatures, total stress was dominated by the thermal expansion mismatch between the oxide layer and the substrate. On cooling, the PT multilayers, which already crystallized into the perovskite structure, ended nearly stress free at room temperature, whereas mostly amorphous PZT multilayers were under a high tensile stress. Densification in PZT layers appeared to occur between 370°C and 520°C. At near 370°C the shrinkage mode for a single PZT layer was also observed to change substantially. A two-stage sintering process employing 450°C-sintering and 650°C-crystallization was found to be as effective as direct furnace insertion method in producing a dense film.