In situ x-ray diffraction of solution-derived ferroelectric thin films for quantitative phase and texture evolution measurement

An in situ measurement technique is developed and presented, which utilizes x-rays from a synchrotron source with a two-dimensional detector to measure thin film microstructural and crystallographic evolution during heating. A demonstration experiment is also shown wherein the measured diffraction patterns are used to describe phase and texture evolution during heating and crystallization of solution-derived thin films. The diffraction images are measured sequentially while heating the thin film with an infrared lamp. Data reduction methodologies and representations are also outlined to extract phase and texture information from the diffraction images as a function of time and temperature. These techniques and data reduction methods are demonstrated during crystallization of solution-derived lead zirconate titanate ferroelectric thin films heated at a rate of 30 degrees C/min and using an acquisition time of 8 s. During heating and crystallization, a PtxPb type phase was not observed. A pyrochlore phase was observed prior to the formation and growth of the perovskite phase. The final crystallized films are observed to have both 111 and 100 texture components. The in situ measurement methodology developed in this work allows for acquiring diffraction images in times as low as 0.25 s and can be used to investigate changes during crystallization at faster heating rates. Moreover, the experiments are shown to provide unique information during materials processing. (C) 2012 American Institute of Physics. [http://dx.doi.org/10.1063/1.4766387]