Thermal Processing and the Evolution of Composition, Structure and Properties for Sol-gel Derived Lead Zirconate Titanate Thin Layers PDF Download
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Author: Charles David Edward Lakeman Publisher: ISBN: Category : Languages : en Pages :
Book Description
Research is reported for the relationships that exist between processing, composition and structure development, and properties, for sol-gel derived $rm Pb(Zrsb{0.53}Tisb{0.47})Osb3$ (PZT) thin layers. Emphasis was placed on the effect of thermal processing conditions on the gel-to-ceramic conversion. In addition, the effects of interfacial reactions, and residual stresses on the measured properties were also considered. The purpose of the work was to contribute to the fundamental understanding of processes which occur during the high temperature treatment of sol-gel derived thin layers. The gel-to-ceramic conversion was monitored by transmission electron microscopy, diffuse reflectance infrared spectroscopy, and X-ray diffraction. As-deposited coatings were found to be amorphous with compositional heterogeneity at the nanoscale. This is the first report which identifies the nature of the compositional heterogeneity. Structural rearrangement occurred during thermal processing and, for slow heating (50$spcirc$C/min), the coatings approached compositional uniformity on crystallization into the perovskite phase. However, for faster heating rates, the degree of structural rearrangement was limited, thereby decreasing the shrinkage normal to the coating, and crystallization was shifted to a higher temperature. Also, for very rapid thermal processing (5000$spcirc$C/min), compositional heterogeneity was retained in the coatings after crystallization. An apparent dependence on thickness for the properties for ferroelectric PZT thin layers was observed. It was confirmed that a cover coat of a PbO-precursor deposited onto the gel-derived layers prior to firing compensated for the volatilization of PbO which occurred during heating, resulting in coatings which displayed improved properties over those prepared without a cover coat. A simple series capacitor model was investigated to interpret the data. SIMS and TEM analyses indicated that diffusion of some of the species resulted in the formation of a sub-electrode nano-crystalline phase, however, no second phases were observed between the electrode and the coating. Measurements of the residual stress state in PZT coatings deposited onto platinized silicon substrates, and fired at 700$spcirc$C, indicated a tensile stress of approximately +200MPa in the plans of the coating. Thermal expansion mismatch stresses were calculated to be of the order of $-$300MPa in compression, indicating that large tensile stresses were generated during constrained shrinkage.
Author: Charles David Edward Lakeman Publisher: ISBN: Category : Languages : en Pages :
Book Description
Research is reported for the relationships that exist between processing, composition and structure development, and properties, for sol-gel derived $rm Pb(Zrsb{0.53}Tisb{0.47})Osb3$ (PZT) thin layers. Emphasis was placed on the effect of thermal processing conditions on the gel-to-ceramic conversion. In addition, the effects of interfacial reactions, and residual stresses on the measured properties were also considered. The purpose of the work was to contribute to the fundamental understanding of processes which occur during the high temperature treatment of sol-gel derived thin layers. The gel-to-ceramic conversion was monitored by transmission electron microscopy, diffuse reflectance infrared spectroscopy, and X-ray diffraction. As-deposited coatings were found to be amorphous with compositional heterogeneity at the nanoscale. This is the first report which identifies the nature of the compositional heterogeneity. Structural rearrangement occurred during thermal processing and, for slow heating (50$spcirc$C/min), the coatings approached compositional uniformity on crystallization into the perovskite phase. However, for faster heating rates, the degree of structural rearrangement was limited, thereby decreasing the shrinkage normal to the coating, and crystallization was shifted to a higher temperature. Also, for very rapid thermal processing (5000$spcirc$C/min), compositional heterogeneity was retained in the coatings after crystallization. An apparent dependence on thickness for the properties for ferroelectric PZT thin layers was observed. It was confirmed that a cover coat of a PbO-precursor deposited onto the gel-derived layers prior to firing compensated for the volatilization of PbO which occurred during heating, resulting in coatings which displayed improved properties over those prepared without a cover coat. A simple series capacitor model was investigated to interpret the data. SIMS and TEM analyses indicated that diffusion of some of the species resulted in the formation of a sub-electrode nano-crystalline phase, however, no second phases were observed between the electrode and the coating. Measurements of the residual stress state in PZT coatings deposited onto platinized silicon substrates, and fired at 700$spcirc$C, indicated a tensile stress of approximately +200MPa in the plans of the coating. Thermal expansion mismatch stresses were calculated to be of the order of $-$300MPa in compression, indicating that large tensile stresses were generated during constrained shrinkage.
Author: Samit Sushil Sengupta Publisher: ISBN: Category : Languages : en Pages : 360
Book Description
Significant progress has been made in recent years on the deposition of ferroelectric thin layers by sol-gel processing. However, to sustain further improvements in the technique necessary for widespread applications, a systematic approach to the study of physical, chemical and structural changes that occur during transformation from the as-deposited state to the desired perovskite phase must be undertaken. In view of the need for a fundamental understanding of structure-processing relationships in these systems, this thesis investigates variations in local structure and network development for sol-gel derived precursors in the lead zirconate titanate (PZT) system as a function of heat treatment conditions. Structural studies were based on extended x-ray absorption fine structure (EXAFS) analysis of gels and thin layers. Consolidation of the thin layer network was monitored by in situ ellipsometry and thermal analysis techniques. The resulting constrained shrinkage for the deposited layers produced large stresses (up to 180 MPa), which were determined by wafer bending measurements. EXAFS measurements for partially heat-treated PZT gels are reported. After gels were dried and pyrolyzed, the amorphous structure was determined from results obtained from the titanium and zirconium K-edges and the lead L$rmsb{III}$-edge. For lead titanate (PT) and PZT53/47 gels, the results indicated the formation of separate TiO$sb6$ and ZrO$sb6$ units linked via corner-sharing oxygen atoms, with Pb in random positions. For lead zirconate (PZ) gels, both Zr-O-Pb and Zr-O-Zr linkages were possible. These findings indicate heterogeneity at the molecular level and nanoscale. Partially heat-treated thin layers of lead titanate deposited on polycrystalline alumina substrates were heat treated under various conditions to examine the evolution of the crystalline phase. Structural ordering was initiated by a progressive enhancement in the Pb-O coordination number and increased occupancy of Pb in the second shell of Ti, with a corresponding breakdown in the Ti-Ti second neighbor ordering. However, crystallization preceded complete development of the short-range order characteristic of the tetragonal perovskite unit. Densification of PZT thin layers spin-coated on silicon was monitored by shrinkage and optical measurements. With increasing Zr content, the net consolidation was greater and occurred over a wider temperature range. These differences were related to differences in the structure of the as-hydrolyzed precursors. Most of the total shrinkage (e.g., 40-45% linear shrinkage) on heating to 500$spcirc$C occurred during drying and pyrolysis, which resulted in large tensile stress ($sim$150MPa). Subsequent stress behavior was primarily governed by the thermal expansion mismatch between the substrate and the coating. Stress development for multideposited PT coatings was determined by the structure of the layer on which the coating was being deposited and heat treated. Progressive crystallization of the layer induced a change in the thermal expansion coefficient, thereby initiating a change in the stress state from tensile to compressive. The observed behavior is discussed in terms of nucleation mechanisms at the multilayer interfaces and within the coating as a whole. This study has demonstrated the importance of identifying structural pathways and developing a basic understanding of the densification behavior in sol-gel derived materials as a function of thermal processing conditions. The findings of this research work should aid in developing suitable experimental procedures for future processing of gel-derived thin layers.
Author: G. Piccaluga Publisher: Trans Tech Publications Ltd ISBN: 3035705941 Category : Technology & Engineering Languages : en Pages : 56
Book Description
Materials with nanometer size particles exhibit unique chemical and physical properties. In particular, nanocomposite materials, composed of nanometric metal and metal oxide particles embedded in vitreous matrices, present a variety of interesting magnetic, electric and catalytic properties, that are strongly size-dependent. Among the different preparation methods which can be used to obtain this kind of materials, the sol-gel process is particularly interesting because it is affected by several parameters which allow a versatile control of the structural, textural and chemical properties of the final products. The present volume focusses on the preparation of metal-silica and metal oxide-silica (Me=Ni, Fe, Zn) nanocomposites by the sol-gel method and the characterization of their structural and magnetic properties.
Author: Charles David Edward Lakeman
Author: Charles David Edward Lakeman
Author: Charles David Edward Lakeman
Author: Cheng-Chen Hsueh
Author: Kashyap Ramachandra Bellur
Author: Stephen Henry Pyke
Author: Samit Sushil Sengupta
Author: 
Author: Michael Walter Russell
Author: Wei Cao
Author: G. Piccaluga