Effects of powder preparation and sintering procedure on microstructure and dielectric properties of PLZT ceramics

PLZT ceramics belong to one of the very important groups of functional materials that make a basis for the production of a large range of electronic devices. The microstructure and properties of ceramics depend on the powder preparation and thermal processing conditions. Various techniques have been used to obtain chemically homogeneous and fine starting powders. PLZT powders have been prepared by two different production routes: by a modified Pechini method, using a polymeric precursor method (PMM) and by a partial oxalate method. A two-step sintering process, including a hot pressing, was carried out at 1100 and 1200degreesC Distinct phases obtained during the sintering process have been investigated by SEM and EDS techniques and dielectric properties such as permittivity and dielectric loss were measured in a frequency range from 1 to 20 kHz.. A significant difference in microstructure and dielectric properties, depending on powder origin and sintering procedure, has been noticed.

Structural characterization of organometallic-derived 9.5/65/35 PLZT ceramics

This study consisted of an investigation of the influence of powder preparation on the phase and chemical compositions and microstructure of 9.5/65/35 PLZT materials sintered in an oxygen atmosphere. The powders with the formula Pb0.905La0.095(Zr0.65Ti0.35)(0.976)O-3+3.5 wt.% PbO were prepared by the polymeric organometallic precursor method (the Pechini method and the partial oxalate procedure). Phase composition was determined by X-ray diffraction of powder and EDS analysis, while grain size was determined based on the micrograph obtained from SEM. (C) 2001 Elsevier B.V. B.V. All rights reserved.

Sintering and characterization of PLZT (9/65/35)

PLZT(9/65/35) obtained by association between the Pechini method (ZT) and partial oxalate (PLZT) was prepared. The stoichiometric phase and monophasic (cubic) PLZT obtained by calcination did not occur after sintering. The sintering process, by using two stages, caused a liquid phase formation due to a PbO excess (5 and 10 wt%). Samples with high density (similar to 8 g/cm(3)) and optical transparency(similar to 12%) were obtained. However, an equilibrium between the excess of PbO of sample/atmosphere PbO leads to a segregated PbO phase on the boundaries of the microstructure. A diffusion of Zr, Ti and La ions from PLZT to PbO phase promoted a stoichiometric deviation of the matrix and modified the optical and dielectric characteristics. (C) 2000 Elsevier B.V. Ltd and Techna S.r.l. All rights reserved.

Screen printed PLZT thick films prepared from nanopowders

The gap between the bulk materials and thin films can be filled with thick films suitably designed and appropriate processed. Thick films of complex system like lead-lanthanum-zirconium titanate (PLZT) is difficult to produce by simple solid-state reaction keeping compositional homogeneity and optimal grain size distribution. In the present work, PLZT thick films were fabricated by screen-printing technique from nanosized powders obtained through soft chemistry by polymeric precursor method. Thick film paste was obtained by mixing PLZT fine powders and organic vehicle. The upper and bottom electrodes based on Ag-Pd and functional component based on PLZT were screen-printed on alumina substrate and after that annealed in air atmosphere. The powder morphology, microstructure, dielectric and ferroelectric properties of 9.5/65/35 PLZT thick films were analysed. (c) 2007 Elsevier Ltd. All rights reserved.

Synthesis and characterization of 9.5/65/35 PLZT prepared from the polymeric precursors

The 9.5/65/35 PLZT was prepared from the polymeric precursors (the Pechini and partial oxalate process) and by sintering in two stages in an oxygen atmosphere. After thermal treatment at 400 degreesC, the powders were calcinated and sintered at 1200 degreesC with slow heating and cooling rates. The second stage of sintering consisted of hot pressing at the same temperature in oxygen atmosphere. After calcination of PLZT powders obtained by both methods, as well as after sintering of PLZT obtained by Pechini process, the paraelectric cubic phase was formed. After sintering of PLZT obtained by partial oxalate procedure, small tetragonality of crystal structure was observed. After hot pressing PLZT was pseudocubic. SEM microstructural analyses were carried out of the sintering and hot pressed samples and indicated the small grain size less than 2 mum. (C) 2001 Elsevier B.V. B.V. All rights reserved.

Hot-pressed 9.5/65/35 PLZT prepared by the polymeric precursor method

A 9.5/65/35 PLZT ceramic with a Pb-0.905 La-0.095 (Zr-0.65 Ti-0.35)(0.976) O-3 + 35 w% PbO formula was prepared using the Pechini method for powder preparation and two-step sintering in an oxygen atmosphere. Thr first step consisted of sintering at 1200 degrees C for 4 h with slow heating and cooling rates. The second step consisted of hot pressing at 1200 degrees C for 3 h, with slow heating and cooling rates and pressing pressures of 20 MPa (initial pressure) and 40 MPa (at sintering temperature). Investigations were made of the powder phase formation and powder morphology, i.e. The structure of sintered and hot-pressed PLZT ceramics. SEM microstructural analyses were carried out on the sintering and hot-pressing processes. (C) 2000 Elsevier B.V. Ltd and Techna S.r.l. All rights reserved.

Preparation of 9/65/35 PLZT thin films deposited by a dip-coating process

Crack-free polycrystalline PLZT (Pb,a)(Zr,Ti)O-3 thin films with the perovskite structure were prepared by dir-coating using the Pechinis process. Lead acetate, hydrated lanthanum carbonate, zirconium n-propoxide and titanium isopropoxide were used as raw materials. The viscosity of the solution was adjusted in the range of 20 to 56 cP and the films were deposited by a dip-coating process on silicon (100) as substrate. Solutions with ionic concentration of 0.1 and 0.2 M were used. Thin film deposition was accomplished by dipping the substrates in the solution with control of withdrawal speed from 5 to 20 mm/min. The thin films were thermally treated in two steps: at 300 degreesC amid 650 degreesC. The influence of withdrawal speed. viscosity, heating rate and ionic concentration on the morphology of PLZT thin film was discussed. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Effect of thermal treatment on the morphology of PLZT thin films prepared from polymeric precursor method

Lead lanthanum zirconate titanate (PLZT) thin films with (9/65/35) stoichiometry were prepared by dip coating from polymeric precursor method. The films deposited on silicon (100) substrates, were thermally treated from 450° to 700°C for 6 hours in order to study the influence of thermal treatment on the crystallinity, microstructure, grain size and roughness of the final film. X-ray diffraction results showed that PLZT phase crystallizes at low temperature (500°C) and present preferential orientation. It was observed by scanning electron microscopy (SEM) that it is possible to obtain dense thin films at temperatures around 650°C. The atomic force microscopy (AFM) studies showed that the grain size and roughness are strongly influenced by the annealing temperature.

Preparation of 9.5/65/35 PLZT powders by organic precursor method

In this study the preparation of 9.5/65/35 PLZT ceramic powders were investigated. The powders with the formula Pb0.905La0.095(Zr0.65 Ti0.35)0.976O3 + 3.5 w% PbO were prepared using Pechini process and partial oxalate method. The powder phase formation, powder morphology, and green density of PLZT were shown.

Síntese e propriedades físicas de filmes ferroelétricos do sistema PLZT

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Estabilização da fase perovskita e propriedades estruturais de filmes finos relaxores do sistema PLZT

Pós-graduação em Ciência dos Materiais - FEIS

Direct precipitation of lead zirconate titanate by the hydrothermal method

Direct precipitation of fine powders of lead zirconate titanate (PZT) in the complete range of solid solution, is investigated under hydrothermal conditions, starting from lead oxide and titania/zirconia mixed gels. The perovskite phase is formed in the temperature range of 165 – 340°C. Sequence of the hydrothermal reactions is studied by identifying the intermediate phases. The initial formation of PbO: TiO2 solid solution is followed by the reaction of the same with the remaining mixed gels giving rise to X-ray amorphous PZT phase. Further, through crystallite growth, the X-ray crystalline PZT is formed. This method can be extended for the preparation of PLZT powder as well. The resulting powders are sinterable to high density ceramics.

Energy principle of ferroelectric ceramics and single domain mechanical model

Many physical experiments have shown that the domain switching in a ferroelectric material is a complicated evolution process of the domain wall with the variation of stress and electric field. According to this mechanism, the volume fraction of the domain switching is introduced in the constitutive law of ferroelectric ceramic and used to study the nonlinear constitutive behavior of ferroelectric body in this paper. The principle of stationary total energy is put forward in which the basic unknown quantities are the displacement u (i) , electric displacement D (i) and volume fraction rho (I) of the domain switching for the variant I. Mechanical field equation and a new domain switching criterion are obtained from the principle of stationary total energy. The domain switching criterion proposed in this paper is an expansion and development of the energy criterion. On the basis of the domain switching criterion, a set of linear algebraic equations for the volume fraction rho (I) of domain switching is obtained, in which the coefficients of the linear algebraic equations only contain the unknown strain and electric fields. Then a single domain mechanical model is proposed in this paper. The poled ferroelectric specimen is considered as a transversely isotropic single domain. By using the partial experimental results, the hardening relation between the driving force of domain switching and the volume fraction of domain switching can be calibrated. Then the electromechanical response can be calculated on the basis of the calibrated hardening relation. The results involve the electric butterfly shaped curves of axial strain versus axial electric field, the hysteresis loops of electric displacement versus electric filed and the evolution process of the domain switching in the ferroelectric specimens under uniaxial coupled stress and electric field loading. The present theoretic prediction agrees reasonably with the experimental results given by Lynch.

基于光纤环形镜的偏振无关的掺镧锆钛酸铅电光开关

利用掺镧锆钛酸铅（PLZT）陶瓷二次电光效应结合光纤环形镜结构的优势构成偏振无关高速电光开关。采用琼斯矩阵方法分析了光纤环形镜的输出特性，给出了开关消光比同器件结构参量之间的关系。测量掺镧锆钛酸铅电光开关具有输入偏振无关特性，光开关消光比达到25dB，响应时间小于3μs。此外利用此开关装置测量获得了实验用掺镧锆钛酸铅陶瓷的克尔系数为k～1．1×10^-16m^2／V^2。理论分析和实验结果表明，利用环形镜结构稳定优势和掺镧锆钛酸铅优良的电光特性结合设计的高速光开关具有良好的应前景。本工作对掺镧锆钛酸铅电光

基于掺镧锆钛酸铅电光材料的光学相控阵光束扫描器

基于掺镧锆钛酸铅(PLZT)电光陶瓷材料的光学特性,提出了一种具有上下电极结构的光学相控阵高速光束扫描器。在理论上,分析了具有这种结构的光学相控阵的光束电光偏转特性和机制;在实验上,分析了掺镧锆钛酸铅材料的相位调制特性和损耗特性,制作了相关的光学相控阵器件,并构建了相应的测试系统,获得了光束在空间的角度偏转,与理论分析结果相符。