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压电薄膜材料制备与性能研究

Study on Preparation and Properties of Piezoelectric Thin Films

作者:龚文
  • 学号
    2001******
  • 学位
    博士
  • 电子邮箱
    gw9******.cn
  • 答辩日期
    2005.12.20
  • 导师
    李龙土
  • 学科名
    材料学
  • 页码
    155
  • 保密级别
    公开
  • 馆藏号
    D06035-25
  • 培养单位
    035 材料系
  • 中文关键词
    压电;铁电;薄膜;锆钛酸铅;溶胶-凝胶
  • 英文关键词
    Piezoelectric;Ferroelectric;lead zirconate titanate;thin films;sol-gel method

摘要

压电薄膜材料的研究是目前信息功能陶瓷材料研究的前沿领域。本论文主要以锆钛酸铅(PZT)体系为研究对象,系统研究了溶胶-凝胶法制备PZT薄膜的制备与性能,并提出了PZT一维微结构的制备方法。采用溶胶-凝胶法以金属醇盐为主要原料制备了PZT压电薄膜。发展了激光扫描测振法和AFM导电探针法测量薄膜的纵向压电常数d33,提出了采用三点弯曲法测量薄膜的横向压电常数e31,f。同时对PZT的铁电性能、介电性能进行了评价。研究了热解工艺和退火制度对薄膜取向性的影响,实验表明通过选择一定的热解温度与退火时间能大幅度提高薄膜的择优取向性。采用在界面处加入PbO晶种层的方法制备了完全[100]择优取向的PZT薄膜。PZT在-PbO晶粒的表面形核生长并继承了其择优取向,得到完全[100]择优取向的PZT薄膜。同时采用金红石结构的TiO2晶种层的方法制备了完全[111]择优取向的PZT薄膜。比较了PZT薄膜的择优取向对薄膜介电、铁电、压电性能的影响。采用溶胶-凝胶法制备了高度[100]择优取向的PMN-PT薄膜,薄膜的纵向压电常数值d33高达114 pC/N,在12.5V电压下的应变量为0.5 %。研究了KNN无铅压电薄膜的溶胶-凝胶法制备,并通过工艺改善制备了有较好铁电性能的KNN薄膜。在STO单晶基片上用溶胶-凝胶法制备了PZT外延薄膜。发现STO衬底不仅决定了PZT薄膜生长取向,同时影响了薄膜的晶体结构。在导电的Nb:STO基片上制备了Nb:PZT外延薄膜,测量了薄膜的电学性能。首次采用Au颗粒限制PZT在STO(100)表面的二维生长的方法制备了PZT带状微晶。该一维材料的制备方法不仅仅局限于制备PZT材料,而且适用于各种无机氧化物材料,只要选择合适的衬底材料与阻挡颗粒物就能生长出类似的一维微结构。

Piezoelectric thin films are the frontier of functional materials for their outstanding ferroelectric and piezoelectric properties. This dissertation mainly focuses on the lead zirconate titanate (PZT) system. The sol-gel method and electric properties of the films were studied systematically, and a novel method was proposed to prepare the PZT one dimensional microstructures. PZT piezoelectric thin films were prepared by a sol-gel method, in which metal alkoxides were used as the raw materials. A laser scanning vibrometer and an atomic force microscopy were used to evaluate the longitudinal piezoelectric coefficient d33, respectively. A simple static 3-point bending test was developed to measure the transverse piezoelectric coefficient e31. The texture dependency on the pyrolysis process and the annealing system were studied. The experimental results proved that the texture of the PZT films could be improved by proper processing parameters. The lead oxide seeding layer on the interface of the PZT film and the substrate results in the formation of a single-phase perovskite and absolutely (100)-textured PZT film. The epitaxial growth of perovskite PZT on PbO inherit the texture of the PbO。The similar method was used to prepare the (111)-textured PZT thin films by introducing rutile TiO2 seeing layer to the interface. The dielectric, ferroelectric, and piezoelectric properties of the PZT films with different texture were studied. Highly (111)-textured PMN-PT thin films were prepared by sol-gel method. The longitudinal piezoelectric coefficient of the PMN-PT thin film is as high as 114 pC/N. The strain is 0.5 % under the voltage of 12.5 V. Lead-free KNN thin films were also prepared by a sol-gel method. Epitaxial PZT thin films were deposited on the SrTiO3 (STO) single crystal wafers with different orientations. It is note that not only the texture of the PZT thin films but also the crystal structure were determined by the substrates. Property measurements were conducted to the Nb doped PZT thin films on Nb doped STO wafers. One dimensional PZT microbelts were prepared by a novel method, in which gold particles restrict the 2D growth of the PZT on STO(100) wafers, resulting the belt-like microstructures. This method is not limited to a specified material, but is also applicable to other kinds of oxides on appropriate substrates, especially to complex oxides with precisely controlled stoichiometric proportions.