【作者】 刘红梅；

【导师】 曹茂盛；

【作者基本信息】 哈尔滨工程大学 ， 材料物理与化学， 2005， 硕士

【摘要】 由于电子技术、信息技术和控制技术的发展,器件的小型化和集成化,对材料提出了新的要求。PZT薄膜因其优良的压电性能、热电性能、铁电性能、光电性能和介电性能以及易与半导体技术集成等特点已成为国际上功能材料和器件的新热点。PZT薄膜广泛应用于微电子学、光电子学、集成光学和微电子机械系统等领域,特别是PZT压电薄膜作为微传感及驱动器件应用时的高灵敏度和高输出应变的特点,使其成为微机电系统（MEMS）最有前途的候选材料。 溶胶-凝胶法制备PZT薄膜是近年来发展起来的一种方法,利用此法获得的薄膜结构致密、成分准确且性能优于用其他方法得到的薄膜。因此,目前在MEMS微机电系统中,溶胶-凝胶法制备PZT铁电薄膜是广泛应用的方法。然而,由于受到无裂纹单层最大厚度难以超过120nm的限制,用Sol-Gel法制备的PZT薄膜总厚度一般不大于2μm。因此,在传统Sol-Gel方法基础上发展了一种改进的0-3复合法,即先将0维的PZT超细粉末混合到的PZT前驱液中,形成均匀、稳定的浆料,然后进行甩胶成膜的方法。它主要针对2～10μm,甚至10μm以上的PZT厚膜的制备,0-3复合法具有设备简单、制备薄膜厚度大、重复性好的优点。 为了采用0-3复合法制备PZT薄膜,本文先采用Sol-Gel法,制备了PZT微粉。经过大量的实验研究并结合粉体制备技术分析,掌握了利用无机盐原料及单一金属醇盐制备完全钙钛矿结构PZT微粉的优化工艺。通过XRD分析确定热处理最佳工艺条件是650℃处理2h,可得到完全的钙钛矿相,经过SEM分析测试,表明实验制备的粉体晶粒分布均匀,粒径在100nm左右。 在传统Sol-Gel法基础上,本文提出一种改进Sol-Gel法,在Au/Ti/SiO₂/Si结构上制备了PZT铁电薄膜。采用PZT溶胶与在PZT溶胶中加入PZT微粉形成的浆料并交替涂覆薄膜的方法。所获得薄膜表面平整、无裂纹,厚度为2μm。经多次重复后,还可以提高PZT薄膜的厚度。采用此方法制备的薄膜厚度大、突破了PZT薄膜的厚度的限制,并且重复性好、使PZT薄膜表面质量得到改善。更多还原

【Abstract】 With the development of electron, information, and control technology, the characteristic of miniaturization and integration of devices demands new materials. The PZT film has become a new hot issue of functional materials and devices in the world due to its excellent performance of piezoelectricity, thermoelectricity, ferroelectric, photovoltaic and dielectric and the characteristic of integration with semiconductor process. PZT film is widely applied to the fields of microelectronics and optoelectronics, integrated photics and MEMS etc. And the characteristics of PZT film-high sensitive and high output strain make it a most promising material of drive devices in MEMS.In recent years, Sol-Gel method, which can produce excellent PZT films with close-knit structure, precise component and superior performance, is one of the newly developed methods in PZT film preparation. Therefore, Sol-Gel method has been widely applied to producing PZT ferroelectric film in modern MEMS so far. But the whole thickness of PZT film made by Sol-Gel method is not more than 2μm thickness, because the maximum thickness of no-crackle single layer can not exceed 120μm. As to 2~10μm or over 10μm, a better 0-3 compound method is developed on the base of the conventional Sol-Gel method preparation. By using 0-3 compound method, first we put 0 dimension PZT superfine mineral powder into 3 dimension PZT premonitory solution to get the equable and steady slurry, and then spin the shurry to form membrane. The 0-3 compound method has many merits, such as using simple equipment, thick enough film and good repetition.In this paper, the author analyze how to use Sol-Gel method to produce PZT micro-powder. With a lot of researches and analysis of technology of producing powder, we have grasped optimize method which can be used to produce Perovskite structure PZT micro-powder with abiosalt as raw material and single metal alcohol salt. The best technics condition is identified by XRD: 2 hours’ annealing under 650 ℃ degree. In that case, we can get the Perovskite structure.SEM has established that the powder particle in the experiment is well-distributed and the diameter is about 100um.In the paper we present an improved Sol-Gel method, on the base of traditional Sol-Gel method we produce PZT ferroelectric membrane on a configuration of Au/Ti/SiO2/Si. we present a method-covering PZT Sol-Gel and the slurry mixed PZT powder on the membrane alternately. The surface of membrane is flat and no crackle with the thickness of 2μm. After repeating it several times, the PZT membrane can become thicker and thicker. By using this method, the thickness of membrane is increased. The method breaks the limitation of thickness, has the good property of repetition and has improved the quality of PZT membrane surface.We have made test and analysis on the electric properties of PZT membrane, which shows that symmetry of hysteresis loops is good, the corresponding nonlinear polarization Pr=50uC/cm2, coercivity Ec=50Kv/cm respectively. The surplus dielectric constant of PZT membrane decreases with the increase of frequency which is tested is up to ε r=1080, loss tangent tanδ=0.05. It indicates the PZT membrane owns excellence dielectric and ferroelectric property.Therefore, the PZT membrane obtained by 0-3 compound method has a lot of advantages, such as even flawless and good repetition. This method also raises the maximum thickness of single-layer PZT membrane. We can raise the total film thickness as a result of continuous repetition. In MEMS, the PZT membranes made by this method overcome the limitation of the film thickness.更多还原