钛酸钡系薄膜的制备及表征
摘要
钛酸钡系薄膜作为特殊形态的材料，已成为微电子、信息、传感器、光学、太等技术的基础，并广泛渗透到当前科技的各个领域。随着科学技术的发展，各种特殊用途对薄膜技术与薄膜材料的性质提出了各种各样的要求，如从尺寸上要求纳米级到微米级，从膜的结构上要求按特定方向取向的或外延生长的，从表面形貌上对表面凹凸也有极高要求等。为了满足实际应用中提出的要求，我们就必须反复实验，仔细研究，从而中获得膜系开发、工艺研究、设备研制、检测与机理研究等方面可喜成绩。
目前，见诸报道的钛酸钡系薄膜的制备方法主要有物理方法如射频磁控溅射、脉冲激光沉积和分子束外延等，化学方法如溶胶-凝胶法、有机金属化学气相沉积(MOCVD)法和水热法等。物理方法大多需要真空的工作环境，对仪器的要求比较高，一般的实验室难以达到其要求。而化学方法相对比较简单，不要求大型的仪器设备，化学法中溶胶-凝胶法由于具有组分均匀、组，其过程是将金属有机物或无机化合物经过水解与缩聚过程形成溶胶，进而逐渐成精确、烧结温度低、易操作等优点是目前制备BaTiO_3系薄膜中最常用的方法凝胶化，再经热处理形成氧化物或化合物固体的方法。大部分文献报道都是采用了溶胶-凝胶工艺制BaTiO_3薄膜。
本文的主要研究内容包括
(1) 稳定溶胶的合成
为了制备优良的钛酸钡系薄膜合成透明稳定的溶胶是非常重要的一步，本文在参阅大量文献的基础上，分别考察了不同溶剂、加水量、加醋酸量、添加螯合剂及溶胶的浓度不同时对溶胶稳定性及薄膜表面形貌的影响。找到了合成稳定溶胶及具有优良表面形貌的最佳条件。
(2) 钛酸钡薄膜的制备与表征
钦酸钡系薄膜的制备与表征
根据我们所选定最佳合成条件制备钦酸钡薄膜，并结合差热一热重
(DTA一TGA)、红外(IR)、X射线衍射(XRD)、扫描电子显微镜(SEM)等
表征手段选择薄膜热处理及退火温度，借助原子力显微镜(AFM)我们可以初
步得到钦酸钡薄膜晶粒生长的一些信息:锻烧退火过程即薄膜的晶化过程是一
个晶粒成核、长大、分裂、吞噬、再生长的过程。这对我们选择退火温度具有
指导意义。
(3)钦酸锯钡薄膜的制备
在这部分内容我们借助XRD、AFM表征手段考察了铭掺杂对结晶温度的
影响，以及随着铭含量的增加，晶胞参数，粒径的变化趋势。从理论上对这种
变化趋势加以说明。
BaTiO3-based thin film as a special material has penetrated into many parts of the science field land it has already been a basic tech for the microelectronics communication, sensor, optics. Along with the development of the Technology, various demands are put forward for the tech and quality of the thin film. They demand the size from u m to nm, of the structure they demand special direction or heteroepitaxial .There are also strict demands on morphology. In order to satisfy the desire we should do more research and get the achievement on development, research, and examine accordingly.
Recently, the preparation of BaTiOa-based thin film are reported .There are physical methods such as radio-frequency magnetron sputtering, pulsed laser deposition, MBE and chemical methods such as Sol-Gel, metallorganic chemical vapor deposition (MOCVD), hydrothermal and so on .Generally, the physical methods need vacuum environment, they are so strict to the apparatus that current laboratory can hardly achieve it. Compared with physical tech the chemical tech is easier. They do not need large equipments. For example, the Sol-Gel processing are better homogeneity. The whole course is to make metal organic or inorganic matter hydrolyze and purse up to sol and then use thermal treatment make it oxide or compound. As it has advantage in accurate, low sinter temperature, stoichiometry control, this processing has become widely used. Much literatures has reported to prepare BaTiO3-based on the Sol-Gel method.
The main content in this paper includes: (1) The synthesization of stable sol To synthesize transparent and stable sol for BST thin film is a very important
step. Based on many literatures we did some research on different solutions, water, HAC, chelating matter dosage respectively and the impact of different sol concentration on the sol stabilization and the morphology. We get the optimum condition here.
(2) The preparation and properties of BST thin films
According to the optimum condition which we have chosen to synthesize the BST thin film and the DTA-TGA, IR, XRD, SEM as functions of thermal treatment and anneal- temperature. By using AFM we can get some information about the growing grains: calcine- anneal is a process of thin film crystallization .That is nucleatio, growing, cleavage, swallow, regeneration. Here the anneal- temperature we chose is of some guidance significance.
(3)The preparation of BST thin films
In this part, the XRD and AFM methods are used to discuss the Sr-doped impact to the crystallization temperature The growing trend of the grain-size, the lattice parameter with the increased strontium concentration are also discussed in theory.
目前，见诸报道的钛酸钡系薄膜的制备方法主要有物理方法如射频磁控溅射、脉冲激光沉积和分子束外延等，化学方法如溶胶-凝胶法、有机金属化学气相沉积(MOCVD)法和水热法等。物理方法大多需要真空的工作环境，对仪器的要求比较高，一般的实验室难以达到其要求。而化学方法相对比较简单，不要求大型的仪器设备，化学法中溶胶-凝胶法由于具有组分均匀、组，其过程是将金属有机物或无机化合物经过水解与缩聚过程形成溶胶，进而逐渐成精确、烧结温度低、易操作等优点是目前制备BaTiO_3系薄膜中最常用的方法凝胶化，再经热处理形成氧化物或化合物固体的方法。大部分文献报道都是采用了溶胶-凝胶工艺制BaTiO_3薄膜。
本文的主要研究内容包括
(1) 稳定溶胶的合成
为了制备优良的钛酸钡系薄膜合成透明稳定的溶胶是非常重要的一步，本文在参阅大量文献的基础上，分别考察了不同溶剂、加水量、加醋酸量、添加螯合剂及溶胶的浓度不同时对溶胶稳定性及薄膜表面形貌的影响。找到了合成稳定溶胶及具有优良表面形貌的最佳条件。
(2) 钛酸钡薄膜的制备与表征
钦酸钡系薄膜的制备与表征
根据我们所选定最佳合成条件制备钦酸钡薄膜，并结合差热一热重
(DTA一TGA)、红外(IR)、X射线衍射(XRD)、扫描电子显微镜(SEM)等
表征手段选择薄膜热处理及退火温度，借助原子力显微镜(AFM)我们可以初
步得到钦酸钡薄膜晶粒生长的一些信息:锻烧退火过程即薄膜的晶化过程是一
个晶粒成核、长大、分裂、吞噬、再生长的过程。这对我们选择退火温度具有
指导意义。
(3)钦酸锯钡薄膜的制备
在这部分内容我们借助XRD、AFM表征手段考察了铭掺杂对结晶温度的
影响，以及随着铭含量的增加，晶胞参数，粒径的变化趋势。从理论上对这种
变化趋势加以说明。
BaTiO3-based thin film as a special material has penetrated into many parts of the science field land it has already been a basic tech for the microelectronics communication, sensor, optics. Along with the development of the Technology, various demands are put forward for the tech and quality of the thin film. They demand the size from u m to nm, of the structure they demand special direction or heteroepitaxial .There are also strict demands on morphology. In order to satisfy the desire we should do more research and get the achievement on development, research, and examine accordingly.
Recently, the preparation of BaTiOa-based thin film are reported .There are physical methods such as radio-frequency magnetron sputtering, pulsed laser deposition, MBE and chemical methods such as Sol-Gel, metallorganic chemical vapor deposition (MOCVD), hydrothermal and so on .Generally, the physical methods need vacuum environment, they are so strict to the apparatus that current laboratory can hardly achieve it. Compared with physical tech the chemical tech is easier. They do not need large equipments. For example, the Sol-Gel processing are better homogeneity. The whole course is to make metal organic or inorganic matter hydrolyze and purse up to sol and then use thermal treatment make it oxide or compound. As it has advantage in accurate, low sinter temperature, stoichiometry control, this processing has become widely used. Much literatures has reported to prepare BaTiO3-based on the Sol-Gel method.
The main content in this paper includes: (1) The synthesization of stable sol To synthesize transparent and stable sol for BST thin film is a very important
step. Based on many literatures we did some research on different solutions, water, HAC, chelating matter dosage respectively and the impact of different sol concentration on the sol stabilization and the morphology. We get the optimum condition here.
(2) The preparation and properties of BST thin films
According to the optimum condition which we have chosen to synthesize the BST thin film and the DTA-TGA, IR, XRD, SEM as functions of thermal treatment and anneal- temperature. By using AFM we can get some information about the growing grains: calcine- anneal is a process of thin film crystallization .That is nucleatio, growing, cleavage, swallow, regeneration. Here the anneal- temperature we chose is of some guidance significance.
(3)The preparation of BST thin films
In this part, the XRD and AFM methods are used to discuss the Sr-doped impact to the crystallization temperature The growing trend of the grain-size, the lattice parameter with the increased strontium concentration are also discussed in theory.
引文
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2、孙一军，张良莹，姚熹。BaTiO_，薄膜的MOCVD方法制备及进展，硅酸盐通报，1998年第2期，34-38。
3、崔大复，王会生，马昆等。激光分子束外延及其在分子水平生长BaTiO_3薄膜中的应用，量子电子学，1996年，13(5)：404。
4、Hu-Yong Tian, Wei-Gen luo,Ai-Li Ding,et al. Influences of annealing temperature on the optical and structural properties of (Ba,Sr)tio3 thin films derived from sol-gel technique,Thin Solid Films 408(2002):200-205.
5、Tian-Ling Ren, Xiao-Ning Wang ,Jian-She Liu,et al,Characteristics of silicon-based Ba_xSr_(1-x)TiO_3 thin films prepared by a sol-gel method,Journal of physics D:Appled Physics,35(2002):923-926.
6、C.B.Parker, J.-P.Maria,and A.L.Kingon,Temperature and thickness dependent permittivity of (Ba,Sr)TiO_3 thin films,Appled physics letters,2002,81(2):86-88.
7、丁星兆 董远达。溶胶-凝胶薄膜工艺及其应用，材料导报，1993，NO。3，32-36。
8、M.N.Kamalasanan et al.Dielectric and ferroelectric properies of BaTiO_3 thin films grown by the sol-gel process,J.Appl.phys, 1993, 74(9):5679-5685.
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