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Efficient sol-gel techniques for fabricating ferroelectric ceramic thin films of desired properties

用于制造具有所需性能的铁电陶瓷薄膜的高效溶胶-凝胶技术

基本信息

批准号：
13555243
负责人：
KOZUKA Hiromitsu
金额：
$ 9.02万
依托单位：
Kansai University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (B)
财政年份：
2001
资助国家：
日本
起止时间：
2001 至 2002
项目状态：
已结题

来源：
https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-13555243/
关键词：
Sol-gel method Ferroelectric materials Piezoelectric materials Thin films Barium titanate PZT Stress Film thickness

项目摘要

PZT thin films were prepared on silica glass substrates from Pb(CH_3COO)_2 - 3H_2O - Zr(OC_3H_<7^n>)_4 - Ti(OC_3H_<7^i>)_4 - H_2O - CH_3COOH - CH_3OC_2H_4OH - n-C_3H_7OH solutions containing polyvinylpyrrolidone (PVP) via non-repetitive dip- or spin-coating. It was found that PVP and CH_3COO- are thermally decomposed at 250°- 320℃, leaving carbonaceous species, followed by the crystallization of Pb_3(CO_3)_2(OH)_2 around 350℃. The oxidation of the carbonaceous species occurred at around 360°- 460℃, then perovskite PZT was formed around 550℃. The film thickness was found to decrease greatly at 200°- 350℃, where thermal decomposition of PVP and CH_3COO- occurred. The films fired at 700℃ were rather porous and not very transparent. Pre-heating the gel films at 100°or 200℃ resulted in particulate microstructure with gaps between the particles, and at 350℃ caused crack formation, both of which further reduced the optical transmittance.PZT, BaTiO_3 and BaBi_4Ti_4O_<15> films were prepared on … More Pt/Ti/SiO_2/Si substrates by spin-coating using alkoxide solutions containing polyvinylpyrrolidone (PVP). Deposition and firing of the gel films were performed just once, not repeated. Crack-free, single-phase PZT, BaTiO_3 and BaBi_4Ti_4O_<15> films as thick as 2.2, 0.77 and 0.40 μm could be prepared, respectively, via non-repetitive spin-coating. The 2.2 μm thick PZT film exhibited P-E hysteresis with remanent polarization and coersive field of 21 μC cm^<-2> and 90 kV cm^<-1>, respectively. The dielectric constant of the PZT, BaTiO_3 and BaBi_4Ti_4O_<15> films were 370, 310 and 380, respectively, at 1 kHz.An aqueous solution-based dip-coating technique was presented for ceramic thin film deposition. Organic polymers with amide groups such as polyvinylpyrrolidone, polyvinyl-acetamide and polyacrylamide, incorporated in aqueous solutions of metal salts, were demonstrated to offer much better wetting of the substrates and gel film formability. Transparent, crack-free TiO_2 and ZrO_2 thin films 0.07 - 0.1 μm in thickness could be obtained from aqueous solutions of Ti(SO_4)_2 and ZrCl_2O, respectively, containing these organic polymers. Less

以Pb(CH_3COO)_2 - 3H_2O - Zr(OC_3H_<7^n>)_4 - Ti(OC_3H_<7^i>)_4 - H_2O - CH_3COOH - CH_3OC_2H_4OH - n- c_3h_7oh为基材，采用不重复浸渍或旋涂法制备了PZT薄膜。结果表明，PVP和CH_3COO-在250°~ 320℃时发生热分解，生成碳质物质，在350℃左右发生Pb_3(CO_3)_2(OH)_2结晶。碳质组分在360°~ 460℃发生氧化反应，550℃左右形成钙钛矿PZT。在200°~ 350℃温度下，PVP和CH_3COO-发生热分解，膜厚明显减小。在700℃下烧制的薄膜多孔且不透明。凝胶膜在100°或200℃预热时，会形成颗粒间有间隙的微观结构，在350℃预热时，会形成裂纹，这两种现象都进一步降低了凝胶膜的透光率。采用含有聚乙烯吡罗烷酮（PVP）的醇盐溶液在…More Pt/Ti/SiO_2/Si衬底上旋涂，制备了PZT、BaTiO_3和BaBi_4Ti_4O_<15>薄膜。凝胶膜的沉积和烧制只进行一次，不重复。通过非重复自旋镀膜，可制得厚度分别为2.2、0.77和0.40 μm的无裂纹单相PZT、BaTiO_3和BaBi_4Ti_4O_<15>薄膜。2.2 μm厚的PZT薄膜表现出P-E迟滞现象，剩余极化值为21 μC cm^<-2>，外加外加场为90 kV cm^<-1>。在1 kHz时，PZT、BaTiO_3和BaBi_4Ti_4O_<15>薄膜的介电常数分别为370、310和380。提出了一种基于水溶液的陶瓷薄膜浸涂技术。具有酰胺基团的有机聚合物，如聚乙烯吡咯烷酮、聚乙烯乙酰胺和聚丙烯酰胺，掺入金属盐的水溶液中，可以提供更好的润湿性和凝胶膜的形成性。在Ti(SO_4)_2和ZrCl_2O的水溶液中分别制备了厚度为0.07 ~ 0.1 μm的透明无裂纹TiO_2和ZrO_2薄膜。少