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Study on the stress generation during gel/ceramic thin film conversion

凝胶/陶瓷薄膜转化过程中应力产生的研究

基本信息

批准号：
12650679
负责人：
KOZUKA Hiromitsu
金额：
$ 2.3万
依托单位：
Kansai University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
2000
资助国家：
日本
起止时间：
2000 至 2001
项目状态：
已结题

来源：
https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-12650679/
关键词：
Sol-gel method Ferroelectrices Piezoelectric materials Thin film Barium titanate PZT Stress Film thickness

项目摘要

1 Silica and titania gel films were deposited on silicon wafers by sol-gel method using alkoxide-derived sols as the coating solutions. The gel films were heated at constant rates in an infrared furnace up to 800℃, and in situ observation was made using an optical microscope. The cracking was found to occur during the heating-up stage, and the cracking onset temperature was lower than that of crystallization. The cracking onset temperatures were found to decrease with increasing initial film thickness and with decreasing heating rate.2 BaTiO_3 thin films were deposited on silica glass and MgO single crystal substrates by sol-gel dip-coating using an alkoxide solutions containing polyvinylpyrrolidone (PVP) as the coating solution. SEM observation revealed that the fihns deposited on the silica glass substrates have microcracks propagating along grain boundaries. On the other hand, no microcracks were found on the films deposited on the MgO single crystal substrates, The microcracks obse … More ived are supposed to be formed by tensile stress in films, which is thought to be generated as a result of the thermal expansion coefficient mismatch between the film and the substrates.3 Titania thin fihns were deposited on silica glass substrates by sol-gel method using alkoxide solutions containing diethanolamine, acetylacetone or acetic acid as the chelating agents. The stress in the fired films were measured by measuring the substrate bending, and the effect of the chelating agent on the stress. The stress was tensile, increasing in the order of acetic acid < acetylacetone < diethanolarnine. The effect of the chelating agent on the stress was interpreted in terms of the difference in the degree of film densification.4 BaTiO_3, Fe_2O_3 and PZT thin films were deposited on silica glass substrates using alkoxide or metal salt solutions containing PVP as the coating solutions. The critical thickness, the maximum thickness achievable without cracking via single-step deposition was found to increase by incorporating PVP in solutions, showing maximum around mole ratios of PVP/Ti(OC_3H_7^i)_4 = 0.5, PVP/Fe(N0_3)_3 = O and PVP/ (Ti(OC_3H_7^i)_4 + Zr(OC_3H_7^n)_4) for BaTiO_3, Fe_2O_3 and PZT films, respectively. Less

1 使用醇盐衍生溶胶作为涂层溶液，通过溶胶-凝胶法在硅片上沉积二氧化硅和二氧化钛凝胶薄膜。将凝胶膜在红外炉中以恒定速率加热至800℃，并使用光学显微镜进行原位观察。发现裂纹发生在升温阶段，且裂纹起始温度低于结晶温度。发现裂纹起始温度随着初始膜厚的增加和加热速率的降低而降低。2以聚乙烯吡咯烷酮(PVP)的醇盐溶液为涂层溶液,采用溶胶-凝胶浸涂法在石英玻璃和MgO单晶基底上沉积BaTiO_3薄膜。 SEM观察表明沉积在石英玻璃基底上的薄膜具有沿晶界扩展的微裂纹。另一方面，在 MgO 单晶基底上沉积的薄膜上没有发现微裂纹，观察到的微裂纹被认为是由薄膜中的拉应力形成的，这被认为是由于薄膜和基底之间的热膨胀系数不匹配而产生的。 3 使用醇盐溶液通过溶胶-凝胶法在石英玻璃基底上沉积二氧化钛薄膜含有二乙醇胺、乙酰丙酮或乙酸作为螯合剂。通过测量基板弯曲以及螯合剂对应力的影响来测量烧制膜中的应力。应力是拉伸的，按乙酸 < 乙酰丙酮 < 二乙醇胺的顺序增加。螯合剂对应力的影响可以通过薄膜致密化程度的差异来解释。4以含有PVP的醇盐或金属盐溶液为镀膜溶液,在石英玻璃基板上沉积BaTiO_3、Fe_2O_3和PZT薄膜。发现通过在溶液中加入 PVP 可以增加临界厚度，即通过单步沉积可实现的不开裂的最大厚度，显示出 PVP/Ti(OC_3H_7^i)_4 = 0.5、PVP/Fe(N0_3)_3 = O 和 PVP/ (Ti(OC_3H_7^i)_4 + BaTiO_3、Fe_2O_3 和 PZT 薄膜分别为 Zr(OC_3H_7^n)_4)。较少的