无机材料学报

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旋涂法制备纳米有机/无机复合膜成膜过程的研究

李琰; 潘庆谊; 张剑平; 程知萱; 陈海华   

  1. 上海大学理学院化学系 上海 200436
  • 收稿日期:2003-09-12 修回日期:2003-10-16 出版日期:2004-09-20 网络出版日期:2004-09-20

Preparation Process of Nanosized Organic/Inorganic Thin Films by Sol-Gel Spin-coating Method

LI Yan; PAN Qing-Yi; ZHANG Jian-Ping; CHENG Zhi-Xuan; CHEN Hai-Hua   

  1. Department of Chemistry; Shanghai University; Shanghai 200436; China
  • Received:2003-09-12 Revised:2003-10-16 Published:2004-09-20 Online:2004-09-20

摘要: 以醋酸镍为原料采用改进的溶胶-凝胶法制备了PEG6000/纳米Ni(OH)2复合溶胶,粘度法确定了溶胶的稳定区域,稳定溶胶有两种流型:牛顿体和假塑体.以稳定溶胶牛顿体配方采用旋涂法制备了纳米NiO薄膜.研究表明,在旋转涂膜过程中旋转角速度(ω)、旋涂液表观粘度(η)、纳米Ni(OH)2含量(M)是影响薄膜厚度(d)的主要因素,符合关系式:d=K((η0.74M2.1)/(ω0.54)) .溶胶的流变型影响薄膜质量:以牛顿体制备的薄膜表面较平整,而以假塑体制备的薄膜表面起伏不平. Ni(OH)2和PEG6000的相对含量主要影响薄膜表面孔隙度,Ni(OH)2含量低而PEG6000含量高,则薄膜表面纳米NiO粒子排列较为稀疏,反之则排列较为紧密.多次涂膜可得均匀致密的薄膜.

关键词: 纳米NiO, 薄膜, 溶胶-凝胶旋涂法, 溶胶流变学

Abstract: PEG6000/nano-Ni(OH)2 sol was prepared by a modified sol-gel method with Ni(Ac)2. The stable region of
the sol was definited by measuring the viscosity of the sol. Furthermore the flow patterns of the stable sol were studied and the results show that the
stable sol has two flow patterns: Newtonian and pseudoplastic fluid. With the Newtonian fluid of the stable sol, the nano-NiO thin films were produced
by the spin-coating method. The research results indicate that the thickness of the film (d) is largely determined by the factors including angular velocity
(ω), the apparent viscosity of the sol (η) and the content of Ni(OH)2(M) to the equation: d=K((η0.74M2.1)/(ω0.54)). The quality of the films is influenced
by the flow patterns and the content of PEG of the stable sol. The surfaces of the thin films with Newtonian sol are smooth while those
with pseudoplastic sol are rough and wavy. The surfaces of nano-NiO films with high content of Ni(OH)2 and low content of PEG6000 are compact and
dense while those with low content of Ni(OH)2 and high content of PEG6000 are loose.

Key words: nano-NiO, thin film, sol-gel spin-coating method, rheology

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