铟锡氧化物纳米微粒表面修饰研究及其悬浮液的制备
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摘要
纳米氧化铟锡[In2O3(SnO2)]是一种N型半导体材料,以其良好的电导、透光性能而成为电子行业显示器、显像管防静电、防辐射、防眩目的热点材料。传统的制备ITO膜方法是真空溅射法,但该方法所需设备复杂,工序多,成本高,而ITO粉体为基的涂膜技术为下一代的印刷电路、导电薄膜制备提供了新的思路。因此,如何制备ITO纳米悬浮液及保持其稳定性成为应用过程中研究重点。
本文采用物理和化学改性的方法,分别用阴离子表面活性剂、阳离子表面活性剂、非离子表面活性剂、高分子表面活性剂和硅烷偶联剂对铟锡氧化物进行表面修饰以改进其悬浮液的稳定性；采用红外光谱(IR)、X射线电子能谱(XPS)、透射电镜(TEM)和分散性实验等手段对表面改性后的纳米铟锡氧化物进行分析表征,并且试验了不同用量的表面活性剂对ITO纳米悬浮液稳定性的影响,3%-4%的用量可以达到最佳的分散效果；对试验条件进行优化,在最佳条件下成功地制备了能稳定存在的ITO纳米悬浮液。
对表面修饰后的ITO纳米悬浮液涂膜进行光学和电学性质的测试,改性后的ITO薄膜透光率变化不大,但导电性质相差悬殊；经试验得出,聚乙烯吡咯烷酮既可以使纳米铟锡氧化物悬浮液稳定性良好,又不影响其电学性质,是最佳的表面活性剂。
Nanoparticles Indium tin oxide [In2O3 (SnO2)] that is an N type semiconductor is an anti-static, radiation protection and anti-glare hotspot material in the electronic industry because of good electroconductibility and optical transmittance. ITO films are synthetized by vaccum sputtering. However the traditionally method is complex equitment, too many procedures and high cost. And ITO suspension is a new method that is for the future printed circuit and conductive films. Now it is an important that the dispersibility of ITO suspension in the application of nanosized-ITO powders.
The paper had a general introduction in modifical mechaniam. Physical and chemical modifications were used to modify the nanosized indium-tin-oxide in the experience. And the effects of improvement the stability of nano-ITO suspention that used different of surfactants were studied including anionic surfactants, cationic surfactants, non-ionic surfactants, high polymer surfactants and silicon surfactants. The microstructural changes were analysed after surface modification by means of infrafed spectra, X-ray photoelectron spectroscopy, transmission electron microscope and dispersity tests. The paper introduced the effect of various surfactants addition on the dispersion property of nanometer ITO powders, and the 3%-4% is best. Experience conditions were tested and the ITO suspension was stable on the optimum conditions of the mearsurement.
The optical property and electrical property of ITO films were tested. The optical transmittance of surface modification ITO films is no changes, but the electronic conduction is augmented. The results showed that PVP is the best surfactant that is not only improved the dispersibility of suspension but also not affected the conduction of ITO films.
本文采用物理和化学改性的方法,分别用阴离子表面活性剂、阳离子表面活性剂、非离子表面活性剂、高分子表面活性剂和硅烷偶联剂对铟锡氧化物进行表面修饰以改进其悬浮液的稳定性；采用红外光谱(IR)、X射线电子能谱(XPS)、透射电镜(TEM)和分散性实验等手段对表面改性后的纳米铟锡氧化物进行分析表征,并且试验了不同用量的表面活性剂对ITO纳米悬浮液稳定性的影响,3%-4%的用量可以达到最佳的分散效果；对试验条件进行优化,在最佳条件下成功地制备了能稳定存在的ITO纳米悬浮液。
对表面修饰后的ITO纳米悬浮液涂膜进行光学和电学性质的测试,改性后的ITO薄膜透光率变化不大,但导电性质相差悬殊；经试验得出,聚乙烯吡咯烷酮既可以使纳米铟锡氧化物悬浮液稳定性良好,又不影响其电学性质,是最佳的表面活性剂。
Nanoparticles Indium tin oxide [In2O3 (SnO2)] that is an N type semiconductor is an anti-static, radiation protection and anti-glare hotspot material in the electronic industry because of good electroconductibility and optical transmittance. ITO films are synthetized by vaccum sputtering. However the traditionally method is complex equitment, too many procedures and high cost. And ITO suspension is a new method that is for the future printed circuit and conductive films. Now it is an important that the dispersibility of ITO suspension in the application of nanosized-ITO powders.
The paper had a general introduction in modifical mechaniam. Physical and chemical modifications were used to modify the nanosized indium-tin-oxide in the experience. And the effects of improvement the stability of nano-ITO suspention that used different of surfactants were studied including anionic surfactants, cationic surfactants, non-ionic surfactants, high polymer surfactants and silicon surfactants. The microstructural changes were analysed after surface modification by means of infrafed spectra, X-ray photoelectron spectroscopy, transmission electron microscope and dispersity tests. The paper introduced the effect of various surfactants addition on the dispersion property of nanometer ITO powders, and the 3%-4% is best. Experience conditions were tested and the ITO suspension was stable on the optimum conditions of the mearsurement.
The optical property and electrical property of ITO films were tested. The optical transmittance of surface modification ITO films is no changes, but the electronic conduction is augmented. The results showed that PVP is the best surfactant that is not only improved the dispersibility of suspension but also not affected the conduction of ITO films.
引文
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2 毋伟,陈建峰,卢寿慈编著.超细粉体表面修饰[M].北京：化学工业出版社,2004.
3 沈钟,赵振国,王国庭编著.胶体与表面化学[M].北京：化学工业出版社,2004,94-96.
4 郭俊颉.利用RF溅镀技术于室温下将ITO成长在塑胶基板上之研究[D].国立中山大学,1994,
5 晋传贵,裴立宅,俞海云.一维无机纳米材料[M].北京：冶金工业出版社,2007.
6 Yoshizawa, et al. New Fe-based soft magnetic alloys composed of ultrafine grain structure. J.Appl.Phys.,1988,10:6044.
7 孙晓霞.纳米ITO粉体的制备及其分散性研究[D].武汉理工大学,2005,2-4.
8 毛黎明.纳米ITO粉体与浆料的制备及其性能[D].中南大学,2005,1-2.
9 洪文进,徐登贵,万明安等.ITO透明导电薄膜：从发展与应用到制备与分析[J].CHEMISTRY,2005,63(3)：409-418.
10 职利,周怀营.ITO薄膜的制备方法与应用[J].桂林电子工业学院学报,2004,24(6)：54-57.
11 Kim S S, Choi S Y, Park C G P, et al. Transparent conductive ITO thin films through the sol-gel process using metak salt [J]. Thin Solid Films,1999,347(1,2):155-160.
12 Liu J M, Lu P Y, Weng W K. Studies on modification of ITO surfaces in OLED devices by Taguchi methods[J]. Material Science Engineer B,2001,85(2):209-211.
13 Card C P, Jamea K M G, Philip G H. Aqueous Sol-gel Routes to Conducting Films of Indium Oxide and Indium Oxide[J]. Sol-Gel Optics,2000,3943:270-279.
14 Mason M G, Hung L S, Tang C W, et al. Characterization of treated indium-tin-oxide surfaces used in electroluminescent devices [J]. J Appl Phys,1999,86(3):1688-1692.
15 Y Wang, N Toshuman. Preparation of Pd-Pt Bimetallic Colloids with Controllable Core/Shell Structures [J]. Phys Chem B,1997,101:5301.
16 林丽梅,赖发春,林永钟等.热处理对直流磁控溅射ITO薄膜光电学性质的影响[J].福建师范大学学报(自然科学版),2006,22(3)：42-46.
17 Toshiro Maruyama and Kunihiro Fukui. Indium tin oxide thin films prepared by chemical vapour deposition [J]. Thin Solid Films,1991,203(2):297-302.
18 Vasu V and Subrahmanyam A. Reaction kinetics of the formation of indium tin oxide films grown by spray pyrolysis [J]. Thin Solid Films,1990,193(1):696-703.
19 欧宝立,李笃信.无机纳米粒子表面修饰[J].高分子材料科学与工程,2008,24(5)：1-5..
20 徐涛,杨静晖,傅强.等离子体处理碳纳米管的研究现状及展望[J].物理学进展,2008,28(1)：78-82.
21 MATHEW G, HUH M Y, RHEE j M, et al. Improvement of properties of silica filled styrene-butadiene rubber compos ites through plasma surface modification of silica[J]. Polymers for Advanced Technologies,2004,15(7):400-408
22 王德生.等离子体处理玻璃纤维布对其环氧复合材料性能的影响[J].化学与粘合.1990,4：216.
23 崔黎黎,范慧俐,肖军等.纳米材料表面修饰的研究[J].材料导报,2006,20(专辑Ⅵ)：5-7.
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