ZnO功能化薄膜的制备及性能研究
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摘要
本文主要研究氧化锌功能化薄膜的湿化学法制备工艺、显微形貌和性能关系。以乙酸锌、硝酸锌、氢氧化钠、六亚甲基四胺和聚乙二醇等为原料,采用化学溶液沉积法、水热合成法和电泳沉积法构筑具有疏水性的氧化锌薄膜材料。利用XRD分析薄膜的晶体结构和化学组成;利用SEM观测薄膜的显微结构、晶粒大小及形态;利用拉曼光谱分析Co2+掺杂前后微结构的变化,并研究薄膜材料的结构与疏水性能等之间的关系。所得氧化锌薄膜经硅烷偶联剂处理后与水的接触角可达到165°。本文的研究主要包括以下内容:
(1)化学溶液沉积法制备氧化锌纳米棒阵列膜。研究缓冲层厚度、氢氧化钠浓度、反应速度及反应温度等条件对氧化锌薄膜形貌的影响。结果表明,增加ZnO缓冲层厚度(六层对比两层)可以提高衬底的均匀性以及缓冲层的结晶性,使ZnO纳米棒更多的沿c轴方向生长。氢氧化钠浓度的提高使得溶液pH值增大,导致ZnO纳米棒生长得更细更致密。化学反应速度的提高显著降低了纳米棒的均匀度和规则性。沉积时间为75mins所得氧化锌薄膜经硅烷偶联剂处理后与水的接触角可达到165°。
(2)水热法制备氧化锌阵列膜。研究缓冲层基底及六亚甲基四氨、乙酸钴含量等对合成薄膜的影响。当六亚甲基四氨浓度为0.1M时,水热合成的氧化锌纳米棒生长致密,沿c轴的取向性较好。以乙酸锌为原材料合成的氧化锌缓冲层薄膜比较致密、均匀,晶粒较小,因而水热合成的氧化锌阵列膜的取向度较高。Co2+的掺杂改变了各晶面的生长速度,降低了氧化锌阵列膜沿c轴的择优生长,导致正六角棒状结构的对称性降低,甚至出现开裂。
(3)电泳沉积法制备氧化锌薄膜。以片式颗粒的悬浮液为电泳液,研究电流强度、沉积时间和缓冲层对薄膜的晶相、显微结构、透光度和润湿性的影响。结果表明:电流强度对薄膜的形貌影响较大,当沉积电流较小时,片状颗粒平铺在ITO基片上;当沉积电流较大时,片状颗粒垂直于基片排列,所得薄膜由纳米尺度的网状结构以及微米尺度的球状物组成。ZnO缓冲层显著改善了薄膜的均匀性。低温热处理可大大提高ZnO薄膜的比表面积,对进一步改善其疏水性和气敏性十分有利。
The fabrication processes, microstructure and properties of ZnO functionalized films are investigated. Hydrophobic ZnO films are constructed by chemical solution deposition (CSD), hydrothermal method and electrophoretic deposition, respectively, with zinc acetate, zinc nitrate, NaOH, urotropine and Polyethylene Glycol (PEG) as raw materials. Crystal structure and chemical composition of ZnO films are analyzed by XRD. Microstructure, grain size and morphology are observed by SEM. Microstructural variation resulting from Co2+ dopants is studied by Laman spectroscopy. The relationship between structure and hydrophobic properties is investigated. ZnO films with water contact angle of 165o are achieved after treatment with alkylsilicane.
(1) ZnO nanorod array films are fabricated by CSD. The effect of buffer layer, the concentration of NaOH, rate of reaction, and temperature on morphology of ZnO films is investigated. The result indicates that the increase in thickness will improve the uniformity and crystallization of buffer layer, and more and more ZnO nanorods grow along c axis. The increase in concentration of NaOH increases pH value, which results in the growth of narrower and denser nanorods. The increase in rate of reaction decreases the uniformity and regularity of nanorods. ZnO films with water contact angle of 165o are achieved at a deposition time of 75mins after treatment with alkylsilicane.
(2) ZnO array films are fabricated by hydrothermal method. The effect of buffer layer, urotropine and the content of cobalt acetate on deposited films are investigated. ZnO nanorods by hydrothermal method grow along c axis at a concentration of 0.1M of urotropine. ZnO buffer layer with zinc acetate as raw material is dense and uniform. Therefore, ZnO array films by hydrothermal method have a preferential orientation. The doping of Co2+ changes the rate of growth of ZnO crystalline faces and hinders the preferential orientation along c axis, which results in the low symmetry of hexagonal structure.
(3) ZnO films are fabricated by electrophoretic deposition. The effect of current density, deposition time and buffer layer on crystalline phase, microstructure, transmittance and wettability is investigated with flake-shaped particles suspension as electrophoretic solution. The result indicates that the current density has a large effect on the morphology of films. Flake-shaped particles align parallel to ITO substrate at a small deposition current, and these particles align normal to the substrate at a large deposition current. The deposited films consist of nano-scaled reticular structure and micro-scaled spheres. The uniformity of ZnO films is improved by adding buffer layer. The specific surface area is increased by the heat treatment at a low temperature, which provides an opportunity for improving hydrophobicity and gas-sensitivity.
(1)化学溶液沉积法制备氧化锌纳米棒阵列膜。研究缓冲层厚度、氢氧化钠浓度、反应速度及反应温度等条件对氧化锌薄膜形貌的影响。结果表明,增加ZnO缓冲层厚度(六层对比两层)可以提高衬底的均匀性以及缓冲层的结晶性,使ZnO纳米棒更多的沿c轴方向生长。氢氧化钠浓度的提高使得溶液pH值增大,导致ZnO纳米棒生长得更细更致密。化学反应速度的提高显著降低了纳米棒的均匀度和规则性。沉积时间为75mins所得氧化锌薄膜经硅烷偶联剂处理后与水的接触角可达到165°。
(2)水热法制备氧化锌阵列膜。研究缓冲层基底及六亚甲基四氨、乙酸钴含量等对合成薄膜的影响。当六亚甲基四氨浓度为0.1M时,水热合成的氧化锌纳米棒生长致密,沿c轴的取向性较好。以乙酸锌为原材料合成的氧化锌缓冲层薄膜比较致密、均匀,晶粒较小,因而水热合成的氧化锌阵列膜的取向度较高。Co2+的掺杂改变了各晶面的生长速度,降低了氧化锌阵列膜沿c轴的择优生长,导致正六角棒状结构的对称性降低,甚至出现开裂。
(3)电泳沉积法制备氧化锌薄膜。以片式颗粒的悬浮液为电泳液,研究电流强度、沉积时间和缓冲层对薄膜的晶相、显微结构、透光度和润湿性的影响。结果表明:电流强度对薄膜的形貌影响较大,当沉积电流较小时,片状颗粒平铺在ITO基片上;当沉积电流较大时,片状颗粒垂直于基片排列,所得薄膜由纳米尺度的网状结构以及微米尺度的球状物组成。ZnO缓冲层显著改善了薄膜的均匀性。低温热处理可大大提高ZnO薄膜的比表面积,对进一步改善其疏水性和气敏性十分有利。
The fabrication processes, microstructure and properties of ZnO functionalized films are investigated. Hydrophobic ZnO films are constructed by chemical solution deposition (CSD), hydrothermal method and electrophoretic deposition, respectively, with zinc acetate, zinc nitrate, NaOH, urotropine and Polyethylene Glycol (PEG) as raw materials. Crystal structure and chemical composition of ZnO films are analyzed by XRD. Microstructure, grain size and morphology are observed by SEM. Microstructural variation resulting from Co2+ dopants is studied by Laman spectroscopy. The relationship between structure and hydrophobic properties is investigated. ZnO films with water contact angle of 165o are achieved after treatment with alkylsilicane.
(1) ZnO nanorod array films are fabricated by CSD. The effect of buffer layer, the concentration of NaOH, rate of reaction, and temperature on morphology of ZnO films is investigated. The result indicates that the increase in thickness will improve the uniformity and crystallization of buffer layer, and more and more ZnO nanorods grow along c axis. The increase in concentration of NaOH increases pH value, which results in the growth of narrower and denser nanorods. The increase in rate of reaction decreases the uniformity and regularity of nanorods. ZnO films with water contact angle of 165o are achieved at a deposition time of 75mins after treatment with alkylsilicane.
(2) ZnO array films are fabricated by hydrothermal method. The effect of buffer layer, urotropine and the content of cobalt acetate on deposited films are investigated. ZnO nanorods by hydrothermal method grow along c axis at a concentration of 0.1M of urotropine. ZnO buffer layer with zinc acetate as raw material is dense and uniform. Therefore, ZnO array films by hydrothermal method have a preferential orientation. The doping of Co2+ changes the rate of growth of ZnO crystalline faces and hinders the preferential orientation along c axis, which results in the low symmetry of hexagonal structure.
(3) ZnO films are fabricated by electrophoretic deposition. The effect of current density, deposition time and buffer layer on crystalline phase, microstructure, transmittance and wettability is investigated with flake-shaped particles suspension as electrophoretic solution. The result indicates that the current density has a large effect on the morphology of films. Flake-shaped particles align parallel to ITO substrate at a small deposition current, and these particles align normal to the substrate at a large deposition current. The deposited films consist of nano-scaled reticular structure and micro-scaled spheres. The uniformity of ZnO films is improved by adding buffer layer. The specific surface area is increased by the heat treatment at a low temperature, which provides an opportunity for improving hydrophobicity and gas-sensitivity.
引文
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