仿生超疏水功能表面的制备及其性能研究
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摘要
超疏水材料是一种对水具有排斥性的材料,水滴在其表面无法滑动铺展而保持球型滚动状,从而达到滚动自清洁的效果。自然界当中的荷叶是该种材料的典型代表。由于该材料的特殊浸润性,使得其在自清洁、防腐蚀、防雾、流体减阻等领域有着广泛的潜在应用。研究发现,材料表面具有较高的粗糙度和较低的表面自由能是实现其超疏水性的两个必要条件。据此,科研人员采用多种方法来构建超疏水表面,如：溶胶凝胶法、等离子体刻蚀法、化学浴法、静电喷涂法、逐层吸附法等等,但能用于大规模应用生产的制备方法较少。本文采用湿化学法制备出超疏水性的无机氧化物薄膜、改性油漆涂层及铝材、锌材,并对其疏水性和隐形性能进行了深入的理论分析,具体内容如下：
在第一章当中,首先对超疏水理论和自然界当中的超疏水表面接进行了简单的介绍；之后对制备有机物、无机物和金属超疏水表面的方法进行了综述；最后对超疏水表面的潜在应用进行了概括分析。
在第二章中,主要做了花状ZnO微球的制备及其浸润性研究和对其形成机机理的探讨。采用HF作为溶液添加剂的方法,影响和控制ZnO材料的结晶生长过程,制备出由花状ZnO微球组成的薄膜。经过氟硅烷修饰后,该薄膜由超亲水性转变为超疏水性,水滴在其表面的接触角为154。,滚动角小于5。,具有良好的超疏水自清洁性。同时结合薄膜表面的结构分析和Cassie-Baxter模型对其浸润性进行了深入的研究,结果表明由片状ZnO组成的微球具有较大的气孔,从而使得水滴和固体表面的接触面积大大减小,加之氟硅烷的修饰使其具有超疏水的性能。然后通过改变ZnO晶体生长时间、改变HF添加量等方法对花状ZnO微球的形成机理进行了研究,结果表明在整个成核生长过程当中,H+的主要作用是减少溶液当中成成核数量,而F的主要作用是限制ZnO沿c轴方向的生长,两种离子的协同作用造成了花状ZnO微球的产生。
在第三章当中,采用ZnO颗粒作为添加剂制备出具有亚超疏水性的改性油漆涂层,水滴在其表面的接触角最高可达147。,接近于超疏水的状态。油漆本身的低表面自由能和ZnO颗粒的掺入增加了涂层表面的粗糙度这两个因素是产生亚超疏水改性涂层的主要原因。本章中对ZnO颗粒的掺入量和油漆掺入量对涂层浸润性的影响进行了研究。结果表明,在固定油漆加入量的前提下,ZnO颗粒的增加可以增加表面的疏水性；而在固定ZnO颗粒掺入量的条件下,油漆量的增加会使得涂层表面的疏水性降低。主要原因是ZnO颗粒与油漆的比例对最终改性涂层表面结构的影响。最后通过与氟硅烷修饰后的ZnO颗粒膜的疏水性进行对比后发现,该表面没有实现超疏水状态的原因有两个：1.油漆自身的疏水性不够高；2.ZnO颗粒提供的气孔量较少。
在第四章中,采用温水浸泡和氟硅烷修饰的方法制备出具有良好的超疏水自清洁性的铝片,水滴在其表面的接触角大于160°,滚动角小于5°。温水处理后使铝片表面形成纳米片组成的粗糙结构,加之氟硅烷的修饰使其具有超疏水的性能。同时文章当中还就温水浸泡的温度及浸泡的时间对铝片浸润性的影响进行了研究,结果表明,采用90℃的温水浸泡且浸泡时间小于2小时可使铝片获得最佳的超疏水效果。
在第五章当中,采用盐酸腐蚀和温水浸泡的方法,使锌片具有了微纳复合结构组成的仿荷叶表面。经过氟硅烷修饰后,该锌片显示出良好的超疏水性。同时文章当中还对盐酸腐蚀的时间对其浸润性的影响进行了研究,结果锌表面经过盐酸处理90秒可以使最终的锌片获得最佳的超疏水性,水滴在其表面的接触角大于160°,滚动角接近于0°。
在第六章中,采用盐酸腐蚀和ZnO晶体生长的方法使白铁皮具有超疏水自清洁性。同时由于ZnO纳米棒对光的散射作用使得该表面同时具有抗红外反射的隐身功能。然后采用理论计算对样品的红外反射性能做了模拟研究,计算结果与实验结果吻合的很好。
第七章对全文进行了总结,对研究当中的不足进行总结的同时对实验结果的应用前景进行了展望。
Superhydrophobicity is a special wettability of a solid surface, on which a water droplet could not spread out and just keep sphere shape, and leading to a rolling motional self-clean function. Superhydrophobic surface possesses water repellent properties as louts leaf. Due to the potential applications in self-cleaning, anti-corrosion, anti-fog, drag reduction and so on, it has attracted a lot of interests of the researcher from both fundamental and industrial fields. It has been realized that the high surface roughness and low surface energy are two basic properties of a superhydrophobic surface. Based on this, a lot of methods were used to fabricate superhydrophobic surface, such as sol-gel, plasma etching, water bath deposition, electrospinning, layer by layer and son on. However, few of these methods could be used in large scale production. In this thesis, wet chemical method was used to prepare superhydrophobic ZnO film, modified paint coating and engineering materials. And their superhydrophobic properties were discussed by using Wenzel and Cassie-Baxter models throughoutly. The content of this thesis is as following. In chapter1, the superhydrophobic theory and superhydrophobic surface in nature were introduced, firstly. Then the methods to prepare superhydrophobic surface and their potential applications were summarized.
In chapter2, the formation and wettability of flower like ZnO micro-sphere were investigated. HF was used to modify ZnO growth process, and nanosheets composed ZnO microsphere was produced. After modified with heptadecafluorodecyltrimethoxy-silane (HTMS), the ZnO film showed superhydrophobicity with water contact angle154°and water sliding angle less than5°. Then the superhydrophobic property of the film was discussed by combing Cassie-Baxter model and surface morphology analysis. The air pocket among nanoshees, wihch reduced the contact between water and solid surface of the film, accounted for the superhydrophobicity of the film. Finally, the formation mechanism of the ZnO micro-sphere was discussed by changing the experiment parameters, such as growth time, HF concentration. The results showed that H+will reduce the nucleary of ZnO, and F-will restrain ZnO growth along c-axis. Due to synergical effect of these tow ions, flower like Zno micro-spheres were formed.
In chapter3, modified paint coating was produced by mixing ZnO particle and paint. As the surface roughness of the surface increased by adding ZnO particles and the low free energy of the paint, the hydrophobicity of the modified paint (water contact angle147°) is better than pure paint (water contact angle95°). The ratios between ZnO and paint will affect the hydrophobicity of the coating, and should be strictly controlled to produce better hydrophobic coating. Finally, by comparing hydrophobicity of the HTMS modified ZnO particle, it could be concluded that the intrinsic poor hydrophobicity of the paint and low air pocket ratio of the ZnO particle are accounted for the sub superhydrophobicity of the coating.
In chapter4, superhydrophobic aluminum sheets were fabricated by hot water immersing process and HTMS modification. The effects of temperature and immersing time on the superhydrophobicity of the aluminum sheet were investigated. The results showed that the best experiment parameter were the90℃water and less than2h immersing. In this condition, the treated aluminum sheet shows best superhydrophobicity with contact angle larger than160°and sliding angle less than5°.
In chapter5, superhydrophobic zinc sheets were fabricated. Firstly, by HCl etching and hot water treatment, lotus leaf like structure was formed on zinc sheets. After modified by HTMS, the zinc sheets showed superhydrophobicity. After throughout researches, it has been shown that the90s HCl etching could product the sample with the best superhydrophobicity (contact angle larger than160°and sliding angle close to0°).
In chapter6, a galvanized iron sheet with both anti-infrared reflectance invisibility functions and superhydrophobic properties was fabricated. Firstly, the micro-scale structures were produced by HCl etching. Then ZnO nanorods were grown on their surface to form lotus-like structure. After modification with HTMS, the surface showed superhydrophobicity. At the same time, the surface possessed anti-infrared reflectance property. It could be ascribed to the light scattering of the ZnO nanorods. Finally, a light scattering model was used to calculate the infrared reflectance of treated sheet. The result fitted well with the experimental data.
In chapter7, the whole thesis contents were summarized and the potential applications of the experiment product were illustrated.
在第一章当中,首先对超疏水理论和自然界当中的超疏水表面接进行了简单的介绍；之后对制备有机物、无机物和金属超疏水表面的方法进行了综述；最后对超疏水表面的潜在应用进行了概括分析。
在第二章中,主要做了花状ZnO微球的制备及其浸润性研究和对其形成机机理的探讨。采用HF作为溶液添加剂的方法,影响和控制ZnO材料的结晶生长过程,制备出由花状ZnO微球组成的薄膜。经过氟硅烷修饰后,该薄膜由超亲水性转变为超疏水性,水滴在其表面的接触角为154。,滚动角小于5。,具有良好的超疏水自清洁性。同时结合薄膜表面的结构分析和Cassie-Baxter模型对其浸润性进行了深入的研究,结果表明由片状ZnO组成的微球具有较大的气孔,从而使得水滴和固体表面的接触面积大大减小,加之氟硅烷的修饰使其具有超疏水的性能。然后通过改变ZnO晶体生长时间、改变HF添加量等方法对花状ZnO微球的形成机理进行了研究,结果表明在整个成核生长过程当中,H+的主要作用是减少溶液当中成成核数量,而F的主要作用是限制ZnO沿c轴方向的生长,两种离子的协同作用造成了花状ZnO微球的产生。
在第三章当中,采用ZnO颗粒作为添加剂制备出具有亚超疏水性的改性油漆涂层,水滴在其表面的接触角最高可达147。,接近于超疏水的状态。油漆本身的低表面自由能和ZnO颗粒的掺入增加了涂层表面的粗糙度这两个因素是产生亚超疏水改性涂层的主要原因。本章中对ZnO颗粒的掺入量和油漆掺入量对涂层浸润性的影响进行了研究。结果表明,在固定油漆加入量的前提下,ZnO颗粒的增加可以增加表面的疏水性；而在固定ZnO颗粒掺入量的条件下,油漆量的增加会使得涂层表面的疏水性降低。主要原因是ZnO颗粒与油漆的比例对最终改性涂层表面结构的影响。最后通过与氟硅烷修饰后的ZnO颗粒膜的疏水性进行对比后发现,该表面没有实现超疏水状态的原因有两个：1.油漆自身的疏水性不够高；2.ZnO颗粒提供的气孔量较少。
在第四章中,采用温水浸泡和氟硅烷修饰的方法制备出具有良好的超疏水自清洁性的铝片,水滴在其表面的接触角大于160°,滚动角小于5°。温水处理后使铝片表面形成纳米片组成的粗糙结构,加之氟硅烷的修饰使其具有超疏水的性能。同时文章当中还就温水浸泡的温度及浸泡的时间对铝片浸润性的影响进行了研究,结果表明,采用90℃的温水浸泡且浸泡时间小于2小时可使铝片获得最佳的超疏水效果。
在第五章当中,采用盐酸腐蚀和温水浸泡的方法,使锌片具有了微纳复合结构组成的仿荷叶表面。经过氟硅烷修饰后,该锌片显示出良好的超疏水性。同时文章当中还对盐酸腐蚀的时间对其浸润性的影响进行了研究,结果锌表面经过盐酸处理90秒可以使最终的锌片获得最佳的超疏水性,水滴在其表面的接触角大于160°,滚动角接近于0°。
在第六章中,采用盐酸腐蚀和ZnO晶体生长的方法使白铁皮具有超疏水自清洁性。同时由于ZnO纳米棒对光的散射作用使得该表面同时具有抗红外反射的隐身功能。然后采用理论计算对样品的红外反射性能做了模拟研究,计算结果与实验结果吻合的很好。
第七章对全文进行了总结,对研究当中的不足进行总结的同时对实验结果的应用前景进行了展望。
Superhydrophobicity is a special wettability of a solid surface, on which a water droplet could not spread out and just keep sphere shape, and leading to a rolling motional self-clean function. Superhydrophobic surface possesses water repellent properties as louts leaf. Due to the potential applications in self-cleaning, anti-corrosion, anti-fog, drag reduction and so on, it has attracted a lot of interests of the researcher from both fundamental and industrial fields. It has been realized that the high surface roughness and low surface energy are two basic properties of a superhydrophobic surface. Based on this, a lot of methods were used to fabricate superhydrophobic surface, such as sol-gel, plasma etching, water bath deposition, electrospinning, layer by layer and son on. However, few of these methods could be used in large scale production. In this thesis, wet chemical method was used to prepare superhydrophobic ZnO film, modified paint coating and engineering materials. And their superhydrophobic properties were discussed by using Wenzel and Cassie-Baxter models throughoutly. The content of this thesis is as following. In chapter1, the superhydrophobic theory and superhydrophobic surface in nature were introduced, firstly. Then the methods to prepare superhydrophobic surface and their potential applications were summarized.
In chapter2, the formation and wettability of flower like ZnO micro-sphere were investigated. HF was used to modify ZnO growth process, and nanosheets composed ZnO microsphere was produced. After modified with heptadecafluorodecyltrimethoxy-silane (HTMS), the ZnO film showed superhydrophobicity with water contact angle154°and water sliding angle less than5°. Then the superhydrophobic property of the film was discussed by combing Cassie-Baxter model and surface morphology analysis. The air pocket among nanoshees, wihch reduced the contact between water and solid surface of the film, accounted for the superhydrophobicity of the film. Finally, the formation mechanism of the ZnO micro-sphere was discussed by changing the experiment parameters, such as growth time, HF concentration. The results showed that H+will reduce the nucleary of ZnO, and F-will restrain ZnO growth along c-axis. Due to synergical effect of these tow ions, flower like Zno micro-spheres were formed.
In chapter3, modified paint coating was produced by mixing ZnO particle and paint. As the surface roughness of the surface increased by adding ZnO particles and the low free energy of the paint, the hydrophobicity of the modified paint (water contact angle147°) is better than pure paint (water contact angle95°). The ratios between ZnO and paint will affect the hydrophobicity of the coating, and should be strictly controlled to produce better hydrophobic coating. Finally, by comparing hydrophobicity of the HTMS modified ZnO particle, it could be concluded that the intrinsic poor hydrophobicity of the paint and low air pocket ratio of the ZnO particle are accounted for the sub superhydrophobicity of the coating.
In chapter4, superhydrophobic aluminum sheets were fabricated by hot water immersing process and HTMS modification. The effects of temperature and immersing time on the superhydrophobicity of the aluminum sheet were investigated. The results showed that the best experiment parameter were the90℃water and less than2h immersing. In this condition, the treated aluminum sheet shows best superhydrophobicity with contact angle larger than160°and sliding angle less than5°.
In chapter5, superhydrophobic zinc sheets were fabricated. Firstly, by HCl etching and hot water treatment, lotus leaf like structure was formed on zinc sheets. After modified by HTMS, the zinc sheets showed superhydrophobicity. After throughout researches, it has been shown that the90s HCl etching could product the sample with the best superhydrophobicity (contact angle larger than160°and sliding angle close to0°).
In chapter6, a galvanized iron sheet with both anti-infrared reflectance invisibility functions and superhydrophobic properties was fabricated. Firstly, the micro-scale structures were produced by HCl etching. Then ZnO nanorods were grown on their surface to form lotus-like structure. After modification with HTMS, the surface showed superhydrophobicity. At the same time, the surface possessed anti-infrared reflectance property. It could be ascribed to the light scattering of the ZnO nanorods. Finally, a light scattering model was used to calculate the infrared reflectance of treated sheet. The result fitted well with the experimental data.
In chapter7, the whole thesis contents were summarized and the potential applications of the experiment product were illustrated.
引文
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