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铁基超疏水表面的制备与研究

Preparation And Reseaches of Superhydrophobic Surfaces on The Iron Substrate

【作者】 高海燕

【导师】 卢士香;

【作者基本信息】 北京理工大学 , 化学, 2016, 硕士

【摘要】 表面的浸润性是决定材料功能的一个重要性质,由于超疏水表面在各个方面的应用性很广,有关超疏水表面的研究已引起了科学家们的兴趣。而铁材料由于其特殊的属性、良好的机械性能、完美的导电性等,已成为国防工业领域的主导材料,但它仍然面临着磨损和腐蚀两大严重问题。基于这些问题,本文采用电化学和退火的方式,在不引入任何低表面能有机物的情况下,在金属铁基表面成功获得了Fe-Zn-ZnO超疏水表面和Fe-Sn超疏水表面,并对超疏水表面的形成机理、超疏水原理及应用进行了分析研究。主要研讨内容及研究结果如下:(1)首次采用电化学沉积和干燥退火相结合的方法在金属铁基上构筑了微纳米双阶层结构的Fe-Zn-ZnO超疏水表面,静态接触角大于150o,滚动角小于10o。该方法所用仪器设备简单,操作简便,制备成本低,实验过程快速有效,突破了传统超疏水表面的制备方法,通过在干燥箱中稳定退火的方法,在不引进任何降低表面自由能的有机物条件下,获得了超疏水性的表面。通过对该超疏水表面的分析表征,研究其表面的化学组成和形成机理。通过对该超疏水表面影响因素(在盐酸中刻蚀时间、电化学沉积时间、电解液浓度、退火温度、退火时间)的分析,得出了制备铁基超疏水薄膜的最佳条件,其中退火成为最关键的因素,并且退火时是否加滤纸对表面超疏水性也有关键性影响,只有加滤纸退火才能保证超疏水性表面的形成。通过对该超疏水表面的表征(扫描电子显微镜(SEM)、X射线衍射仪(XRD)、X射线光电子能谱仪(XPS)原子力显微镜(AFM)等手段),说明由电化学沉积法及退火形成的Fe-Zn-ZnO微-纳米双阶层结构中所占95.3%的空气对超疏水性能的形成有关键作用;之后对超疏水原理以及Fe-Zn-ZnO微-纳米双阶层结构的生长机理进行了研究。通过置于空气中一年,镀锌铁基底超疏水材料的疏水性不变,得出此超疏水表面具有持久性。对其进行抗冰性测试,表明具有良好的抗冰性能;对其进行抗腐蚀测试,表明其抗腐蚀性良好。(2)首次利用电化学沉积和干燥退火相结合的方法在金属铁基体上制备了纳米Sn超疏水表面,进行超疏水表面的润湿性、表面形貌和化学组成的分析,其静态接触角大于150o,滚动角小于10o。通过单因素实验可知Fe-Sn超疏水表面制备的最佳条件。通过实验证明此超疏水表面在大气中具有良好的环境稳定性和抗土壤腐蚀能力。退火在制备金属基底的超疏水表面的过程中起到了十分关键的作用,这也为超疏水材料在工农业生产中的大面积使用提供了一定的思路。

【Abstract】 Wettability is one of the very important property to determine the qualitiy of solid surfaces. Because of the large application of superhydrophobic surface, the research has attracted great attentions. Steel is a common kind of material that is extensively used in many areas owing to its particular properties such as good mechanical properties, perfect electrical conductivity and so on. Practically, the only factor which limits the lifetime of steel is corrosion which disables its excellent properties. To solve these problems, we herein fabricated Fe-Zn-ZnO and Fe-Sn superhydrophobic surfaces by electrochemical machinining and followed by subsequent thermal annealing withoout introducing any low surface energy organics. And the formation mechanism, the principle and application of superhydrophobic surfaces were also analysed.(1) We firstly fabricated micro/nano Fe-Zn-ZnO superhydrophobic surfaces by electrochemical machinining and followed by subsequent thermal annealing. These surfaces display water contact angles(WCA) larger than 150° and sliding angles(SA) less than 10°. The instruments and equipments used in this method were in common, the preparations were of low cost, the experimental procedures were quick and effective, which broke the traditional preparation methods for superhydrophobic surfaces. And by annealing in the drying oven, we did not introduce any organic matters. Through analyzing superhydrophobic surfaces, the surface chemical compositions and formation mechanism were studied. A series of influencing factors should be considered to prepare optimized superhydrophobic surfaces. These include annealing conditions, the concentration of zinc ion(CZI), electrochemical deposition time and etching time. The annealing treatment leads to the most critical factor. After electrochemical depositionon, the surfaces showed superhydrophilic state, however after annealing, they presented superhydrophobic state,The presence or not of filter papers in the process of annealing has crucial influence, and only add filter papers can ensure the formation of superhydrophobic surface. Based on the XPS, XRD and SEM results, it can be concluded that after annealing, the grown Zn micro/nano-particles were well crystallized, the remaining 95.3 % served as the contactarea of the water droplet and air,which can reduce the surface energy and improve the superhydrophobicity. Then the principle and the growth mechanism of Fe-Zn-ZnO micro-nano superhydrophobic were studied. The durability of the SHSs and the freezing properties of water droplets on sample surfaces were also done to show the superhydrophobic surfaces have good environmental stability in the atmosphere. Through the corrosion test, they showed good corrosion resistance.(2) We firstly fabricated micro-nano Fe-Sn superhydrophobic surfaces by electrochemical machinining and followed by subsequent thermal annealing. We analyzed the wettability, the morphology and the chemical composition of superhydrophobic surfaces.Through the single factor experiments, the Fe-Sn superhydrophobic surfaces were the result of comprehensive effects of etching time, electrochemical deposition, electrolyte concentration, annealing temperature and annealing time. The best conditions for its preparation were considered. The experiment proved that the superhydrophobic surfaces in the atmosphere had good environmental stability and soil corrosion resistance. Annealing has played a very key role in the process of building superhydrophobic surfaces on the metal substrates, which provides a train of thought for large applications of superhydrophobic surfaces in industry and agriculture.

  • 【分类号】O647;TQ153
  • 【被引频次】2
  • 【下载频次】425
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