表面微观多级结构镍的电化学构建调控及其性质

发布时间：2018-09-12 13:07

【摘要】：近年来,超疏水技术作为一种新型的环境友好型防腐方式得到了广泛的关注。本文通过廉价简单的电化学沉积方式制备了具有微米-纳米复合微观结构的镍镀层,经十四酸修饰后,镀层显示出了良好的超疏水性能。在此基础上,为了进一步提高超疏水镍镀层的机械性能、超疏水性能和防腐性能。作者通过添加SiO_2纳米粒子、片层石墨烯,制备了超疏水Ni-SiO_2复合镀层和超疏水石墨烯复合镍镀层。同时,本文通过静态接触角和滚动角测试镀层的润湿特性,通过摩擦测试测量超疏水镀层的机械性能,通过电化学测试和腐蚀介质浸泡试验考察超疏水镀层的耐蚀性,最后通过扫描电镜和EDS能谱图观察镀层的微观形貌和镀层的化学成分。对比研究发现制备的三种超疏水镀层各项性能的差异,其中得出的结论如下:(1)通过电化学沉积法制得镍镀层在经化学修饰后,显示出良好的超疏水性能。当电流密度为3 A/dm2,电镀时间为10min时,制得的超疏水镍镀层具有最佳的机械性能,经10次循环摩擦测试仍能保持超疏水性能,其静态接触角达到153.2±0.54°,其滚动角约为15°。通过与普通镍镀层进行对比,超疏水镍镀层具有更佳的耐腐蚀性能,其自腐蚀电流密度为1.324×10-7 A·cm-2,阻抗值高达3.39×105Ω·cm2。经3.5 wt.%Na Cl腐蚀溶液的浸泡48小时后,仍具有良好的耐蚀性能。(2)通过溶胶凝胶法制备的SiO_2纳米粒子粒径大约为200-300 nm,当电流密度为3 A/dm2,电镀时间为10 min时,镀层中SiO_2纳米粒子含量显著提高。制得的超疏水Ni-SiO_2复合镀层在经15次循环摩擦测试仍能保持超疏水性能,其静态接触角最大达到156.7±0.74°,其滚动角为8.7±1.0°,表现出优异的超疏水性能。其自腐蚀电流密度为1.099×10-7 A·cm-2,阻抗值3.47×105Ω·cm2,表现出良好的耐腐蚀性能。(3)经过添加片层石墨烯制得的超疏水镀层,具有明显的微米-纳米多级分层结构。表现出了最佳的超疏水性能,当电流密度为2 A/dm2时,其静态接触角最大可达到160.4±1.5°,滚动角低至4°。镀层的阻抗达为2.8×106Ω·cm2,自腐蚀电流密度低至1.961×10-8 A·cm-2。经过60次的循环摩擦测试仍具有超疏水特性。进过72小时腐蚀介质浸泡,仍具有较好的防腐蚀性能。
[Abstract]:In recent years, superhydrophobic technology as a new type of environmental-friendly anticorrosion has been widely concerned. In this paper, nickel coatings with micron-nano composite microstructure were prepared by cheap and simple electrochemical deposition. The coatings showed excellent superhydrophobic properties after modification with tetradecanoic acid. On this basis, in order to further improve the mechanical properties, super hydrophobic and anticorrosive properties of super hydrophobic nickel coating. Superhydrophobic Ni-SiO_2 composite coating and superhydrophobic graphene composite nickel coating were prepared by adding SiO_2 nanoparticles and lamellar graphene. At the same time, the wetting characteristics of the coating were tested by static contact angle and rolling angle, the mechanical properties of superhydrophobic coating were measured by friction test, and the corrosion resistance of superhydrophobic coating was investigated by electrochemical test and corrosion medium immersion test. Finally, the microstructure and chemical composition of the coating were observed by scanning electron microscope (SEM) and EDS spectroscopy. The results show that the properties of the three kinds of superhydrophobic coatings are different. The conclusions are as follows: (1) the electrochemically modified nickel coatings show good superhydrophobic properties. When the current density is 3 A / dm2 and the electroplating time is 10min, the superhydrophobic nickel coating has the best mechanical properties. After 10 cycles of friction test, the superhydrophobicity can still be maintained. The static contact angle is 153.2 卤0.54 掳and the rolling angle is about 15 掳. Compared with ordinary nickel coating, superhydrophobic nickel coating has better corrosion resistance, and its corrosion current density is 1.324 脳 10 ~ (-7) A cm-2, impedance of 3.39 脳 10 ~ 5 惟 cm2.. After being immersed in 3.5 wt.%Na Cl corrosion solution for 48 hours, the SiO_2 nanoparticles still have good corrosion resistance. (2) the diameter of SiO_2 nanoparticles prepared by sol-gel method is about 200-300 nm, when the current density is 3 A / dm2 and the electroplating time is 10 min. The content of SiO_2 nanoparticles in the coating increased significantly. The superhydrophobic Ni-SiO_2 composite coating can maintain its hydrophobicity after 15 cycles of friction test. The maximum static contact angle is 156.7 卤0.74 掳and the rolling angle is 8.7 卤1.0 掳, showing excellent superhydrophobic properties. The self-corrosion current density is 1.099 脳 10 ~ (-7) A cm-2, impedance value 3.47 脳 10 ~ 5 惟 cm2, shows good corrosion resistance. (3) the superhydrophobic coating prepared by adding graphene lamellar has obvious micron-nanometer multilevel delamination structure. When the current density is 2 A/dm2, the maximum static contact angle is 160.4 卤1.5 掳and the rolling angle is as low as 4 掳. The impedance of the coating is 2.8 脳 10 ~ 6 惟 cm2, and the corrosion current density is as low as 1.961 脳 10 ~ (-8) A cm-2.. After 60 times of cyclic friction test, it still has super hydrophobic property. After 72 hours of immersion in corrosion medium, it still has good corrosion resistance.
【学位授予单位】：南京航空航天大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TG174.4

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