纳米CeO_2颗粒对镀锌层的改性工艺及其机理研究
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摘要
镀锌是应用最广泛的防止钢铁材料腐蚀的有效措施。但随着环境中酸雨和风沙侵蚀的日益加重,不仅对镀锌层的耐蚀性提出了更高的要求,而且还要求镀锌层具有高的耐磨性。因此,研究和开发新型高耐蚀、高耐磨锌基镀层具有十分重要的意义。本文将纳米科技与电沉积锌和热浸镀锌技术相结合,基于稀土元素对提高镀锌层性能的特殊作用和我国稀土资源富有的国情,提出了采用纳米稀土氧化物CeO_2颗粒改性锌及锌铝合金镀层的构想,并对改性工艺及机理开展了深入系统的研究,为纳米锌基复合镀层的基础研究和产业化应用奠定了重要基础。
本文完成的主要工作和取得的成果如下:
1.采用复合电沉积工艺制备了纳米CeO_2颗粒呈单分散状态弥散分布的Zn-CeO_2纳米复合镀层,并利用电化学阻抗谱技术研究了复合电沉积过程的机理,发现纳米CeO_2颗粒的加入降低了反应的电荷传递电阻,更有利于锌的电沉积过程。
2.首次采用超声波辅助热浸镀方法成功地制备了Zn-CeO_2和Galfan-CeO_2纳米复合镀层,并利用TEM、XRD、SEM以及EDS等对其组织结构进行了表征,发现镀层中纳米CeO_2颗粒呈理想的单分散状态弥散分布;归纳了高能超声在热浸镀纳米颗粒增强锌基复合镀层中的作用机制。
3.首次深入系统地研究了中间体预制辅助热浸镀锌基纳米复合镀层的制备方法。采用高能球磨技术分别制备了纳米CeO_2/Zn、CeO_2/Al和CeO_2/Zn-5%Al复合粉末,利用TEM、XPS、XRD、SEM以及EDS等分析和表征了其组织结构,发现复合粉末中纳米CeO_2颗粒被很好地分散开且呈均匀弥散分布,提出了粉末的复合模型;采用真空热压技术将球磨得到的复合粉末制成纳米CeO_2颗粒呈单个弥散分布的复合材料块体,并利用正交试验对热压工艺参数进行了优化;将纳米CeO_2/Zn复合材料块体作为中间体加入热浸镀锌和Galfan合金镀液中对钢片进行热浸镀,成功地获得了单分散状态的纳米CeO_2颗粒弥散均匀分布在镀层基体上的Zn-CeO_2和Galfan-CeO_2纳米复合镀层。
4.系统地研究了纳米CeO_2颗粒对镀层耐腐蚀性、耐磨性、硬度、结合力及镀层钢丝拉伸强度等的影响规律,发现纳米CeO_2颗粒的加入显著提高了镀锌层的耐蚀性、显微硬度、耐磨性等。腐蚀失重法、阳极极化法以及电化学阻抗谱技术研究表明,改善镀层耐蚀性的效果与镀液中CeO_2颗粒尺寸、含量及分散情况等有关;冲蚀磨损试验研究表明,在一定范围内增加镀液中纳米CeO_2颗粒的含量,镀层的耐冲蚀磨损性能随之提高。
5.首次利用电化学阻抗谱方法并结合组织结构分析深入系统地研究了纳米CeO_2颗粒提高电沉积锌层、热浸镀锌和Galfan合金镀层耐蚀性的机理;探讨了CeO_2颗粒改善镀层耐磨性机理以及强化镀层的机制。为进一步全面提升锌基复合镀层的综合性能提供了理论依据。
Galvanizing is the most efficient and widely used measure in protecting steel from corrosion. But with the increasing possibilities of acid rain and sand-dust, the galvanized coatings are required to provide not only a higher corrosion resistance, but also a good wear resistance. Therefore, it is significantly important to research and develop novel galvanized coatings with improved corrosion and wear resistances. Combining nano-technology with galvanizing technology, and based on the special effects of rare earth elements on the corrosion resistance of galvanized coating and the abundance of rare earth elements in China, it was proposed in this dissertation to modify the galvanized coatings with rare earth oxide CeO_2 nano-particles. A systematic research on the modification process and mechanism was carried out, and the results provide the fundamental for the application of nano-composite galvanized coatings. The main work and results are as follows:
1. Zn-CeO_2 nanocomposite coatings with homogeneously distributed monodisperse CeO_2 nano-particle have been obtained by electrochemical codeposition. The electrochemical impedance spectroscopy technique was used to investigate the mechanism of codeposition. The result shows that the charge transfer resistances are lowered with the addition of CeO_2 nano-particle which is in favor of the deposition of zinc.
2. Zn-CeO_2 and Galfan-CeO_2 nanocomposite coatings were fabricated successfully for the first time by hot-dip process with high intensity ultrasonic stirring, and then characterized using TEM, XRD, SEM and EDS methods. It was found that the monodisperse CeO_2 nano-particle was distributed homogeneously in the coatings. The mechanism of high intensity ultrasonic stirring on the dispersion of nano-particles in the hot-dip galvanized coatings was deduced as well.
3. The method of preparing Zn-based hot-dipped nano-composite coating via“master alloy”was originally investigated in details. The CeO_2/Zn, CeO_2/Al and CeO_2/Zn-5%Al nano-composite powders were fabricated by high-energy ball milling. The morphology and microstructure were investigated by means of TEM, XPS, XRD, SEM and EDS, respectively. The results show that nano-CeO_2 particles are distributed homogeneously in the composite powders, which was described using formation models of composite powders. The nano-composite bulks were produced by hot-press sintering under vacuum with as-prepared nano-composite powders, and the processing parameters were optimized by ways of orthogonal design. Adding the as-sintered CeO_2 /Zn nanocomposite bulks into the hot-dip galvanizing and Galfan alloy bath as“master alloy”, Zn-CeO_2 and Galfan-CeO_2 nanocomposite coatings were obtained with homogeneously distributed monodisperse CeO_2 nano-particle.
4. The effects of CeO_2 nano-particle on the corrosion and wear resistances, hardness, adhesion strength of the Zn-based coatings were investigated, as well as the tensile properties of the steel wire coated with the Zn-CeO_2 and Galfan-CeO_2 nanocomposite. It was found that the properties of the coatings, such as corrosion and wear resistances, microhardness, and so on, are improved obviously as the result of adding CeO_2 nano-particles. The results of corrosion weight loss, anodic polarization and electrochemical impedance spectroscopy analysis indicate that the improving effect on corrosion resistance is relevant to the size, content and dispersion of CeO_2 nano-particles in galvanizing solution. Erosion test shows that the erosion resistance increases with the increasing content of CeO_2 nano-particles within the concentration range used.
5. The improving mechanisms of CeO_2 nano-particle on the corrosion resistance of the electrodeposited galvanized coatings, hot-dip galvanized and Galfan alloy coatings were investigated by combining the electrochemical impedance spectroscopy technique with morphology and microstructure analyses. Furthermore, the mechanisms of CeO_2 nano-particle on improving the erosion resistance and strengthening of composite coatings were discussed. All provides a theoretical basis for improving the whole properties of Zn-based composite coatings.
本文完成的主要工作和取得的成果如下:
1.采用复合电沉积工艺制备了纳米CeO_2颗粒呈单分散状态弥散分布的Zn-CeO_2纳米复合镀层,并利用电化学阻抗谱技术研究了复合电沉积过程的机理,发现纳米CeO_2颗粒的加入降低了反应的电荷传递电阻,更有利于锌的电沉积过程。
2.首次采用超声波辅助热浸镀方法成功地制备了Zn-CeO_2和Galfan-CeO_2纳米复合镀层,并利用TEM、XRD、SEM以及EDS等对其组织结构进行了表征,发现镀层中纳米CeO_2颗粒呈理想的单分散状态弥散分布;归纳了高能超声在热浸镀纳米颗粒增强锌基复合镀层中的作用机制。
3.首次深入系统地研究了中间体预制辅助热浸镀锌基纳米复合镀层的制备方法。采用高能球磨技术分别制备了纳米CeO_2/Zn、CeO_2/Al和CeO_2/Zn-5%Al复合粉末,利用TEM、XPS、XRD、SEM以及EDS等分析和表征了其组织结构,发现复合粉末中纳米CeO_2颗粒被很好地分散开且呈均匀弥散分布,提出了粉末的复合模型;采用真空热压技术将球磨得到的复合粉末制成纳米CeO_2颗粒呈单个弥散分布的复合材料块体,并利用正交试验对热压工艺参数进行了优化;将纳米CeO_2/Zn复合材料块体作为中间体加入热浸镀锌和Galfan合金镀液中对钢片进行热浸镀,成功地获得了单分散状态的纳米CeO_2颗粒弥散均匀分布在镀层基体上的Zn-CeO_2和Galfan-CeO_2纳米复合镀层。
4.系统地研究了纳米CeO_2颗粒对镀层耐腐蚀性、耐磨性、硬度、结合力及镀层钢丝拉伸强度等的影响规律,发现纳米CeO_2颗粒的加入显著提高了镀锌层的耐蚀性、显微硬度、耐磨性等。腐蚀失重法、阳极极化法以及电化学阻抗谱技术研究表明,改善镀层耐蚀性的效果与镀液中CeO_2颗粒尺寸、含量及分散情况等有关;冲蚀磨损试验研究表明,在一定范围内增加镀液中纳米CeO_2颗粒的含量,镀层的耐冲蚀磨损性能随之提高。
5.首次利用电化学阻抗谱方法并结合组织结构分析深入系统地研究了纳米CeO_2颗粒提高电沉积锌层、热浸镀锌和Galfan合金镀层耐蚀性的机理;探讨了CeO_2颗粒改善镀层耐磨性机理以及强化镀层的机制。为进一步全面提升锌基复合镀层的综合性能提供了理论依据。
Galvanizing is the most efficient and widely used measure in protecting steel from corrosion. But with the increasing possibilities of acid rain and sand-dust, the galvanized coatings are required to provide not only a higher corrosion resistance, but also a good wear resistance. Therefore, it is significantly important to research and develop novel galvanized coatings with improved corrosion and wear resistances. Combining nano-technology with galvanizing technology, and based on the special effects of rare earth elements on the corrosion resistance of galvanized coating and the abundance of rare earth elements in China, it was proposed in this dissertation to modify the galvanized coatings with rare earth oxide CeO_2 nano-particles. A systematic research on the modification process and mechanism was carried out, and the results provide the fundamental for the application of nano-composite galvanized coatings. The main work and results are as follows:
1. Zn-CeO_2 nanocomposite coatings with homogeneously distributed monodisperse CeO_2 nano-particle have been obtained by electrochemical codeposition. The electrochemical impedance spectroscopy technique was used to investigate the mechanism of codeposition. The result shows that the charge transfer resistances are lowered with the addition of CeO_2 nano-particle which is in favor of the deposition of zinc.
2. Zn-CeO_2 and Galfan-CeO_2 nanocomposite coatings were fabricated successfully for the first time by hot-dip process with high intensity ultrasonic stirring, and then characterized using TEM, XRD, SEM and EDS methods. It was found that the monodisperse CeO_2 nano-particle was distributed homogeneously in the coatings. The mechanism of high intensity ultrasonic stirring on the dispersion of nano-particles in the hot-dip galvanized coatings was deduced as well.
3. The method of preparing Zn-based hot-dipped nano-composite coating via“master alloy”was originally investigated in details. The CeO_2/Zn, CeO_2/Al and CeO_2/Zn-5%Al nano-composite powders were fabricated by high-energy ball milling. The morphology and microstructure were investigated by means of TEM, XPS, XRD, SEM and EDS, respectively. The results show that nano-CeO_2 particles are distributed homogeneously in the composite powders, which was described using formation models of composite powders. The nano-composite bulks were produced by hot-press sintering under vacuum with as-prepared nano-composite powders, and the processing parameters were optimized by ways of orthogonal design. Adding the as-sintered CeO_2 /Zn nanocomposite bulks into the hot-dip galvanizing and Galfan alloy bath as“master alloy”, Zn-CeO_2 and Galfan-CeO_2 nanocomposite coatings were obtained with homogeneously distributed monodisperse CeO_2 nano-particle.
4. The effects of CeO_2 nano-particle on the corrosion and wear resistances, hardness, adhesion strength of the Zn-based coatings were investigated, as well as the tensile properties of the steel wire coated with the Zn-CeO_2 and Galfan-CeO_2 nanocomposite. It was found that the properties of the coatings, such as corrosion and wear resistances, microhardness, and so on, are improved obviously as the result of adding CeO_2 nano-particles. The results of corrosion weight loss, anodic polarization and electrochemical impedance spectroscopy analysis indicate that the improving effect on corrosion resistance is relevant to the size, content and dispersion of CeO_2 nano-particles in galvanizing solution. Erosion test shows that the erosion resistance increases with the increasing content of CeO_2 nano-particles within the concentration range used.
5. The improving mechanisms of CeO_2 nano-particle on the corrosion resistance of the electrodeposited galvanized coatings, hot-dip galvanized and Galfan alloy coatings were investigated by combining the electrochemical impedance spectroscopy technique with morphology and microstructure analyses. Furthermore, the mechanisms of CeO_2 nano-particle on improving the erosion resistance and strengthening of composite coatings were discussed. All provides a theoretical basis for improving the whole properties of Zn-based composite coatings.
引文
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