AZ91D镁合金微弧氧化—溶胶凝胶复合膜层制备及其耐蚀性
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摘要
镁合金是最轻的金属结构材料之一,在汽车、航空航天以及电子行业中具有广阔的应用前景,但较差的耐腐蚀性能限制了镁合金的应用。微弧氧化技术是近年来公认的最有前途的镁合金表面处理方法之一。它是在普通阳极氧化基础上发展而来的一种表面处理技术,能够在Al、Mg、Ti等阀金属及其合金表面原位形成陶瓷膜层,极大地提高金属的耐蚀、耐磨等性能。但微弧氧化膜的多孔结构也对其防腐蚀作用埋下了隐患。常用的镁合金微弧氧化电解质溶液有两大类,一类为以含Cr(VI)化合物为主要组分的电解质溶液；另一类为以磷酸盐和／或氟化物为主要组分的电解质溶液。这些电解质溶液中均含有对环境有极大危害的物质,因此,开发绿色环保型镁合金微弧氧化电解液体系,深入探讨微弧氧化处理工艺、膜层的结构与性能以及其生长过程是十分必要的。为进一步提高镁合金的耐蚀性,改善微弧氧化膜的结构,于镁合金表面制备复合膜层并系统研究复合膜的组成、结构与性能之间的关系,以及膜层之间的结合机制,对镁合金的广泛应用也具有重要的意义。
本文首先采用单因素实验和正交实验,系统讨论了微弧氧化电解液中主成膜剂、辅助成膜剂、添加剂等成分及其浓度对微弧氧化过程和膜层性能的影响,开发出了一种绿色环保型的镁合金微弧氧化电解液体系,并分析了各成分在镁合金微弧氧化过程中所起的作用。所开发出的绿色环保型镁合金微弧氧化电解液体系为：铝酸钠30g/dm3,氢氧化钠20g/dm3,蒙脱石3g/dm3,阿拉伯树胶2g/dm3。
采用田口实验设计方法,研究了工艺参数对微弧氧化膜表面形貌和耐蚀性的影响,优化了微弧氧化过程工艺参数。通过扫描电镜、能谱、X衍射、极化曲线和交流阻抗等测试方法,分析了微弧氧化膜的形貌、组成、结构和耐腐蚀性能。结果表明,最佳微弧氧化工艺条件为：终止电压180V,氧化时间30min,脉冲频率50Hz,占空比30%。优化工艺下所制备的微弧氧化膜为多孔结构,A1、O元素含量较高,膜层主要由MgO.MgAl2O4和Al12Mg17组成,耐腐蚀性能比AZ91D镁合金基体有了一定程度的提高。
在镁合金微弧氧化的基础上,采用微弧氧化与溶胶凝胶技术相结合,在镁合金微弧氧化膜表面制备出了具有一定厚度的溶胶凝胶层,形成复合膜层。通过扫描电镜、能谱、X衍射、差热-热重、红外光谱、极化曲线、交流阻抗和循环阳极极化曲线等分析测试方法,优化了溶胶制备工艺和溶胶凝胶层沉积工艺,系统研究了复合膜的形貌、组成、结构等特征及其耐蚀性。结果表明,最佳溶胶制备工艺为：Si：Zr摩尔比为2：1,水浴时间30min,水浴温度50℃,pH值为3。最佳溶胶凝胶膜层沉积工艺为：采用凝胶化工艺处理,干燥温度控制在80℃右,干燥时间1h,固化温度150℃,固化时间0.5h,浸涂次数3次。优化工艺下所制备的复合膜为微晶与玻璃态的混合结构,表面微观缺陷较少,结合力和致密性都较好,具有较强的耐蚀性。
研究了微弧氧化膜的生长过程,分析了处于不同生长阶段氧化膜的形貌、成分和耐蚀性。首次采用Gaussian03分析软件,计算了溶胶凝胶层吸附前后体系中的相关键长、荷电状态和结合能,从分子或原子水平上分析了复合膜层间的结合状态。结果表明,处于不同生长阶段氧化膜的结构形貌与其耐蚀性具有对应关系。溶胶凝胶膜在微弧氧化膜表面的吸附更加稳定,复合膜的层间结合力较好,为在AZ91D镁合金表面制备高性能的防腐蚀涂层提供了一定的理论依据。
使用极化曲线与交流阻抗技术,深入研究了微弧氧化膜和复合膜在不同腐蚀介质中的腐蚀扩展过程。并针对性的建立了不同的等效电路模型,对微弧氧化膜和复合膜在不同腐蚀介质和不同腐蚀时期的腐蚀行为进行了详细的分析。结果表明,在3.5%氯化钠溶液、3.5%硫酸钠溶液和模拟海水溶液中,微弧氧化膜和复合膜表现出某些相似的腐蚀电化学行为,也出现一些不同的特征。在不同的腐蚀介质以及不同的腐蚀时期,腐蚀控制过程会发生改变。
最后,在镁合金表面成功制备了有色复合膜层,并采用扫描电镜、能谱、红外光谱、极化曲线和循环阳极极化曲线等分析测试方法,探讨了有色复合膜的结构形貌、耐腐蚀性能和耐蚀机理。结果表明,本文所制备的有色复合膜表面光滑,着色效果较好。其中添加CuSO4·5H2O所制备出的有色复合膜耐腐蚀性能最好。
Magnesium alloy is one of the most light weight metal structure materials. Their potential applied fields include automobile, aerospace and consuming electronics, etc. However, the extensive use of magnesium alloys is limited due to poor corrosion resistance. Micro-arc oxidation (MAO) technique is one of the most favorable method in the surface treatment of magnesium alloys in recent years. It is a surface treatment technique developed from the common anodic oxidation. By use of this technique, a ceramic coating can be in situ formed on Al, Mg, Ti and their alloys. This enhances the corrosion resistance and abrasion resistance of the magnesium alloy. Unfortunately, there exist micropores and microcracks in the MAO coating. Usually, the two types of electrolyte solution apply to the micro-arc oxidation of magnesium alloy. One of the electrolyte contains Cr(VI) compounds, the other of the electrolyte contains phosphate and/or fluoride. Both of them contains the poisonous ingredients, such as chromate, phosphate, fluoride which do harm to environment and human beings. Therefore, it is essential that environment-friendly electrolyte system was developed and the effects of all kinds of process parameters on the formation and properties of anodic films were investigated. To further enhance the corrosion resistance of magnesium alloys and improve the structure of MAO coating, the composite coatings were prepared on magnesium alloy. The relationship between structure and performance of the composite coatings, and the binding mechanism between the sol-gel layer and MAO layer were studied.
In this paper, single factor and orthogonal layout experiment were applied. The effects of main film-forming agent, auxiliary film-forming agent, additives and their concentration on MAO process and film properties were discussed in the system. An environment-friendly MAO electrolyte system was developed as following,30g/dm3 NaAl2O4, 20g/dm3 NaOH,3g/dm3 montmorillonite, 2g/dm3 gum arabic. And the function of single electrolyte in MAO process was analyzed.
The effects of process parameters on surface morphologies and corrosion resistance of MAO coating were systematically investigated using the Taguchi experimental analysis method of four factors with three levels. The optimized parameters were 180V voltage,30min treatment time,50Hz frequency,30%duty cycle. The morphology, components, structure and corrosion resistance of MAO coating were examined by means of SEM, EDS, XRD, potentiodynamic polarization and AC impedance. The results showed that the MAO coating was a uniform distribution of porous structure. The components of aluminium and oxygen were higher, and the microstructure of the coating consisted of MgO、MgAl2O4and Al12Mg17 phases. Compared with the untreated magnesium alloy, the MAO coating exhibited higher corrosion resistance.
Based on micro-arc oxidation, a process of MAO combined with a sol-gel method was used to prepare composite coatings on magnesium alloy AZ91D. The composite coatings were formed using multi immersion technique to plus a sol-gel layer on the MAO coating. SEM, EDS, XRD, DSC-TGA, FT-IR, potentiodynamic polarization, AC impedance and cyclic anodic polarization curve were used to evaluate the morphologies, components, structure and corrosion resistance of composite coatings. The results showed that the optimum sol preparation process were Si:Zr molar ratio of 2:1, water bath time was 30min, temperature was 50℃, pH value was 3. The optimum sol-gel film deposition conditions were obtained as following, dipping times was 3, drying temperature was controlled about 80℃, drying time was 1h, curing temperature and curing time were 150℃and 0.5h, respectively. The structure of composite coatings was microcrystalline and glass. The composite coatings were more compact and had good adhesion. Few tiny cracks were visible on the surface layer. The corrosion resistance of the composite coatings was enhanced significantly.
The morphology, composition and corrosion resistance of oxide film at different growth stages were studied. Gaussian03 analysis software firstly used to calculate the bond length, charge and binding energy of adsorption system. The bound state of the coatings was analyzed in molecular level. The results showed that the structure characteristics and the corrosion resistance of oxide film at different growth stages had a corresponding relationship. Sol-gel layer of the MAO coating surface in the adsorption was more stable. For the preparation of high-performance anti-corrosion coating on AZ91D magnesium alloy provided a theoretical basis.
It was researched the corrosion development process of the MAO coating and the composite coatings in various corrosive media by using polarization curves and AC impedance techniques. Then different equivalent circuits were put forward to detailed describe the corrosion behavior of the MAO coating and composite coatings in different corrosive media and different corrosion stages. The results showed that the MAO coating and composite coatings showed some similarity corrosion electrochemical behavior and some different characteristics in 3.5-wt.%NaCl,3.5-wt.%Na2SO4 and simulated sea water solution. Corrosion control process would change in different corrosive media and different corrosion stages.
Finally, colored composite coatings were successfully prepared on the magnesium alloy. The structure, morphologies, corrosion resistance and corrosion mechanism of colored composite coatings were analyzed by SEM, EDS, FT-IR, polarization curves and cyclic anodic polarization curve. The results showed that the color composite coatings had smooth surface and better appearance. In particular, add CuSO4·5H2O colored composite coatings had the best corrosion resistance.
本文首先采用单因素实验和正交实验,系统讨论了微弧氧化电解液中主成膜剂、辅助成膜剂、添加剂等成分及其浓度对微弧氧化过程和膜层性能的影响,开发出了一种绿色环保型的镁合金微弧氧化电解液体系,并分析了各成分在镁合金微弧氧化过程中所起的作用。所开发出的绿色环保型镁合金微弧氧化电解液体系为：铝酸钠30g/dm3,氢氧化钠20g/dm3,蒙脱石3g/dm3,阿拉伯树胶2g/dm3。
采用田口实验设计方法,研究了工艺参数对微弧氧化膜表面形貌和耐蚀性的影响,优化了微弧氧化过程工艺参数。通过扫描电镜、能谱、X衍射、极化曲线和交流阻抗等测试方法,分析了微弧氧化膜的形貌、组成、结构和耐腐蚀性能。结果表明,最佳微弧氧化工艺条件为：终止电压180V,氧化时间30min,脉冲频率50Hz,占空比30%。优化工艺下所制备的微弧氧化膜为多孔结构,A1、O元素含量较高,膜层主要由MgO.MgAl2O4和Al12Mg17组成,耐腐蚀性能比AZ91D镁合金基体有了一定程度的提高。
在镁合金微弧氧化的基础上,采用微弧氧化与溶胶凝胶技术相结合,在镁合金微弧氧化膜表面制备出了具有一定厚度的溶胶凝胶层,形成复合膜层。通过扫描电镜、能谱、X衍射、差热-热重、红外光谱、极化曲线、交流阻抗和循环阳极极化曲线等分析测试方法,优化了溶胶制备工艺和溶胶凝胶层沉积工艺,系统研究了复合膜的形貌、组成、结构等特征及其耐蚀性。结果表明,最佳溶胶制备工艺为：Si：Zr摩尔比为2：1,水浴时间30min,水浴温度50℃,pH值为3。最佳溶胶凝胶膜层沉积工艺为：采用凝胶化工艺处理,干燥温度控制在80℃右,干燥时间1h,固化温度150℃,固化时间0.5h,浸涂次数3次。优化工艺下所制备的复合膜为微晶与玻璃态的混合结构,表面微观缺陷较少,结合力和致密性都较好,具有较强的耐蚀性。
研究了微弧氧化膜的生长过程,分析了处于不同生长阶段氧化膜的形貌、成分和耐蚀性。首次采用Gaussian03分析软件,计算了溶胶凝胶层吸附前后体系中的相关键长、荷电状态和结合能,从分子或原子水平上分析了复合膜层间的结合状态。结果表明,处于不同生长阶段氧化膜的结构形貌与其耐蚀性具有对应关系。溶胶凝胶膜在微弧氧化膜表面的吸附更加稳定,复合膜的层间结合力较好,为在AZ91D镁合金表面制备高性能的防腐蚀涂层提供了一定的理论依据。
使用极化曲线与交流阻抗技术,深入研究了微弧氧化膜和复合膜在不同腐蚀介质中的腐蚀扩展过程。并针对性的建立了不同的等效电路模型,对微弧氧化膜和复合膜在不同腐蚀介质和不同腐蚀时期的腐蚀行为进行了详细的分析。结果表明,在3.5%氯化钠溶液、3.5%硫酸钠溶液和模拟海水溶液中,微弧氧化膜和复合膜表现出某些相似的腐蚀电化学行为,也出现一些不同的特征。在不同的腐蚀介质以及不同的腐蚀时期,腐蚀控制过程会发生改变。
最后,在镁合金表面成功制备了有色复合膜层,并采用扫描电镜、能谱、红外光谱、极化曲线和循环阳极极化曲线等分析测试方法,探讨了有色复合膜的结构形貌、耐腐蚀性能和耐蚀机理。结果表明,本文所制备的有色复合膜表面光滑,着色效果较好。其中添加CuSO4·5H2O所制备出的有色复合膜耐腐蚀性能最好。
Magnesium alloy is one of the most light weight metal structure materials. Their potential applied fields include automobile, aerospace and consuming electronics, etc. However, the extensive use of magnesium alloys is limited due to poor corrosion resistance. Micro-arc oxidation (MAO) technique is one of the most favorable method in the surface treatment of magnesium alloys in recent years. It is a surface treatment technique developed from the common anodic oxidation. By use of this technique, a ceramic coating can be in situ formed on Al, Mg, Ti and their alloys. This enhances the corrosion resistance and abrasion resistance of the magnesium alloy. Unfortunately, there exist micropores and microcracks in the MAO coating. Usually, the two types of electrolyte solution apply to the micro-arc oxidation of magnesium alloy. One of the electrolyte contains Cr(VI) compounds, the other of the electrolyte contains phosphate and/or fluoride. Both of them contains the poisonous ingredients, such as chromate, phosphate, fluoride which do harm to environment and human beings. Therefore, it is essential that environment-friendly electrolyte system was developed and the effects of all kinds of process parameters on the formation and properties of anodic films were investigated. To further enhance the corrosion resistance of magnesium alloys and improve the structure of MAO coating, the composite coatings were prepared on magnesium alloy. The relationship between structure and performance of the composite coatings, and the binding mechanism between the sol-gel layer and MAO layer were studied.
In this paper, single factor and orthogonal layout experiment were applied. The effects of main film-forming agent, auxiliary film-forming agent, additives and their concentration on MAO process and film properties were discussed in the system. An environment-friendly MAO electrolyte system was developed as following,30g/dm3 NaAl2O4, 20g/dm3 NaOH,3g/dm3 montmorillonite, 2g/dm3 gum arabic. And the function of single electrolyte in MAO process was analyzed.
The effects of process parameters on surface morphologies and corrosion resistance of MAO coating were systematically investigated using the Taguchi experimental analysis method of four factors with three levels. The optimized parameters were 180V voltage,30min treatment time,50Hz frequency,30%duty cycle. The morphology, components, structure and corrosion resistance of MAO coating were examined by means of SEM, EDS, XRD, potentiodynamic polarization and AC impedance. The results showed that the MAO coating was a uniform distribution of porous structure. The components of aluminium and oxygen were higher, and the microstructure of the coating consisted of MgO、MgAl2O4and Al12Mg17 phases. Compared with the untreated magnesium alloy, the MAO coating exhibited higher corrosion resistance.
Based on micro-arc oxidation, a process of MAO combined with a sol-gel method was used to prepare composite coatings on magnesium alloy AZ91D. The composite coatings were formed using multi immersion technique to plus a sol-gel layer on the MAO coating. SEM, EDS, XRD, DSC-TGA, FT-IR, potentiodynamic polarization, AC impedance and cyclic anodic polarization curve were used to evaluate the morphologies, components, structure and corrosion resistance of composite coatings. The results showed that the optimum sol preparation process were Si:Zr molar ratio of 2:1, water bath time was 30min, temperature was 50℃, pH value was 3. The optimum sol-gel film deposition conditions were obtained as following, dipping times was 3, drying temperature was controlled about 80℃, drying time was 1h, curing temperature and curing time were 150℃and 0.5h, respectively. The structure of composite coatings was microcrystalline and glass. The composite coatings were more compact and had good adhesion. Few tiny cracks were visible on the surface layer. The corrosion resistance of the composite coatings was enhanced significantly.
The morphology, composition and corrosion resistance of oxide film at different growth stages were studied. Gaussian03 analysis software firstly used to calculate the bond length, charge and binding energy of adsorption system. The bound state of the coatings was analyzed in molecular level. The results showed that the structure characteristics and the corrosion resistance of oxide film at different growth stages had a corresponding relationship. Sol-gel layer of the MAO coating surface in the adsorption was more stable. For the preparation of high-performance anti-corrosion coating on AZ91D magnesium alloy provided a theoretical basis.
It was researched the corrosion development process of the MAO coating and the composite coatings in various corrosive media by using polarization curves and AC impedance techniques. Then different equivalent circuits were put forward to detailed describe the corrosion behavior of the MAO coating and composite coatings in different corrosive media and different corrosion stages. The results showed that the MAO coating and composite coatings showed some similarity corrosion electrochemical behavior and some different characteristics in 3.5-wt.%NaCl,3.5-wt.%Na2SO4 and simulated sea water solution. Corrosion control process would change in different corrosive media and different corrosion stages.
Finally, colored composite coatings were successfully prepared on the magnesium alloy. The structure, morphologies, corrosion resistance and corrosion mechanism of colored composite coatings were analyzed by SEM, EDS, FT-IR, polarization curves and cyclic anodic polarization curve. The results showed that the color composite coatings had smooth surface and better appearance. In particular, add CuSO4·5H2O colored composite coatings had the best corrosion resistance.
引文
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