铝合金表面钛/锆转化膜的着色及性能优化
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摘要
本论文以氟钛酸和氟锆酸为主要组分，以单宁酸为着色剂，以锰盐为成膜促进剂在铝合金表面制备出了耐蚀性能优异的金黄色转化膜，并对转化膜的耐蚀性能、成膜机理和显色原因进行了分析。具体研究工作主要包括以下五个方面：
（1）以氟钛酸和氟锆酸为基础配方，添加成膜促进剂和着色剂，制备了金黄色的钛/锆系转化膜，对其进行粉末喷涂后的漆膜按照铝合金建筑型材国家标准《GB5237.4-2004第4部分粉末喷涂型材》进行测试，完全符合标准要求，具备了工业化应用的条件。
（2）最优工艺条件制备的转化膜腐蚀电流密度由基体的5.894A·cm-2下降到0.083A·cm-2，盐雾实验160h时无腐蚀，360h的腐蚀面积约占总面积的60%，超过铬酸盐的耐蚀水平。电化学交流阻抗谱表明添加成膜促进剂锰盐，使得膜层更加致密、均匀，耐蚀性能提高。
（3）对转化膜的组织结构进行了分析，结果表明，转化膜的主要成分均为Na_3AlF_6，其次是单宁酸水解产物与金属离子形成的络合物以及少量TiO_2、Al_2O_3·3H_2O等。转化膜具有双层结构，外层主要是单宁酸水解产物与金属离子形成的有机络合物，内层主要是Na_3AlF_6。
（4）转化膜的形成可以分为Na_3AlF_6晶核形成、生长、金属有机络合物沉积三个阶段：在成核阶段，Na_3AlF_6晶核在铝基体表面形成，晶体的大小不一，零星分布在基体表面；在生长阶段，晶体不断长大并形成连续转化膜覆盖了整个基体；在金属有机络合物沉积阶段，溶液中由单宁酸水解得到的三羟基苯甲酸与金属离子反应形成金属络合物并逐渐覆盖在Na_3AlF_6晶体层表面，金属有机络合物的存在使转化膜呈现出了金黄色。
（5）分析了F-和Mn~(2+)在成膜过程中的作用。由于F-的屏蔽作用，从基体上溶解下来的Al~(3+)来不及扩散到溶液中就和附近的F-反应生成配位离子AlF_6~(3-)，阻碍了Al(OH)_3沉淀生成。Mn~(2+)的加入改变了转化膜的形貌，成膜速度加快，耐蚀性能进一步提高，但成膜机理以及膜层结构没有变化，在溶液中Mn~(2+)被氧化成MnOOH并沉积在基体表面为Na_3AlF_6形成提供晶核，加速Na_3AlF_6成核、生长，从而加快了成膜速度；同时由于MnOOH晶核的存在，改变了Na_3AlF_6晶体的取向，使转化膜的微观形貌发生了变化。
A golden conversion coating on the surface of aluminum alloy which has excellentcorrosion resisting property was prepared by using the treatment solution containing H2TiF6and H2ZrF6as essential component, tannic acid as the coloring agent, Mn~(2+)as thecoating-forming accelerators. The corrosion resistance, coating-forming mechanism andcolored reason had been investigated deeply. The related results were as follows:
(1) The golden Ti/Zr conversion coating on the surface of aluminum alloy was obtainedthrough the treatment solutioin with H2TiF6and H2ZrF6as the main composites accompaniedwith the coloring agent and coating-forming accelerators. Powder spray experiment of thealuminium alloy after the treatment showed that the current prepared conversion coating metthe requirement of Part4of National Standard GB5237.4-2004of powder coating profiles,which means that the conversion coating technigue can be candidate for industrial application.
(2) The corrosion current density of the optimized conversion coating decreased to0.083uA·cm-2from5.894uA·cm-2of the substrate alloy. The surface of conversion coating was stillintact after160h salt spray test and the corrosion area about60%after360h. The resistancecorrosion of this conversion coating was better than that of chromate conversion coating. Theelectrochemical impedance spectroscopy research showed that conversion coating was muchmore compact and uniform and the corrosion resistance wss significantly increased when thecoating-forming accelerator Mn~(2+)was introduced into the treatment solution.
(3) Through the characterization to main components of the conversion coating, it wasshown that the main components of both conversion coating got in these two optimizedformulas was Na_3AlF_6, followed by the metal-organic complex, a little of Al_2O_3·3H_2O, TiO_2and so on. A double-layer structure was evidenced in the conversion coating. The outer layerconsists of the metal-organic complex which were formed by the reaction of gallic with Ti4+and Al~(3+), the inner layer was mainly made up of Na_3AlF_6.
(4)The formation mechanism of the conversion coating can be divided into three stages:the nucleation and the growth of Na_3AlF_6crystals and the formation of metal-organic complex.First, Na_3AlF_6crystals preferentially nucleate on the surface of the substrate. The Na_3AlF_6crystals present as ellipsoidal globules with different size. Then, the Na_3AlF_6crystallinegrains grow in sizes and nearly cover all of the substrate surfaces. At last, the metal-organiccomplex formed and covered the Na_3AlF_6crystals which made the conversion coating golden.
(5) The effect of Al~(3+)and F-had been analyzed. The Al~(3+)dissolved from the surface of thesubstrate and reacted with F-to form AlF_6~(3-)which prevented the precipitation of Al(OH)3. Mn~(2+)changed the morphology of conversion coating and accelerated the coating-forming andimproved the corrosion resistance further. However, the formation mechanism and coatingstructure was not changed. Mn~(2+)had a strong reducibility and was readily to be oxidized toMnOOH by O2in the solution，and the MnOOH deposited on the substrate surface as thenucleation for the Na_3AlF_6deposition, which accelerated the growth speed of thecoating-forming. MnOOH nucleation may change the orientation of Na_3AlF_6crystal and thuschange the morphology of conversion coating.
（1）以氟钛酸和氟锆酸为基础配方，添加成膜促进剂和着色剂，制备了金黄色的钛/锆系转化膜，对其进行粉末喷涂后的漆膜按照铝合金建筑型材国家标准《GB5237.4-2004第4部分粉末喷涂型材》进行测试，完全符合标准要求，具备了工业化应用的条件。
（2）最优工艺条件制备的转化膜腐蚀电流密度由基体的5.894A·cm-2下降到0.083A·cm-2，盐雾实验160h时无腐蚀，360h的腐蚀面积约占总面积的60%，超过铬酸盐的耐蚀水平。电化学交流阻抗谱表明添加成膜促进剂锰盐，使得膜层更加致密、均匀，耐蚀性能提高。
（3）对转化膜的组织结构进行了分析，结果表明，转化膜的主要成分均为Na_3AlF_6，其次是单宁酸水解产物与金属离子形成的络合物以及少量TiO_2、Al_2O_3·3H_2O等。转化膜具有双层结构，外层主要是单宁酸水解产物与金属离子形成的有机络合物，内层主要是Na_3AlF_6。
（4）转化膜的形成可以分为Na_3AlF_6晶核形成、生长、金属有机络合物沉积三个阶段：在成核阶段，Na_3AlF_6晶核在铝基体表面形成，晶体的大小不一，零星分布在基体表面；在生长阶段，晶体不断长大并形成连续转化膜覆盖了整个基体；在金属有机络合物沉积阶段，溶液中由单宁酸水解得到的三羟基苯甲酸与金属离子反应形成金属络合物并逐渐覆盖在Na_3AlF_6晶体层表面，金属有机络合物的存在使转化膜呈现出了金黄色。
（5）分析了F-和Mn~(2+)在成膜过程中的作用。由于F-的屏蔽作用，从基体上溶解下来的Al~(3+)来不及扩散到溶液中就和附近的F-反应生成配位离子AlF_6~(3-)，阻碍了Al(OH)_3沉淀生成。Mn~(2+)的加入改变了转化膜的形貌，成膜速度加快，耐蚀性能进一步提高，但成膜机理以及膜层结构没有变化，在溶液中Mn~(2+)被氧化成MnOOH并沉积在基体表面为Na_3AlF_6形成提供晶核，加速Na_3AlF_6成核、生长，从而加快了成膜速度；同时由于MnOOH晶核的存在，改变了Na_3AlF_6晶体的取向，使转化膜的微观形貌发生了变化。
A golden conversion coating on the surface of aluminum alloy which has excellentcorrosion resisting property was prepared by using the treatment solution containing H2TiF6and H2ZrF6as essential component, tannic acid as the coloring agent, Mn~(2+)as thecoating-forming accelerators. The corrosion resistance, coating-forming mechanism andcolored reason had been investigated deeply. The related results were as follows:
(1) The golden Ti/Zr conversion coating on the surface of aluminum alloy was obtainedthrough the treatment solutioin with H2TiF6and H2ZrF6as the main composites accompaniedwith the coloring agent and coating-forming accelerators. Powder spray experiment of thealuminium alloy after the treatment showed that the current prepared conversion coating metthe requirement of Part4of National Standard GB5237.4-2004of powder coating profiles,which means that the conversion coating technigue can be candidate for industrial application.
(2) The corrosion current density of the optimized conversion coating decreased to0.083uA·cm-2from5.894uA·cm-2of the substrate alloy. The surface of conversion coating was stillintact after160h salt spray test and the corrosion area about60%after360h. The resistancecorrosion of this conversion coating was better than that of chromate conversion coating. Theelectrochemical impedance spectroscopy research showed that conversion coating was muchmore compact and uniform and the corrosion resistance wss significantly increased when thecoating-forming accelerator Mn~(2+)was introduced into the treatment solution.
(3) Through the characterization to main components of the conversion coating, it wasshown that the main components of both conversion coating got in these two optimizedformulas was Na_3AlF_6, followed by the metal-organic complex, a little of Al_2O_3·3H_2O, TiO_2and so on. A double-layer structure was evidenced in the conversion coating. The outer layerconsists of the metal-organic complex which were formed by the reaction of gallic with Ti4+and Al~(3+), the inner layer was mainly made up of Na_3AlF_6.
(4)The formation mechanism of the conversion coating can be divided into three stages:the nucleation and the growth of Na_3AlF_6crystals and the formation of metal-organic complex.First, Na_3AlF_6crystals preferentially nucleate on the surface of the substrate. The Na_3AlF_6crystals present as ellipsoidal globules with different size. Then, the Na_3AlF_6crystallinegrains grow in sizes and nearly cover all of the substrate surfaces. At last, the metal-organiccomplex formed and covered the Na_3AlF_6crystals which made the conversion coating golden.
(5) The effect of Al~(3+)and F-had been analyzed. The Al~(3+)dissolved from the surface of thesubstrate and reacted with F-to form AlF_6~(3-)which prevented the precipitation of Al(OH)3. Mn~(2+)changed the morphology of conversion coating and accelerated the coating-forming andimproved the corrosion resistance further. However, the formation mechanism and coatingstructure was not changed. Mn~(2+)had a strong reducibility and was readily to be oxidized toMnOOH by O2in the solution，and the MnOOH deposited on the substrate surface as thenucleation for the Na_3AlF_6deposition, which accelerated the growth speed of thecoating-forming. MnOOH nucleation may change the orientation of Na_3AlF_6crystal and thuschange the morphology of conversion coating.
引文
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