镁锂基合金腐蚀特性及其表面涂层制备研究
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摘要
镁锂合金作为目前最轻的金属结构材料，密度仅为1.35-1.65g/cm3，除了具有超轻质特性外，镁锂合金还具有高比强度、高比刚度、电磁屏蔽性能好和导热导电性能好等优点，因此，镁锂合金被认为是目前在航空航天、武器装备、电子器材、交通装备、体育用品器材等领域具有广泛应用前景的先进材料之一。然而，由于镁锂合金中主体元素镁和锂均是非常活泼的元素，使得此合金的活性较高，耐腐蚀性能较差，这已成为制约镁锂合金在相关领域获得广泛应用的关键难题之一。
本论文在研究三种常见相组成镁锂合金的腐蚀特性的基础上，分别采用熔盐置换扩散法和微弧氧化法在镁锂合金表面制备铝金属涂层和微弧氧化陶瓷膜，分别优化了表面处理工艺，并对熔盐置换扩散法制备铝金属涂层的热力学和动力学进行了分析，研究微弧氧化表面处理过程中分别利用铝酸钠和铝溶胶作为电解液添加剂对微弧氧化膜的影响。具体研究内容和获得的相关研究结果如下：
对于三种具有典型组织的镁锂合金（LAZ532、LAZ832、LAZ1432）分别进行了显微组织、耐腐蚀性能和高温氧化行为等方面的对比研究。采用金相照片、XRD等对三种合金进行显微分析表明，LAZ532由(Mg)和AlLi相组成，AlLi相呈层片状并以网状分布于(Mg)基体晶界上，有少量分布于晶内；LAZ832由(Mg)、(Li)和AlLi相组成，AlLi相呈颗粒状分布于β(Li)相内；LAZ1432由(Li)和AlLi相组成，AlLi相呈块状分布于粗大的(Li)相基体中；采用析氢测试、失重测试、电化学极化曲线测试等方式对三种合金的腐蚀特性进行表征表明，三种镁锂合金的耐腐蚀性能均较差，并且合金的抗腐蚀能力随着锂含量的增加而降低，即耐腐蚀能力的顺序为：LAZ532>LAZ832>LAZ1432，三种合金的腐蚀电流密度基本各相差一个数量级；把三种镁锂合金在25-225℃条件下经0-24小时高温氧化，并对氧化后合金表面进行显微观察、腐蚀失重测试和电化学测试，结果表明，LAZ1432合金氧化最严重，LAZ832其次，LAZ532合金氧化程度最轻。在这些合金中存在的各种物相中，β(Li)相最易被氧化，AlLi相其次，(Mg)相最不易被氧化。经过高温氧化后的三组合金试样的耐腐蚀性能相比对应裸样具有一定的提升，但是随着时间的推移，合金表面的氧化膜会被破坏，腐蚀速度会有所增加。LAZ1432表面氧化膜存在孔洞，其腐蚀速率明显高于其它合金成分的腐蚀试样。
采用熔盐置换扩散法对LAZ532镁锂合金进行表面合金化涂层制备，制备过程在等摩尔熔盐体系（AlCl3:NaCl=1:1）中进行处理，温度范围300~400℃，处理时间2~8h。在合金表面获得了富铝的合金化层，厚度在10μm左右，合金化层与基体为冶金结合。合金化层主要以Mg17Al12（γ相）组成，还有少量的镁、锂、铝之间的固溶体。经过处理的合金的耐腐蚀性能均有一定程度的提高，其中350℃+8h处理条件下获得的合金化涂层耐腐蚀能最好，自腐蚀电位提高0.2V，自腐蚀电流降低一个数量级，连续的γ相阻碍了合金基体的进一步腐蚀。对涂层形成的热力学和动力学进行理论分析表明，合金化层的形成包括置换、扩散、相变三个过程。
为获得镁锂合金表面陶瓷涂层，对LAZ832镁锂合金进行了微弧氧化处理，优化了硅酸盐电解液体系中微弧氧化的工艺条件，并初步研究了向电解液中添加铝酸钠或铝溶胶作为添加剂时对膜层的影响。研究表明，在硅酸盐电解液体系中优化的工艺条件为：九水硅酸钠4g；氢氧化钠5g；十水四硼酸钠3g；蒸馏水1L；正向占空比：20%；电流大小：0.3A。在此工艺下制备的涂层使腐蚀电流密度降低了大约两个数量级；铝酸钠添加剂的引入可降低电解液的电导率，使得氧化膜表面微孔的数目明显减少，膜厚增加，膜的电阻率提高，但对耐腐蚀性能提高并没有益处。当加入铝溶胶后微弧氧化膜表面单位面积内微孔的数目及孔径明显减少，随着铝溶胶的增加，电阻也有所增加，微弧氧化膜的耐腐蚀性能也有所提高，极化电阻也逐渐变大。当铝溶胶的添加量为7ml/600ml时，微弧氧化膜的耐腐蚀性能最好。
As the lightest structural materials, Mg-Li alloys possess low densities of1.35-1.65g/cm3. Besides the superlight property, Mg-Li alloys have some other advantages, such ashigh specific strength, high specific stiffness, good property of electromagnetic shielding,good heat-conductivity and electricity-conductivity, etc. Therefore, Mg-Li alloy is deemed asone of prospective advanced materials having wide applications in the fields of aerospace,weapon equipment, electric equipment, traffic equipment, and sports equipment, etc. However,Mg and Li, which are the two main elements in Mg-Li alloys, are both very active. Thismakes Mg-Li base alloys very active with poor corrosion resistance, which becomes the keyproblem restricting the wide application of Mg-Li alloys.
In this dissertation, the corrosion characteristics of three common Mg-Li base alloys withdifferent phase compositon are studied. Then two surface treatment methods, molten saltsubstitution and diffusion and micro-arc oxidation, are used to prepare coatings on Mg-Libase alloys. Besides the parameters optimizations for these two methods, the thermodynamicsand dynamics of the aluminum diffusion during the process of molten salt substitution anddiffusion are studied. The effects of the additives, sodium aluminate and alumina sol. on theprocess of micro-arc oxidation are also studied. The research content and the results are asfollow:
The microstructure, corrosion resistance and high temperature oxidization behavior ofthree common Mg-Li base alloys, LAZ532, LAZ832and LAZ1432, are researched. OM andXRD analysis show that, LAZ532is composed of (Mg) and AlLi. AlLi phase mainly existsat the grain boundary of (Mg) in the form of reticulation, and a small amount of it exists atthe inner of (Mg) grains. In LAZ832, there are (Mg),(Li) and AlLi. AlLi exists in the
(Li) in the form of particle. In LAZ1432, there are (Li) and AlLi. AlLi phase exists in thelarge scale (Li) in the form of block. Hydrogen evolution, weight loss, electrochemicalpotentiodynamic polarization, et al. are used to evalute the corrosion characteristics of thethree Mg-Li base alloys. Results show that the three Mg-Li base alloys all possess poorcorrosion resistance. With the increase of Li content, the corrosion resistance becomes poorerand poorer. The sequence of the corrosion resistant capability of the three alloys is: LAZ532>LAZ832>LAZ1432. The corrosive electric current density difference among thethree alloys is about one order of magnitude. The high temperature oxidations of the threealloys were carried at25-225℃for0-24hours. Results show that, as for the oxidationresistance, LAZ532is best, LAZ832is the second, and LAZ1432is the poorest. Comparingthe phases in the three alloys,(Mg) phase possesses the best oxidation resistance, AlLi phaseis the second, and β(Li) phase is the poorest. After hight temperature oxidation, the corrosionresistances of the three alloys are all better than those of the alloys before oxidaiton. However,with the increase of corrosion time, the oxide film will be destroyed, making the corrosionrate increase. Among the three alloys, the corrosion rate of LAZ1432after high temperatureoxidation is obviously higher than those of LAZ532and LAZ832, because of many cavitiesexisting in the oxide film of LAZ1432.
Molten salt substitution and diffusion treatment was used to prepare metallic coat onLAZ532. The opitimized parameters are listed as follow: molten salt composition(AlCl3:NaCl=1:1, mol. ratio), temperature (300~400℃), treatment time (2-8h). Under theseexperimental parameters, a good Al-riched alloy layer with a thickness of about10μm can beprepared on the surface of LAZ532. The bonding between the alloy layer and LAZ532ismetallurgical bonding. The alloy layer is mainly composed of Mg17Al12, and small amount ofsolid solution with the elements of Mg, Li and Al. Temperature and treatment time are twoimportant parameters affecting the formation of diffusion layer.350℃+8his goog parameters.After treatment, the corrosion resistance of the alloy is improved obviously. The corrosionpotential increases by0.2V, and the corrosion current deceases by one order of magnitude.The corrosion resistance improvement can be attributed to the continuous Mg17Al12, whichcan hinder the matrix alloy from further corrosion. The formation of alloy layer includes threeprocesses, substitution, diffusion and phase transformation.
To botain a ceramic coat on Mg-Li alloy, micro-arc oxidization treatment was carried inthe silicate electrolyte. The effects of the additives of sodium aluminate and alumina sol onthe film were also researched. The optimization parameters are listed as follow:Na2SiO3·9H2O4g, NaOH5g, Na2B4O7·10H2O3g, distilled water1L, positive duty rate20%,electric current0.3A. After the micro-arc oxidization treatment with these parameters, thecorrosion current of the alloy decreases by two orders of magnitude compared with the alloywithout surface treatment. When the sodium aluminate is added in silicate electrolyte, the electric conductivity of the electrolyte will decrease, and the amount of micro-pores on theoxidation film will decrease obviously. With the increase of sodium aluminate content, thethickness and electric resistivity of film both increase, although the corrosion resistance of theoxidation film does not improve obviously. When the sodium aluminate content is2g/L, thecorrosion resistance of the corresponding oxidation film is the best. When alumina sol isadded into electrolyte, the amount and size of pores on the micro-arc oxidation film bothdecrease obviously. With the increase of alumina sol content, electric resistivity of the filmincreases, and the corrosion resistance of the film is also improved. When the alumina solcontent is7ml/600ml, the corrosion resistance of the corresponding film is the best.
本论文在研究三种常见相组成镁锂合金的腐蚀特性的基础上，分别采用熔盐置换扩散法和微弧氧化法在镁锂合金表面制备铝金属涂层和微弧氧化陶瓷膜，分别优化了表面处理工艺，并对熔盐置换扩散法制备铝金属涂层的热力学和动力学进行了分析，研究微弧氧化表面处理过程中分别利用铝酸钠和铝溶胶作为电解液添加剂对微弧氧化膜的影响。具体研究内容和获得的相关研究结果如下：
对于三种具有典型组织的镁锂合金（LAZ532、LAZ832、LAZ1432）分别进行了显微组织、耐腐蚀性能和高温氧化行为等方面的对比研究。采用金相照片、XRD等对三种合金进行显微分析表明，LAZ532由(Mg)和AlLi相组成，AlLi相呈层片状并以网状分布于(Mg)基体晶界上，有少量分布于晶内；LAZ832由(Mg)、(Li)和AlLi相组成，AlLi相呈颗粒状分布于β(Li)相内；LAZ1432由(Li)和AlLi相组成，AlLi相呈块状分布于粗大的(Li)相基体中；采用析氢测试、失重测试、电化学极化曲线测试等方式对三种合金的腐蚀特性进行表征表明，三种镁锂合金的耐腐蚀性能均较差，并且合金的抗腐蚀能力随着锂含量的增加而降低，即耐腐蚀能力的顺序为：LAZ532>LAZ832>LAZ1432，三种合金的腐蚀电流密度基本各相差一个数量级；把三种镁锂合金在25-225℃条件下经0-24小时高温氧化，并对氧化后合金表面进行显微观察、腐蚀失重测试和电化学测试，结果表明，LAZ1432合金氧化最严重，LAZ832其次，LAZ532合金氧化程度最轻。在这些合金中存在的各种物相中，β(Li)相最易被氧化，AlLi相其次，(Mg)相最不易被氧化。经过高温氧化后的三组合金试样的耐腐蚀性能相比对应裸样具有一定的提升，但是随着时间的推移，合金表面的氧化膜会被破坏，腐蚀速度会有所增加。LAZ1432表面氧化膜存在孔洞，其腐蚀速率明显高于其它合金成分的腐蚀试样。
采用熔盐置换扩散法对LAZ532镁锂合金进行表面合金化涂层制备，制备过程在等摩尔熔盐体系（AlCl3:NaCl=1:1）中进行处理，温度范围300~400℃，处理时间2~8h。在合金表面获得了富铝的合金化层，厚度在10μm左右，合金化层与基体为冶金结合。合金化层主要以Mg17Al12（γ相）组成，还有少量的镁、锂、铝之间的固溶体。经过处理的合金的耐腐蚀性能均有一定程度的提高，其中350℃+8h处理条件下获得的合金化涂层耐腐蚀能最好，自腐蚀电位提高0.2V，自腐蚀电流降低一个数量级，连续的γ相阻碍了合金基体的进一步腐蚀。对涂层形成的热力学和动力学进行理论分析表明，合金化层的形成包括置换、扩散、相变三个过程。
为获得镁锂合金表面陶瓷涂层，对LAZ832镁锂合金进行了微弧氧化处理，优化了硅酸盐电解液体系中微弧氧化的工艺条件，并初步研究了向电解液中添加铝酸钠或铝溶胶作为添加剂时对膜层的影响。研究表明，在硅酸盐电解液体系中优化的工艺条件为：九水硅酸钠4g；氢氧化钠5g；十水四硼酸钠3g；蒸馏水1L；正向占空比：20%；电流大小：0.3A。在此工艺下制备的涂层使腐蚀电流密度降低了大约两个数量级；铝酸钠添加剂的引入可降低电解液的电导率，使得氧化膜表面微孔的数目明显减少，膜厚增加，膜的电阻率提高，但对耐腐蚀性能提高并没有益处。当加入铝溶胶后微弧氧化膜表面单位面积内微孔的数目及孔径明显减少，随着铝溶胶的增加，电阻也有所增加，微弧氧化膜的耐腐蚀性能也有所提高，极化电阻也逐渐变大。当铝溶胶的添加量为7ml/600ml时，微弧氧化膜的耐腐蚀性能最好。
As the lightest structural materials, Mg-Li alloys possess low densities of1.35-1.65g/cm3. Besides the superlight property, Mg-Li alloys have some other advantages, such ashigh specific strength, high specific stiffness, good property of electromagnetic shielding,good heat-conductivity and electricity-conductivity, etc. Therefore, Mg-Li alloy is deemed asone of prospective advanced materials having wide applications in the fields of aerospace,weapon equipment, electric equipment, traffic equipment, and sports equipment, etc. However,Mg and Li, which are the two main elements in Mg-Li alloys, are both very active. Thismakes Mg-Li base alloys very active with poor corrosion resistance, which becomes the keyproblem restricting the wide application of Mg-Li alloys.
In this dissertation, the corrosion characteristics of three common Mg-Li base alloys withdifferent phase compositon are studied. Then two surface treatment methods, molten saltsubstitution and diffusion and micro-arc oxidation, are used to prepare coatings on Mg-Libase alloys. Besides the parameters optimizations for these two methods, the thermodynamicsand dynamics of the aluminum diffusion during the process of molten salt substitution anddiffusion are studied. The effects of the additives, sodium aluminate and alumina sol. on theprocess of micro-arc oxidation are also studied. The research content and the results are asfollow:
The microstructure, corrosion resistance and high temperature oxidization behavior ofthree common Mg-Li base alloys, LAZ532, LAZ832and LAZ1432, are researched. OM andXRD analysis show that, LAZ532is composed of (Mg) and AlLi. AlLi phase mainly existsat the grain boundary of (Mg) in the form of reticulation, and a small amount of it exists atthe inner of (Mg) grains. In LAZ832, there are (Mg),(Li) and AlLi. AlLi exists in the
(Li) in the form of particle. In LAZ1432, there are (Li) and AlLi. AlLi phase exists in thelarge scale (Li) in the form of block. Hydrogen evolution, weight loss, electrochemicalpotentiodynamic polarization, et al. are used to evalute the corrosion characteristics of thethree Mg-Li base alloys. Results show that the three Mg-Li base alloys all possess poorcorrosion resistance. With the increase of Li content, the corrosion resistance becomes poorerand poorer. The sequence of the corrosion resistant capability of the three alloys is: LAZ532>LAZ832>LAZ1432. The corrosive electric current density difference among thethree alloys is about one order of magnitude. The high temperature oxidations of the threealloys were carried at25-225℃for0-24hours. Results show that, as for the oxidationresistance, LAZ532is best, LAZ832is the second, and LAZ1432is the poorest. Comparingthe phases in the three alloys,(Mg) phase possesses the best oxidation resistance, AlLi phaseis the second, and β(Li) phase is the poorest. After hight temperature oxidation, the corrosionresistances of the three alloys are all better than those of the alloys before oxidaiton. However,with the increase of corrosion time, the oxide film will be destroyed, making the corrosionrate increase. Among the three alloys, the corrosion rate of LAZ1432after high temperatureoxidation is obviously higher than those of LAZ532and LAZ832, because of many cavitiesexisting in the oxide film of LAZ1432.
Molten salt substitution and diffusion treatment was used to prepare metallic coat onLAZ532. The opitimized parameters are listed as follow: molten salt composition(AlCl3:NaCl=1:1, mol. ratio), temperature (300~400℃), treatment time (2-8h). Under theseexperimental parameters, a good Al-riched alloy layer with a thickness of about10μm can beprepared on the surface of LAZ532. The bonding between the alloy layer and LAZ532ismetallurgical bonding. The alloy layer is mainly composed of Mg17Al12, and small amount ofsolid solution with the elements of Mg, Li and Al. Temperature and treatment time are twoimportant parameters affecting the formation of diffusion layer.350℃+8his goog parameters.After treatment, the corrosion resistance of the alloy is improved obviously. The corrosionpotential increases by0.2V, and the corrosion current deceases by one order of magnitude.The corrosion resistance improvement can be attributed to the continuous Mg17Al12, whichcan hinder the matrix alloy from further corrosion. The formation of alloy layer includes threeprocesses, substitution, diffusion and phase transformation.
To botain a ceramic coat on Mg-Li alloy, micro-arc oxidization treatment was carried inthe silicate electrolyte. The effects of the additives of sodium aluminate and alumina sol onthe film were also researched. The optimization parameters are listed as follow:Na2SiO3·9H2O4g, NaOH5g, Na2B4O7·10H2O3g, distilled water1L, positive duty rate20%,electric current0.3A. After the micro-arc oxidization treatment with these parameters, thecorrosion current of the alloy decreases by two orders of magnitude compared with the alloywithout surface treatment. When the sodium aluminate is added in silicate electrolyte, the electric conductivity of the electrolyte will decrease, and the amount of micro-pores on theoxidation film will decrease obviously. With the increase of sodium aluminate content, thethickness and electric resistivity of film both increase, although the corrosion resistance of theoxidation film does not improve obviously. When the sodium aluminate content is2g/L, thecorrosion resistance of the corresponding oxidation film is the best. When alumina sol isadded into electrolyte, the amount and size of pores on the micro-arc oxidation film bothdecrease obviously. With the increase of alumina sol content, electric resistivity of the filmincreases, and the corrosion resistance of the film is also improved. When the alumina solcontent is7ml/600ml, the corrosion resistance of the corresponding film is the best.
引文
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