纯镁及镁合金大气腐蚀和化学氧化工艺研究
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摘要
镁合金具有比强度高、减震性能好、易于压铸成型和可回收等优良的综合性能，逐渐受到交通工具和电子通讯器材等行业的青睐，被认为是21世纪最富有开发和应用潜力的“绿色材料”。但是，耐蚀性问题一直制约着镁合金的大量使用。目前关于变形镁合金腐蚀行为的报道较少，对其腐蚀机理研究不够深入。同时，镁合金化学氧化技术中，铬酸盐化学氧化工艺存在废液处理成本高和污染环境等问题。而无铬处理工艺目前还不够成熟，处理液寿命短，氧化膜耐蚀性不够理想，能耗高，工艺复杂。因此，研究变形镁合金的腐蚀机理，开发高效、低毒、环境友好的化学氧化处理工艺成为当前研究热点之一。
本文对AZ31镁合金和纯镁暴露在大连地区海洋性气候中的腐蚀行为进行研究，同时进行室内模拟暴露实验和薄层液膜电化学检测，探讨了大气污染物对AZ31镁合金和纯镁腐蚀规律的影响。采用扫描电镜(SEM)、电子能谱(EDX)、电子探针(EPMA)以及X射线光电子能谱仪(XPS)等检测技术对表面腐蚀产物进行分析。400d的室外暴露实验结果表明，两种试样表面覆盖一层深灰色的腐蚀产物膜，AZ31镁合金表面腐蚀产物膜较纯镁光滑、致密，腐蚀程度较轻。去除腐蚀产物后发现，试样表面腐蚀轻微的区域形成了一些孤立的“小岛”，“小岛”之间出现较深的蚀坑。AZ31镁合金和纯镁腐蚀面积分别占各自总面积的42.3％和65.0％。AZ31镁合金表面腐蚀产物主要由MgO、Mg(OH)_2、Al(OH)_3、Al_2O_3以及镁和铝的碳酸盐，硫酸盐和氯化物所组成，纯镁腐蚀产物与AZ31镁合金基本相同，但不含Al元素。图像法统计腐蚀面积后拟合的AZ31镁合金和纯镁腐蚀动力学遵循指数关系，动力学方程分别为：H_(AZ31)=0.403×t~(0.653)，H_(pMg)=0.549×t~(0.665)。
室内模拟暴露实验研究发现，表面沉积NaCl、Na_2SO_4和NaNO_3后，AZ31镁合金和纯镁发生明显的局部腐蚀。随着表面盐沉积量的增加，腐蚀速度加快。NaCl、Na_2SO_4和NaNO_3对镁合金侵蚀性强度排序为：NaCl＞Na_2SO_4＞NaNO_3。薄层电解液中含有NaCl、Na_2SO_4和NaNO_3时的电化学测试表明，随着试样表面液层厚度的减薄，腐蚀产物的沉积速度加快导致腐蚀产物膜变得粗糙、疏松；液膜越薄，局部腐蚀越易发生。液膜较薄时，三种电解液中R_f和R_(ct)大小顺序为NaNO_3＞Na_2SO_4＞NaCl，表明其侵蚀性强度顺序为NaCl＞Na_2SO_4＞NaNO_3，验证了室内模拟暴露实验检测结果。此外，NaNO_3的液膜下，液膜厚度变化对镁合金极化行为的影响较NaCl和Na_2SO_4液膜下显著，这是由于阴极过程除了生成氢气外，还产生NO_3~-的去极化反应所致。
开发了一种KMnO_4-REMS化学氧化工艺，AZ91、AM60、AZ31镁合金以及纯镁经该工艺氧化处理后，获得的氧化膜质量优于磷酸盐处理等典型的无铬镁合金化学氧化处理工艺，与传统铬酸盐处理工艺相当。经KMnO_4-REMS工艺氧化后，镁合金表面氧化膜层呈网状微裂纹结构，氧化膜厚度约为10μm，膜层的主要成分为CeO_2、MnO和MnO_2，还有少量MgO、Mg(OH)_2以及铝的化合物。镁合金表面的KMnO_4-REMS氧化膜具有三层结构，最内层是镁和铝的氧化物和氢氧化物，中间层则主要由锰的氧化物组成，表层沉积了铈的氧化物。氧化膜表面的网状微裂纹结构在氧化过程中形成，由镁合金结构和化学氧化处理后干燥过程中氢氧化物脱水所造成。
为了解决氧化液存在的环境污染问题，本文对环保无毒的植酸氧化液在镁合金表面化学氧化工艺中的应用进行研究。发现植酸氧化液的最佳pH值范围为9～10，在AZ91、AM60、AZ31镁合金以及纯镁表面形成的氧化膜透明、光亮，膜层致密、均匀。经植酸处理后，在0.05mol·L~(-1)的NaCl溶液中耐蚀性能测试结果表明，镁及镁合金腐蚀电位升高，极化电流密度减小，电化学性能得到改善；化学浸泡8h未见腐蚀，耐蚀性能得到提高。植酸处理液在镁合金表面形成的氧化膜含有Mg、Al、Zn、O、P和C元素，膜的组成为植酸的镁盐和铝盐，以及镁和铝的氧化物和氢氧化物。植酸在镁合金表面发生化学吸附，形成一层致密的有机保护膜，膜层有效地阻滞活性离子向基体表面扩散，隔离基体与腐蚀介质，从而抑制镁合金腐蚀。
Magnesium alloys are of great importance at present and future fields of engineering for their attractive combination of low density and high strength/weight ratio. However, since magnesium is intrinsically active in the environment, the corrosion resistance of magnesium alloys is generally inadequate, which limits their application. In order to improve the corrosion resistance of magnesium alloys, surface treatment technologies, like chemical conversion, are commonly applied. Nowadays, the methods applied introduce chromate ions in the solutions, which is progressively restricted due to its high toxicity to the environment. The trend in the field is oriented to investigate the corrosion mechanism of magnesium alloy and develop environmental friendly chemical treatment technologies.
In this paper, the atmospheric corrosion behavior of extruded AZ31 magnesium alloy and pure magnesium samples is studied by weight loss test, electrochemical measurements and physical detection technologies, such as SEM, EDX, EPMA and XPS. After 400d atmospheric exposure station in Dalian city, the samples are covered with a plumbeous corrosion production film. Compared with pure magnesium sample, the film on AZ31 magnesium alloy is more compact. Moreover, after the corrosion production is wiped off, some insulated "island", which formed on the corrosion slightly area, are observed on the surface of the samples. The proportions of the corrosion region to the general area are 65.0% and 42.3% on AZ31 and pure magnesium, respectively. The compositiones of corrosion production on the two samples are almost similar. They are MgO, Mg(OH)_2, Al(OH)_3, Al_2O_3 and carbonate, sulfate and chloride of Mg and Al. The corrosion kinetics calculated by image methods accord with exponential equation and the dynamics equations for AZ31 and pure magnesium are H_(AZ31)=0.403×t~(0.653) and H_(PMg)=0.549×t~(0.665), respectively.
The effect of NaCl, Na_2SO_4 and NaNO_3 on the atmospheric corrosion of AZ31 magnesium alloy and pure magnesium samples was studied by the indoor simulated exposure experiment and electrochemical test under thin electrolyte layers. After 40d indoor simulated exposure station with the addition of NaCl, Na_2SO_4 and NaNO_3 on the surface of AZ31 and pure magnesium, the samples occur local corrosion. The corrosion rate of the samples increases with the salt concentratiom increasing. The aggressiveness of the salt is NaCl > Na_2SO_4> NaNO_3 Electrochemical tests under thin electrolyte layers show that decreasing the thickness of electrolyte layers results in accelerating corrosion rate. The thinner the layer is, the easier the occurrence of local corrosion on the samples is. The difference of the corrosion behaviors between in solution and under thin layer is mainly due to the dissolve of O_2 and CO_2 in the electrolyte. In addition, the NO_3~- is more sensitive to the thickness of the layer than Cl~- and SO_4~-, which is caused by the participation of NO_3~- in the cathodic depolarization.
In order to avoid high toxicity like Cr treatment to the environment and improve the corrosion resistance of magnesium alloys, KMnO_4-REMS chemical conversion treatment technique is developed in this paper. The conversion coatings obtained with this method show better corrosion resistance than previously used phosphate-based conversion treatment for AZ91, AM60, AZ31 and pure magnesium samples, and reach the levels of chrome-based treatment. Furthermore, the electrochemical polarization tests show that compared with the samples treated by chrome-based method, the anodic current density of the alloy coated in permanganate-REMS bath, at the same potential, decreases evidently in 0.05mol·L~(-1)NaCl solution. Simultaneously, the open-circuit potential of magnesium alloy increases 0.06V compared with blank samples. The thickness of the coating formed by the permanganate-REMS bath on AZ91 magnesium alloy is about 10μm and net-like cracks exists on the coatings. The conversion coating mainly composes of CeO_2, MnO, MnO_2, and some oxides of Mg and Al.
Phytic acid, as an environmental- friendly agent, has been growing applied in the application of metal surface treatments. In this paper, the corrosion protects afforded by phytic acid conversion coatings on magnesium and magnesium alloy has been developed. The results show that optimal pH range for the treatment is 9-10. In 0.05mol L~(-1)NaCl solutions, Magnesium alloy coated by phytic acid solution don't corrode until 8 hours. Simultaneously, compared with blank samples, the open-circuit potential of magnesium alloy treated by phytic acid solutin is increased and the anodic current density is decreased at the same potential. A compact film is found on the surface of magnesium alloy with the combination of phytic acids and the metal. The film is mainly composed of phytate and some oxides of Mg and Al. This film may insulate the metal from the deleterious anion, thus protect the magnesium alloy against corrosion. Moreover, by reacting to the paint, the phytic acid coating can improve the resin binding power.
本文对AZ31镁合金和纯镁暴露在大连地区海洋性气候中的腐蚀行为进行研究，同时进行室内模拟暴露实验和薄层液膜电化学检测，探讨了大气污染物对AZ31镁合金和纯镁腐蚀规律的影响。采用扫描电镜(SEM)、电子能谱(EDX)、电子探针(EPMA)以及X射线光电子能谱仪(XPS)等检测技术对表面腐蚀产物进行分析。400d的室外暴露实验结果表明，两种试样表面覆盖一层深灰色的腐蚀产物膜，AZ31镁合金表面腐蚀产物膜较纯镁光滑、致密，腐蚀程度较轻。去除腐蚀产物后发现，试样表面腐蚀轻微的区域形成了一些孤立的“小岛”，“小岛”之间出现较深的蚀坑。AZ31镁合金和纯镁腐蚀面积分别占各自总面积的42.3％和65.0％。AZ31镁合金表面腐蚀产物主要由MgO、Mg(OH)_2、Al(OH)_3、Al_2O_3以及镁和铝的碳酸盐，硫酸盐和氯化物所组成，纯镁腐蚀产物与AZ31镁合金基本相同，但不含Al元素。图像法统计腐蚀面积后拟合的AZ31镁合金和纯镁腐蚀动力学遵循指数关系，动力学方程分别为：H_(AZ31)=0.403×t~(0.653)，H_(pMg)=0.549×t~(0.665)。
室内模拟暴露实验研究发现，表面沉积NaCl、Na_2SO_4和NaNO_3后，AZ31镁合金和纯镁发生明显的局部腐蚀。随着表面盐沉积量的增加，腐蚀速度加快。NaCl、Na_2SO_4和NaNO_3对镁合金侵蚀性强度排序为：NaCl＞Na_2SO_4＞NaNO_3。薄层电解液中含有NaCl、Na_2SO_4和NaNO_3时的电化学测试表明，随着试样表面液层厚度的减薄，腐蚀产物的沉积速度加快导致腐蚀产物膜变得粗糙、疏松；液膜越薄，局部腐蚀越易发生。液膜较薄时，三种电解液中R_f和R_(ct)大小顺序为NaNO_3＞Na_2SO_4＞NaCl，表明其侵蚀性强度顺序为NaCl＞Na_2SO_4＞NaNO_3，验证了室内模拟暴露实验检测结果。此外，NaNO_3的液膜下，液膜厚度变化对镁合金极化行为的影响较NaCl和Na_2SO_4液膜下显著，这是由于阴极过程除了生成氢气外，还产生NO_3~-的去极化反应所致。
开发了一种KMnO_4-REMS化学氧化工艺，AZ91、AM60、AZ31镁合金以及纯镁经该工艺氧化处理后，获得的氧化膜质量优于磷酸盐处理等典型的无铬镁合金化学氧化处理工艺，与传统铬酸盐处理工艺相当。经KMnO_4-REMS工艺氧化后，镁合金表面氧化膜层呈网状微裂纹结构，氧化膜厚度约为10μm，膜层的主要成分为CeO_2、MnO和MnO_2，还有少量MgO、Mg(OH)_2以及铝的化合物。镁合金表面的KMnO_4-REMS氧化膜具有三层结构，最内层是镁和铝的氧化物和氢氧化物，中间层则主要由锰的氧化物组成，表层沉积了铈的氧化物。氧化膜表面的网状微裂纹结构在氧化过程中形成，由镁合金结构和化学氧化处理后干燥过程中氢氧化物脱水所造成。
为了解决氧化液存在的环境污染问题，本文对环保无毒的植酸氧化液在镁合金表面化学氧化工艺中的应用进行研究。发现植酸氧化液的最佳pH值范围为9～10，在AZ91、AM60、AZ31镁合金以及纯镁表面形成的氧化膜透明、光亮，膜层致密、均匀。经植酸处理后，在0.05mol·L~(-1)的NaCl溶液中耐蚀性能测试结果表明，镁及镁合金腐蚀电位升高，极化电流密度减小，电化学性能得到改善；化学浸泡8h未见腐蚀，耐蚀性能得到提高。植酸处理液在镁合金表面形成的氧化膜含有Mg、Al、Zn、O、P和C元素，膜的组成为植酸的镁盐和铝盐，以及镁和铝的氧化物和氢氧化物。植酸在镁合金表面发生化学吸附，形成一层致密的有机保护膜，膜层有效地阻滞活性离子向基体表面扩散，隔离基体与腐蚀介质，从而抑制镁合金腐蚀。
Magnesium alloys are of great importance at present and future fields of engineering for their attractive combination of low density and high strength/weight ratio. However, since magnesium is intrinsically active in the environment, the corrosion resistance of magnesium alloys is generally inadequate, which limits their application. In order to improve the corrosion resistance of magnesium alloys, surface treatment technologies, like chemical conversion, are commonly applied. Nowadays, the methods applied introduce chromate ions in the solutions, which is progressively restricted due to its high toxicity to the environment. The trend in the field is oriented to investigate the corrosion mechanism of magnesium alloy and develop environmental friendly chemical treatment technologies.
In this paper, the atmospheric corrosion behavior of extruded AZ31 magnesium alloy and pure magnesium samples is studied by weight loss test, electrochemical measurements and physical detection technologies, such as SEM, EDX, EPMA and XPS. After 400d atmospheric exposure station in Dalian city, the samples are covered with a plumbeous corrosion production film. Compared with pure magnesium sample, the film on AZ31 magnesium alloy is more compact. Moreover, after the corrosion production is wiped off, some insulated "island", which formed on the corrosion slightly area, are observed on the surface of the samples. The proportions of the corrosion region to the general area are 65.0% and 42.3% on AZ31 and pure magnesium, respectively. The compositiones of corrosion production on the two samples are almost similar. They are MgO, Mg(OH)_2, Al(OH)_3, Al_2O_3 and carbonate, sulfate and chloride of Mg and Al. The corrosion kinetics calculated by image methods accord with exponential equation and the dynamics equations for AZ31 and pure magnesium are H_(AZ31)=0.403×t~(0.653) and H_(PMg)=0.549×t~(0.665), respectively.
The effect of NaCl, Na_2SO_4 and NaNO_3 on the atmospheric corrosion of AZ31 magnesium alloy and pure magnesium samples was studied by the indoor simulated exposure experiment and electrochemical test under thin electrolyte layers. After 40d indoor simulated exposure station with the addition of NaCl, Na_2SO_4 and NaNO_3 on the surface of AZ31 and pure magnesium, the samples occur local corrosion. The corrosion rate of the samples increases with the salt concentratiom increasing. The aggressiveness of the salt is NaCl > Na_2SO_4> NaNO_3 Electrochemical tests under thin electrolyte layers show that decreasing the thickness of electrolyte layers results in accelerating corrosion rate. The thinner the layer is, the easier the occurrence of local corrosion on the samples is. The difference of the corrosion behaviors between in solution and under thin layer is mainly due to the dissolve of O_2 and CO_2 in the electrolyte. In addition, the NO_3~- is more sensitive to the thickness of the layer than Cl~- and SO_4~-, which is caused by the participation of NO_3~- in the cathodic depolarization.
In order to avoid high toxicity like Cr treatment to the environment and improve the corrosion resistance of magnesium alloys, KMnO_4-REMS chemical conversion treatment technique is developed in this paper. The conversion coatings obtained with this method show better corrosion resistance than previously used phosphate-based conversion treatment for AZ91, AM60, AZ31 and pure magnesium samples, and reach the levels of chrome-based treatment. Furthermore, the electrochemical polarization tests show that compared with the samples treated by chrome-based method, the anodic current density of the alloy coated in permanganate-REMS bath, at the same potential, decreases evidently in 0.05mol·L~(-1)NaCl solution. Simultaneously, the open-circuit potential of magnesium alloy increases 0.06V compared with blank samples. The thickness of the coating formed by the permanganate-REMS bath on AZ91 magnesium alloy is about 10μm and net-like cracks exists on the coatings. The conversion coating mainly composes of CeO_2, MnO, MnO_2, and some oxides of Mg and Al.
Phytic acid, as an environmental- friendly agent, has been growing applied in the application of metal surface treatments. In this paper, the corrosion protects afforded by phytic acid conversion coatings on magnesium and magnesium alloy has been developed. The results show that optimal pH range for the treatment is 9-10. In 0.05mol L~(-1)NaCl solutions, Magnesium alloy coated by phytic acid solution don't corrode until 8 hours. Simultaneously, compared with blank samples, the open-circuit potential of magnesium alloy treated by phytic acid solutin is increased and the anodic current density is decreased at the same potential. A compact film is found on the surface of magnesium alloy with the combination of phytic acids and the metal. The film is mainly composed of phytate and some oxides of Mg and Al. This film may insulate the metal from the deleterious anion, thus protect the magnesium alloy against corrosion. Moreover, by reacting to the paint, the phytic acid coating can improve the resin binding power.
引文
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