Mg-9Gd-4Y-1Nd-0.6Zr合金的耐蚀性及铈转化膜研究
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摘要
Mg-9Gd-4Y-1Nd-0.6Zr合金具有轻质、高强、耐热和深冲性能好等优异性能,这是在具有减重需求的航空航天、武器装备和交通运输等领域的应用前提。但该合金较差的耐蚀性,将影响其使用寿命和应用成本。只有提高Mg-9Gd-4Y-1Nd-0.6Zr合金的耐腐蚀性能,才能使该合金得以快速发展。针对这一主要问题,本文采用光学显微镜、带能谱分析的扫描电镜、透射电镜、X射线衍射仪、红外光谱仪、电化学工作站等分析手段,系统研究了Mg-9Gd-4Y-1Nd-0.6Zr合金在不同环境中的腐蚀行为,采用时效热处理、合金化及铈转化膜等途径增强该合金耐蚀性等内容,获得了以下结果：
1.采用SEM等手段对Mg-9Gd-4Y-1Nd-0.6Zr合金在NaCl溶液中的点腐蚀行为进行研究,揭示了该合金的点蚀形成规律,建立了点腐蚀动力学模型。Mg-9Gd-4Y-1Nd-0.6Zr合金板点蚀的主要原因是合金中的第二相粒子与a-Mg基体存在电势差,在溶液中很容易产生电偶腐蚀效应,粗大的第二相富稀土粒子是诱发点蚀的根源。通过适当的热处理工艺,或添加合金元素Ce,可以改善合金内第二相粒子的尺寸与分布,提高合金的耐腐蚀性能。
2.探求了时效工艺对Mg-9Gd-4Y-1Nd-0.6Zr合金强度和腐蚀性能的影响规律。过时效合金强度下降很少是由于合金中存在大量β相和β1相。过时效合金耐蚀性显著增强的原因是富稀土粒子在晶界处析出变得细小,分布不连续,有效阻断了腐蚀通道的形成。
3、在Mg-9Gd-4Y-1Nd-0.6Zr合金中加入Ce后,形成了钝化的表面膜,细化了第二相,使第二相呈连续网状分布,提高了合金的腐蚀电位,增大了镁离子生成镁的反应速率常数,减少了镁的阳极溶解速率常数,合金的腐蚀速率明显下降,提高了合金的耐蚀性。Ce加入量为0.5%时,Mg-9Gd-4Y-1Nd-0.6Zr合金获得了较优化的耐蚀性。
4.采用正交实验方法在镁稀土合金表面获得了制备铈转化膜的最佳条件：pH值为10.0,成膜时间为30 min,成膜促进剂的浓度为0.05 M,成膜温度为25℃。具体分析了pH值,成膜时间,成膜促进剂的浓度和温度等因素对铈转化膜耐蚀性的影响。
5.利用LDHs插层组装原理,采用共沉淀法在镁稀土合金表面制备了MgCe-LDHs转化膜,MgCe-LDHs膜层内是共价键结合,不容易被破坏,而层间碳酸根离子经长时间浸泡被氯离子部分置换,膜结构没有改变。因为碳酸根离子一旦嵌入MgCe-LDHs的结构中,其他阴离子很难将其置换,能够增强MgCe-LDHs转化膜在含氯离子溶液中的耐蚀性。
Mg-9Gd-4Y-1Nd-0.6Zr alloy was characterized as light, high strength, heat resistant and good deep drawability etc.It is significant for those fields with a strong demand for weight reduction, such as aerospace components, weapon equipments, and communication and transport tools and so on. But bad corrosion resistance of the Mg alloy made it short life and expensive in its application. Only to improve corrosion resistance of the Mg alloy can the Mg alloy industry develop fast. According to this problem, corrosion resistance of Mg-9Gd-4Y-1Nd-0.6Zr alloy in different environments was investigated. To improve the corrosion resistance of Mg-9Gd-4Y-1Nd-0.6Zr alloy, ageing treatment, alloying Ce and cerium conversion film were studied. All were studied systematically by experimental methods such as optical microscopy (OM), scanning electron microscopy (SEM) with energy dispersive X-ray (EDAX), X-ray diffractometer (XRD), Fourier Transform Infrared Spectrometer (FTIR), electrochemical workstation etc. Draw a conclusion as following:
(1) To explore the pitting mechanism, the pitting corrosion behavior of Mg-9Gd-4Y-1Nd-0.6Zr alloy was investigated by SEM. The pitting kinetic mode of the Mg alloy was established.The pitting of Mg-9Gd-4Y-1Nd-Zr alloy plate was caused by potential between second phase particles and a-magnesium. The galvanic corrosion occurred in aqueous environment around the coarse second phase particles which riched rare earth in the Mg alloy. The Mg alloy corrosion resistance can be improved by proper heat-treatment or alloying Ce.
(2) The effect of ageing treatment on the strength and corrosion resistance of Mg-9Gd-4Y-1Nd-0.6Zr alloy was revealed. The high strength over-aged Mg alloy was related to theβ'andβ1 phase. The over-aged sample at the grain boundaries were decorated with small and discontinuously distributed particles. The corrosion channels were blocked by small particles which distributed discontinuously at grain boundaries.
(3) It is found that by adding Ce into Mg-9Gd-4Y-1Nd-0.6Zr alloy, the Mg alloy corrosion rate decreased by the passivation film. It makes not only second phase particles distribute continuously as net which can restrain corrosion, but also refines the Mg alloy grain with addition of Ce. By adding Ce to Mg-9Gd-4Y-1Nd-0.6Zr alloy, corrosion potential moved positive and the passivation current decreased, which indicate that the corrosion resistance of the Mg alloy has been improved. The positive corrosion potential makes oxidation rate constant decrease and dioxidation rate constant increase. With the addition of 0.5% Ce into Mg-9Gd-4Y-1Nd-0.6Zr alloy, the Mg alloy got the optimum corrosion resistance.
(4) The optimization of deposition parameters of cerium conversion film was pH 10.0, time 30 min,0.05 M accelerating agent and T 25℃by orthogonal table L (9,34). The effects of corrosion resistance influenced in sequence pH> electrochemical deposition time> concentration of accelerating agent> temperature.
(5)Mg-Ce hydrotalcite film on Mg-9Gd-4Y-1Nd-0.6Zr magnesium alloy surface provides better corrosion protection than Ce conversion film. The better corrosion resistance can be attributed to the Mg-Ce hydrotalcite exhibiting Cl" and CO32- anion exchangeability without changing its structure in chloride media. The carbonate anion has been proved to be the preferred anion for intercalation, and once intercalated, it was very hard to exchange with other anions。
1.采用SEM等手段对Mg-9Gd-4Y-1Nd-0.6Zr合金在NaCl溶液中的点腐蚀行为进行研究,揭示了该合金的点蚀形成规律,建立了点腐蚀动力学模型。Mg-9Gd-4Y-1Nd-0.6Zr合金板点蚀的主要原因是合金中的第二相粒子与a-Mg基体存在电势差,在溶液中很容易产生电偶腐蚀效应,粗大的第二相富稀土粒子是诱发点蚀的根源。通过适当的热处理工艺,或添加合金元素Ce,可以改善合金内第二相粒子的尺寸与分布,提高合金的耐腐蚀性能。
2.探求了时效工艺对Mg-9Gd-4Y-1Nd-0.6Zr合金强度和腐蚀性能的影响规律。过时效合金强度下降很少是由于合金中存在大量β相和β1相。过时效合金耐蚀性显著增强的原因是富稀土粒子在晶界处析出变得细小,分布不连续,有效阻断了腐蚀通道的形成。
3、在Mg-9Gd-4Y-1Nd-0.6Zr合金中加入Ce后,形成了钝化的表面膜,细化了第二相,使第二相呈连续网状分布,提高了合金的腐蚀电位,增大了镁离子生成镁的反应速率常数,减少了镁的阳极溶解速率常数,合金的腐蚀速率明显下降,提高了合金的耐蚀性。Ce加入量为0.5%时,Mg-9Gd-4Y-1Nd-0.6Zr合金获得了较优化的耐蚀性。
4.采用正交实验方法在镁稀土合金表面获得了制备铈转化膜的最佳条件：pH值为10.0,成膜时间为30 min,成膜促进剂的浓度为0.05 M,成膜温度为25℃。具体分析了pH值,成膜时间,成膜促进剂的浓度和温度等因素对铈转化膜耐蚀性的影响。
5.利用LDHs插层组装原理,采用共沉淀法在镁稀土合金表面制备了MgCe-LDHs转化膜,MgCe-LDHs膜层内是共价键结合,不容易被破坏,而层间碳酸根离子经长时间浸泡被氯离子部分置换,膜结构没有改变。因为碳酸根离子一旦嵌入MgCe-LDHs的结构中,其他阴离子很难将其置换,能够增强MgCe-LDHs转化膜在含氯离子溶液中的耐蚀性。
Mg-9Gd-4Y-1Nd-0.6Zr alloy was characterized as light, high strength, heat resistant and good deep drawability etc.It is significant for those fields with a strong demand for weight reduction, such as aerospace components, weapon equipments, and communication and transport tools and so on. But bad corrosion resistance of the Mg alloy made it short life and expensive in its application. Only to improve corrosion resistance of the Mg alloy can the Mg alloy industry develop fast. According to this problem, corrosion resistance of Mg-9Gd-4Y-1Nd-0.6Zr alloy in different environments was investigated. To improve the corrosion resistance of Mg-9Gd-4Y-1Nd-0.6Zr alloy, ageing treatment, alloying Ce and cerium conversion film were studied. All were studied systematically by experimental methods such as optical microscopy (OM), scanning electron microscopy (SEM) with energy dispersive X-ray (EDAX), X-ray diffractometer (XRD), Fourier Transform Infrared Spectrometer (FTIR), electrochemical workstation etc. Draw a conclusion as following:
(1) To explore the pitting mechanism, the pitting corrosion behavior of Mg-9Gd-4Y-1Nd-0.6Zr alloy was investigated by SEM. The pitting kinetic mode of the Mg alloy was established.The pitting of Mg-9Gd-4Y-1Nd-Zr alloy plate was caused by potential between second phase particles and a-magnesium. The galvanic corrosion occurred in aqueous environment around the coarse second phase particles which riched rare earth in the Mg alloy. The Mg alloy corrosion resistance can be improved by proper heat-treatment or alloying Ce.
(2) The effect of ageing treatment on the strength and corrosion resistance of Mg-9Gd-4Y-1Nd-0.6Zr alloy was revealed. The high strength over-aged Mg alloy was related to theβ'andβ1 phase. The over-aged sample at the grain boundaries were decorated with small and discontinuously distributed particles. The corrosion channels were blocked by small particles which distributed discontinuously at grain boundaries.
(3) It is found that by adding Ce into Mg-9Gd-4Y-1Nd-0.6Zr alloy, the Mg alloy corrosion rate decreased by the passivation film. It makes not only second phase particles distribute continuously as net which can restrain corrosion, but also refines the Mg alloy grain with addition of Ce. By adding Ce to Mg-9Gd-4Y-1Nd-0.6Zr alloy, corrosion potential moved positive and the passivation current decreased, which indicate that the corrosion resistance of the Mg alloy has been improved. The positive corrosion potential makes oxidation rate constant decrease and dioxidation rate constant increase. With the addition of 0.5% Ce into Mg-9Gd-4Y-1Nd-0.6Zr alloy, the Mg alloy got the optimum corrosion resistance.
(4) The optimization of deposition parameters of cerium conversion film was pH 10.0, time 30 min,0.05 M accelerating agent and T 25℃by orthogonal table L (9,34). The effects of corrosion resistance influenced in sequence pH> electrochemical deposition time> concentration of accelerating agent> temperature.
(5)Mg-Ce hydrotalcite film on Mg-9Gd-4Y-1Nd-0.6Zr magnesium alloy surface provides better corrosion protection than Ce conversion film. The better corrosion resistance can be attributed to the Mg-Ce hydrotalcite exhibiting Cl" and CO32- anion exchangeability without changing its structure in chloride media. The carbonate anion has been proved to be the preferred anion for intercalation, and once intercalated, it was very hard to exchange with other anions。
引文
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