NdFeB磁体环境加速腐蚀行为研究
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摘要
NdFeB磁体作为一种重要的金属功能器件被广泛应用于信息电子、能源交通、通讯医疗、国防航空等众多领域,在高科技领域及社会生活中占据越来越重要的地位。由于稀土钕元素的化学活性非常高,易于氧化,所以耐蚀性对于NdFeB磁体的应用非常关键。恒定湿热腐蚀试验、盐雾腐蚀试验和高压加速腐蚀试验通常用于评价稀土永磁材料的耐蚀性,本文针对不同合金成分的NdFeB磁体在这三种加速腐蚀环境中的腐蚀行为及其机理进行研究,讨论合金成分及不同腐蚀试验条件对磁体磁通损失的影响,首次研究了热变形NdFeB磁体耐腐蚀特性。通过电化学腐蚀试验的方法研究了烧结NdFeB磁体的电化学腐蚀行为和机理。这为大幅度提高NdFeB磁体自身的耐腐蚀性能,为进一步揭示NdFeB磁体的腐蚀机制提供可能的理论指导。
通过恒定湿热腐蚀试验、中性盐雾腐蚀试验和高压加速腐蚀试验,系统研究了不同成分的烧结NdFeB磁体在这三种环境下的腐蚀行为和腐蚀动力学。研究发现尽管高压加速腐蚀试验的条件无论是温度、湿度、压力都比恒定湿热腐蚀试验要严苛,但是烧结NdFeB磁体在高压加速腐蚀环境中的腐蚀速率比恒定湿热和中性盐雾腐蚀环境要缓慢得多。认为高压加速腐蚀试验的湿度为100%RH(饱和湿度),试样表面液膜厚度较大,氧的扩散受到限制,加上高压水蒸汽致使供氧不足,导致腐蚀速率放缓。
研究发现NdFeB磁体的盐雾腐蚀进程可分为两个阶段,并给出了盐雾腐蚀反应速率拟合方程。在盐雾腐蚀环境中,样品表面首先形成点蚀。认为由于氯离子极容易吸附和扩散到基体相中,在氯离子的协同作用下腐蚀面不断扩大。在腐蚀初期由于腐蚀产物的生成速率大于溶解速率,表现为“腐蚀增重期”；当腐蚀进一步进行时,由于体积膨胀使得样品内部产生应力,导致腐蚀产物脱落溶解,当腐蚀产物的溶解速率远大于生成速率时,表现为“腐蚀失重期”。
通过对比分析烧结NdFeB磁体和热变形NdFeB磁体在中性盐雾腐蚀环境中的耐蚀性,发现热变形磁体在中性盐雾腐蚀环境中展现出了更好的耐蚀性能。认为热变形磁体具有独特的片状纳米晶组织结构,富钕相的晶粒更加细小,分布更加均匀,使得晶间腐蚀发生的通道变窄,从而最大限度的抑制晶间腐蚀的速率,提高磁体的耐蚀性能。
通过电化学腐蚀试验测量了烧结NdFeB磁体在3.0%NaOH溶液,自来水,3.5%NaCl溶液以及0.1mol/LHCl溶液中的极化曲线和交流阻抗谱,研究发现：在NaOH溶液中,烧结NdFeB磁体发生了明显的钝化现象,磁体表面形成了致密的氢氧化物钝化膜,对基体有一定的保护作用；在自来水中,磁体表面生成的腐蚀产物膜对磁体的腐蚀进程具有一定的缓冲作用,但无法阻止腐蚀反应的继续进行；在NaCl溶液中,大量的Cl-离子不仅会破坏腐蚀产物膜在磁体表面的覆盖,还会加速阳极区域的活性溶解；在HCl溶液中,磁体很容易发生活性溶解反应,腐蚀速率明显快于其他溶液。
通过对不同合金成分的烧结NdFeB磁体在不同腐蚀环境和不同性质电化学溶液中的腐蚀行为研究,系统阐明了以重稀土元素Dy部分取代Nd,及微量添加Co等元素,能够明显提高烧结NdFeB磁体在不同环境,不同介质中的耐蚀性。这对钕铁硼生产厂家通过合金成分设计有效提高烧结NdFeB基体的耐蚀性具有重要的指导意义。
NdFeB permanent magnets which serve as important metal functional devices are widely used in various fields, such as electronics, information, communication, energy, transportation, medical apparatus, aviation and so on. They play more and more important roles in our high-tech and daily life. Due to the high chemical activity of Nd and easily oxidized, poor corrosion resistance of NdFeB magnets greatly limit the application. Constant hot-humid(HH), neutral salt spray(NSS) and pressure cooker test(PCT) are usually used to evaluate corrosion resistance of NdFeB magnets. Corrosion behavior and mechanism of different alloy composition of NdFeB magnets in the above corrosive climates were discussed. The effects of alloy composition and different corrosive environments on magnetic flux loss were also discussed. Electrochemical corrosion behavior and mechanism were investigated via dynamic potential polarization curve and electrochemical impedance spectroscopy.
The corrosion velocity rate in PCT climate was much slower than that in NSS and HH climates through the NSS, HH and PCT tests. The thickness of liquid film of magnet surface in PCT climate was much bigger than those in NSS and HH climates because of its saturated humidity(100%RH). It was probably because that high-pressure steam led to an oxygen-deficient supply, and the steam/liquid film on the surface of magnets would hinder the diffusion of oxygen. The atmospheric corrosion happened electrochemical reaction under the thin liquid film. The corrosion velocity rate under full immersion state(PCT) was much slower than those under thin liquid membrane state(NSS and HH).
The corrosion process of NdFeB magnets in NSS climate included two steps, and corrosion reaction dynamic velocity equation was given. In NSS climate, magnet surface formed pitting corrosion at first, and then the corrosion areas expanded increasingly due to the synergy effect of chloride ion which could adsorb and diffuse into the matrix phases. In the beginning, magnet surface formed oxidation film when formation velocity of corrosion products on the magnet surface was faster than dissolution velocity of them, corrosion process displayed weight gain slightly. Then corrosion proceeded further, corrosion products film spalled and dissolved into the solution because of internal stress resulted from volume expansion. When dissolution velocity of corrosion products film was faster than formation velocity, corrosion process displayed weight loss fast.
The corrosion behavior of NdFeB magnets prepared by sintering and hot deforming were compared. Effect of microstructures on corrosion resistance of NdFeB magnets had been discussed. Hot deformed magnets exhibited much better corrosion resistance than sintered ones in the neutral salt spray climate. It was because that hot deformed magnets had platelet-shaped nanograins microstructure, in which grain boundary Nd-rich phases were much fine, uniform and disperse. The different microstructure between sintered and hot deformed magnets caused the different corrosion behavior.
The corrosion behavior and mechanism of sintered NdFeB magnets under different electrochemical conditions were investigated by means of electrochemical technology including polarization curve, electrochemical impedance spectroscopy. The corrosion dynamic models of sintered NdFeB magnets in different solutions were established. In alkaline solution, NdFeB magnets exhibited passive phenomenon evidently. The uniform and compact hydroxide passivation film formed on the magnets surface could protect the matrix of NdFeB magnets away from attack. In piped water, corrosion product film could not prevent corrosion reaction occuring, but could slow corrosion reaction velocity to a certain extent. In NaCl solution, a large member of Cl ions would not only destroy corrosion product film, but also accelerate active dissolution of anode areas. In HCl solution, sintered NdFeB magnets occured activation dissolution easily. Therefore, corrosion rate in acid solution was obviously higher than those in other solutions.
The corrosion behavior and mechanism of different alloy composition of NdFeB magnets in different corrosion climates and electrochemical electrolytes was investigated. It showed that corrosion resistance of NdFeB magnets could be improved obviously by Dy substitution for Nd partially and minor Co addition. It is very significant for NdFeB manufacturers to improve corrosion resistance of magnet substrate through alloy composition design.
通过恒定湿热腐蚀试验、中性盐雾腐蚀试验和高压加速腐蚀试验,系统研究了不同成分的烧结NdFeB磁体在这三种环境下的腐蚀行为和腐蚀动力学。研究发现尽管高压加速腐蚀试验的条件无论是温度、湿度、压力都比恒定湿热腐蚀试验要严苛,但是烧结NdFeB磁体在高压加速腐蚀环境中的腐蚀速率比恒定湿热和中性盐雾腐蚀环境要缓慢得多。认为高压加速腐蚀试验的湿度为100%RH(饱和湿度),试样表面液膜厚度较大,氧的扩散受到限制,加上高压水蒸汽致使供氧不足,导致腐蚀速率放缓。
研究发现NdFeB磁体的盐雾腐蚀进程可分为两个阶段,并给出了盐雾腐蚀反应速率拟合方程。在盐雾腐蚀环境中,样品表面首先形成点蚀。认为由于氯离子极容易吸附和扩散到基体相中,在氯离子的协同作用下腐蚀面不断扩大。在腐蚀初期由于腐蚀产物的生成速率大于溶解速率,表现为“腐蚀增重期”；当腐蚀进一步进行时,由于体积膨胀使得样品内部产生应力,导致腐蚀产物脱落溶解,当腐蚀产物的溶解速率远大于生成速率时,表现为“腐蚀失重期”。
通过对比分析烧结NdFeB磁体和热变形NdFeB磁体在中性盐雾腐蚀环境中的耐蚀性,发现热变形磁体在中性盐雾腐蚀环境中展现出了更好的耐蚀性能。认为热变形磁体具有独特的片状纳米晶组织结构,富钕相的晶粒更加细小,分布更加均匀,使得晶间腐蚀发生的通道变窄,从而最大限度的抑制晶间腐蚀的速率,提高磁体的耐蚀性能。
通过电化学腐蚀试验测量了烧结NdFeB磁体在3.0%NaOH溶液,自来水,3.5%NaCl溶液以及0.1mol/LHCl溶液中的极化曲线和交流阻抗谱,研究发现：在NaOH溶液中,烧结NdFeB磁体发生了明显的钝化现象,磁体表面形成了致密的氢氧化物钝化膜,对基体有一定的保护作用；在自来水中,磁体表面生成的腐蚀产物膜对磁体的腐蚀进程具有一定的缓冲作用,但无法阻止腐蚀反应的继续进行；在NaCl溶液中,大量的Cl-离子不仅会破坏腐蚀产物膜在磁体表面的覆盖,还会加速阳极区域的活性溶解；在HCl溶液中,磁体很容易发生活性溶解反应,腐蚀速率明显快于其他溶液。
通过对不同合金成分的烧结NdFeB磁体在不同腐蚀环境和不同性质电化学溶液中的腐蚀行为研究,系统阐明了以重稀土元素Dy部分取代Nd,及微量添加Co等元素,能够明显提高烧结NdFeB磁体在不同环境,不同介质中的耐蚀性。这对钕铁硼生产厂家通过合金成分设计有效提高烧结NdFeB基体的耐蚀性具有重要的指导意义。
NdFeB permanent magnets which serve as important metal functional devices are widely used in various fields, such as electronics, information, communication, energy, transportation, medical apparatus, aviation and so on. They play more and more important roles in our high-tech and daily life. Due to the high chemical activity of Nd and easily oxidized, poor corrosion resistance of NdFeB magnets greatly limit the application. Constant hot-humid(HH), neutral salt spray(NSS) and pressure cooker test(PCT) are usually used to evaluate corrosion resistance of NdFeB magnets. Corrosion behavior and mechanism of different alloy composition of NdFeB magnets in the above corrosive climates were discussed. The effects of alloy composition and different corrosive environments on magnetic flux loss were also discussed. Electrochemical corrosion behavior and mechanism were investigated via dynamic potential polarization curve and electrochemical impedance spectroscopy.
The corrosion velocity rate in PCT climate was much slower than that in NSS and HH climates through the NSS, HH and PCT tests. The thickness of liquid film of magnet surface in PCT climate was much bigger than those in NSS and HH climates because of its saturated humidity(100%RH). It was probably because that high-pressure steam led to an oxygen-deficient supply, and the steam/liquid film on the surface of magnets would hinder the diffusion of oxygen. The atmospheric corrosion happened electrochemical reaction under the thin liquid film. The corrosion velocity rate under full immersion state(PCT) was much slower than those under thin liquid membrane state(NSS and HH).
The corrosion process of NdFeB magnets in NSS climate included two steps, and corrosion reaction dynamic velocity equation was given. In NSS climate, magnet surface formed pitting corrosion at first, and then the corrosion areas expanded increasingly due to the synergy effect of chloride ion which could adsorb and diffuse into the matrix phases. In the beginning, magnet surface formed oxidation film when formation velocity of corrosion products on the magnet surface was faster than dissolution velocity of them, corrosion process displayed weight gain slightly. Then corrosion proceeded further, corrosion products film spalled and dissolved into the solution because of internal stress resulted from volume expansion. When dissolution velocity of corrosion products film was faster than formation velocity, corrosion process displayed weight loss fast.
The corrosion behavior of NdFeB magnets prepared by sintering and hot deforming were compared. Effect of microstructures on corrosion resistance of NdFeB magnets had been discussed. Hot deformed magnets exhibited much better corrosion resistance than sintered ones in the neutral salt spray climate. It was because that hot deformed magnets had platelet-shaped nanograins microstructure, in which grain boundary Nd-rich phases were much fine, uniform and disperse. The different microstructure between sintered and hot deformed magnets caused the different corrosion behavior.
The corrosion behavior and mechanism of sintered NdFeB magnets under different electrochemical conditions were investigated by means of electrochemical technology including polarization curve, electrochemical impedance spectroscopy. The corrosion dynamic models of sintered NdFeB magnets in different solutions were established. In alkaline solution, NdFeB magnets exhibited passive phenomenon evidently. The uniform and compact hydroxide passivation film formed on the magnets surface could protect the matrix of NdFeB magnets away from attack. In piped water, corrosion product film could not prevent corrosion reaction occuring, but could slow corrosion reaction velocity to a certain extent. In NaCl solution, a large member of Cl ions would not only destroy corrosion product film, but also accelerate active dissolution of anode areas. In HCl solution, sintered NdFeB magnets occured activation dissolution easily. Therefore, corrosion rate in acid solution was obviously higher than those in other solutions.
The corrosion behavior and mechanism of different alloy composition of NdFeB magnets in different corrosion climates and electrochemical electrolytes was investigated. It showed that corrosion resistance of NdFeB magnets could be improved obviously by Dy substitution for Nd partially and minor Co addition. It is very significant for NdFeB manufacturers to improve corrosion resistance of magnet substrate through alloy composition design.
引文
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