稀土对低碳结构钢耐工业及海洋大气腐蚀性能的影响研究
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摘要
随着对钢材服役寿命要求的提高,在大气中使用的低碳结构钢(碳钢)除了需要更好的强韧性匹配外,同时还应具有较为良好的耐大气腐蚀性能。但Ni、Cu、Cr等合金元素的高成本使常规耐候钢的使用受到很大限制。因此,采用添加低成本元素进而研发经济型耐候钢逐渐成为国内外钢铁研究的新热点。而通过添加少量稀土元素,开发出具有较好耐大气腐蚀性的高效低碳结构钢符合我国国情,并对节约资源及钢铁材料的可持续发展有着重要的实际意义。
早期文献表明,除稀土总量外,RE/S是稀土在钢中作用的重要参数,其数值直接影响了稀土在钢中的存在状态以及对钢铁材料力学性能的改善效果。然而,RE/S值与碳钢耐大气腐蚀性关系的研究缺乏报道。同时,随着钢铁冶金水平的提高,普通低碳结构钢的洁净度也有了显著的改善,这使稀土在钢中的存在形式有所改变。因此研究RE/S值及稀土的不同存在形式对碳钢耐大气腐蚀性的影响具有重要的现实意义。此外,早期文献中稀土对碳钢锈层保护性的影响缺乏论述,因而开展稀土对碳钢锈层作用的系统研究同样具有一定的理论价值。
本文通过实验室周期浸润加速腐蚀试验和实地大气暴晒试验考察了在工业及海洋大气环境中稀土对低碳结构钢耐腐蚀性能的改善效果。借助物理化学相分析、夹杂物研究、微区pH值原位观察以及电化学等手段系统探讨了钢中稀土的不同存在形式对钢基体及锈层耐蚀性能改善作用的影响规律及机理。
试验钢夹杂物的扫描电镜观察及热力学计算的研究结果表明,稀土在碳钢中能以多种形式存在,主要包括稀土硫化物、稀土氧化物、稀土氧硫化物、RE-Fe金属间化合物以及固溶稀土。除稀土总量以外,RE/S对钢中稀土的夹杂物性质及合金化量具有显著影响。对本文中研究的试验钢(RE～0.030wt%,O～0.0030wt%)而言,控制RE/S值在2.35-4.62之间时,钢中夹杂物球化完全,且数量最少；而当RE/S≥8.57时,钢中稀土的合金化量将占稀土总量的50%左右。此外,试验钢珠光体片间距随RE/S的升高而减小；且在较高RE/S试验钢中,珠光体的片层形貌有退化趋势。
试验钢的周浸加速腐蚀试验和实地大气暴晒试验结果均显示,碳钢中添加适量稀土能够有效改善基体的耐工业及海洋大气腐蚀性能。在模拟大气环境中,随RE/S数值增大,试验钢的耐蚀效果逐渐提高。
微区pH的原位分析结果显示,碳钢夹杂物引起的严重局部腐蚀能使其表面薄液膜的pH明显降低；与此相比,钢中的稀土硫化物和合金化稀土有利于抑制材料表面薄液膜的酸化。由腐蚀动力学方程可知,随碳钢表面薄液膜的pH的升高,基体的腐蚀电流将呈降低趋势。稀土硫化物和合金化稀土对薄液膜酸化效应的抑制作用,不仅使稀土钢在工业大气环境中的阳极溶解速率较低,还有利于其锈层中保护性腐蚀产物α-FeOOH的形成,并能减少稀土钢锈层中的缺陷数量。
裸钢在0.2%NaCl溶液中的极化曲线结果表明,随着RE/S值的提高,试验钢的自腐蚀电位及腐蚀电流均呈降低趋势,阴极极化特征逐渐明显；此外,RE/S较高的试验钢极化曲线阳极区出现较为明显的钝化平台。点蚀源的微观观察发现,在含有氯离子的腐蚀溶液中,钢中的不同类型的夹杂物在腐蚀初期的点蚀行为有所不同。随着稀土的加入及RE/S的升高,试验钢的点蚀形貌发生变化。与碳钢夹杂物相比,稀土夹杂物的影响范围较大,由稀土夹杂物离解产生的Ce3+可以作为试验钢在Cl-溶液中的阴极沉淀型缓蚀剂,使钢基体体现出对Cl-腐蚀更强的抵御作用。同时,结合试验钢点蚀的微观形貌及电化学特征,本工作分别建立并比较了钢中四类不同夹杂物在海洋大气环境中的诱发点蚀模型。
实地大气暴晒试验表明,在真实的工业大气环境中,试验钢暴晒两年的腐蚀产物均由α-FeOOH,γ-FeOOH,δ-FeOOH、Fe3O4以及非晶态锈组成。碳钢锈层疏松,与基体的结合力不强,且其中存在较多的裂纹和孔洞,且锈层中活性组元比例较大；而稀土可以促进锈层中保护性腐蚀产物的生成,并降低锈层中导电相Fe3O4的比例,从而可以有效保护基体,降低钢的腐蚀速率。在海洋大气环境下,稀土在锈层中不均匀分布,并能与Cl-和SO42-结合,进而有效阻止环境中的腐蚀性阴离子向基体的迁移,削弱了锈层阴离子选择性的倾向。同时,稀土能能细化锈颗粒,提高铁锈中非晶相比例和致密性,增强试验钢锈层的物理及化学保护性。
大气暴晒试验带锈试样的电化学研究结果表明,稀土可以减缓钢基体的电化学腐蚀。在热力学方面,稀土钢自腐蚀电位高于对比碳钢,降低了基体离子化的倾向；在动力学方面,稀土钢的腐蚀电流密度较小,且随着暴晒时间延长,其锈层趋于钝化。结合锈层EIS谱的演化结果可知,经过两年的大气暴晒,稀土钢锈层电阻和电荷传输电阻均远大于碳钢,腐蚀产物对钢基体耐电化学腐蚀能力显著增强。
In order to extend the service life of the steel material, the excellent corrosion resistance apart from outstanding strength-toughness matching is required of the low carbon-structural steel (carbon steel) used in atmospheric environment. However, the usage of weathering steel is restricted by the increasing cost of alloying elements. Therefore, the research on economical weathering steel has gradually become a new focus of advanced steel. In general, most of the research was carried out by adding the low-cost alloying elements. It is conformed to the conditions of our country to develop high performance RE-bearing low carbon steel with better weatherability, which also possesses important significance in saving resource and for sustainable development of steel material.
The early literatures showed that RE/S was an important parameters which could characterize the function of RE in steel, besides total RE contant. And the RE/S value could influence directly the existing form of RE and improvement effect on mechanical properties of RE-bearing steel. However, research reports on the relationships between the RE/S value and anti-atmospheric corrosion properties of carbon steel were few. Meanwhile, with the development of the metallurgical technology, the purity of the steel has been raised. The existing form and corrosion resistance mechanism of RE in the new carbon steel will certainly be corresponding changed. Therefore, it is practical significance to carry out the further study of the effect of the RE/S value and RE in different forms on carbon steel and the underlying mechanisms. In addition, since the influence of RE on the protection of rust layer of the carbon steel is not yet well understood, it is beneficial to engaged in systematically study in the contribution of RE to the rust layer of the carbon steel.
The influence of RE on the industry and marine environmental corrosion resistance of low carbon-structural steel was studied by means of cycle immersion corrosion tests and atmospheric exposure tests. Meanwhile, considering the characteristics of the corrosive medium in different atmospheric environment, the rules and mechanisms of the different RE phase in improving atmospheric corrosion resistance of the steel substrate and the rust layer had been investigated by physical chemistry phase analysis, investigation of inclusions, in-situ observation of micro-area pH value as well as electrochemical methods.
Based on the results of the SEM observation and the thermodynamic calculation, we found that RE could exist in low carbon steel in different forms, mainly including sulfides, oxides, oxysulfide, RE-Fe intermetallic and solid soluble RE. The properties of RE-inclusion and the RE alloying quantity were remarkably related to the RE/S value apart from the total RE. As far as experimental steel(RE-0.030wt%, O～0.0030wt%) was concerned, the amount of the inclusion was elevated and the shape of the inclusion was completely deteriorated, when the RE/S value was controlled in the range of 2.35 to 4.62. And the RE alloying quantity would account for about 50% of the total RE, while the RE/S value was higher than 8.57. Besides, the interval between pearlite slice was decreased with the increase of RE/S value. Moreover, the pearlite slice tended to degenerate in the steel with high RE/S value.
As shown by the cycle immersion corrosion test and atmospheric exposure test, the addition of RE to low carbon-structural steel could effectively improve the industrial and marine atmospheric corrosion resistance. In the simulated atmospheric environment, the corrosion resistant effect of experimental steel was gradually improved with the increasing of the RE/S value.
The in-situ observation result of micro-area pH value showed that a serious localized corrosion caused by the inclusion in the carbon steel could decrease the pH value of the thin liquid film of the carbon steel significantly. By contrast, RE sulfides and RE-Fe intermetallic as well as solid soluble RE were helpful to the inhibition of the acidification of the thin liquid film on RE-bearing steel. According to the corrosion kinetics, the corrosion current of the substrate was decreased with the increasing of the pH value of the thin liquid film of the steel. The inhibition of the acidizing caused by RE sulfides, RE-Fe intermetallic and solid soluble RE were not only able to decrease the anodic dissolution rate of RE-bearing steel in the industrial atmospheric environment, but also able to promote the formation ofα-FeOOH which was a steady protective corrosion product and make the rust layer more compact.
Polarization curves of the bare steel were investigated in 0.2% NaCl solution. Experimental results revealed that both self-corrosion potential and corrosion current of experimental steels decreased with the increasing of the RE/S value, showing the developing trends of the characteristics of the cathodic polarization. Moreover, an obvious passivation phenomenon was found in the anode region of the polarization curves of high RE/S steel. As shown by the microscopic observation of pitting initiation, the initial pitting corrosion behaviors with various types of inclusion were different in chloride solution. The pitting morphologies of the experimental steel would be changed by adding RE and increasingthe RE/S value. Compared with the carbon steel, the corrosion influence scope of inclusion in RE-bearing steel had a much wider range. The dissociated Ce3+ form inclusion could be used as cathodal depositing inhibitor in NaCl solution with neutral pH value, and thus leaded to a much stronger corrosion resistance of the RE-bearing steel to Cl-Furthermore, based on the pitting micro-morphologies and electrochemical characteristics of experimental steel, the marine atmospheric pitting initiation models of four types inclusions were also established, respectively.
The result of the industrial atmospheric exposure test showed that the rust phase of the experimental steels were quite similar, which were composed ofα-FeOOH,γ-FeOOH,δ-FeOOH, Fe3O4 and amorphous rust. Binding weakly with the steel matrix, the rust layer of the carbon steel was loose and porous, which contained a large percentage of active components. Whereas, RE could promote the formation of the steady protective corrosion products, decrease the ratio of conductive phase Fe3O4, which could inhibit the corrosion effectively. On the other hand, the result of the marine atmospheric exposure test showed that RE distributed unevenly in the rust layer and could be combined with Cl- and SO42-. Thus, in the presence of RE, the electromigration of corrosive anion in the corrosion product would be prevented effectively and the anion-selective tendency of rust layer was weakened. Meanwhile, RE had the capability to refine the rust particles and raise the ratio of amorphous in the rust.
The measurement results of electrochemical studies showed that RE could inhibit the electrochemical reaction of corrosion of the carbon steel exposed in Jiangjin area. Based on the thermodynamics analysis, the introduction of RE in the carbon steel could cause the free corrosion potential shift positively, and reduce the ionization tendency of the steel matrix. On the other hand, kinetics analysis indicated that RE in the steel could reduce corrosion current, and make the rust layer tend to be passivated with the extending of the exposure time. The equivalent circuit of the electrochemical reaction was obtained by analyzing EIS of the experimental steel. The parameters of Rr and Rct could characterize the anti-corrosion of the rust layer. After 2 years exposure test, both Rr and Rct of RE-bearing steel were much bigger than those of carbon steel. The test indicated that the rust layer on the surface of RE-bearing steel had strong ability to lower the corrosion rate.
早期文献表明,除稀土总量外,RE/S是稀土在钢中作用的重要参数,其数值直接影响了稀土在钢中的存在状态以及对钢铁材料力学性能的改善效果。然而,RE/S值与碳钢耐大气腐蚀性关系的研究缺乏报道。同时,随着钢铁冶金水平的提高,普通低碳结构钢的洁净度也有了显著的改善,这使稀土在钢中的存在形式有所改变。因此研究RE/S值及稀土的不同存在形式对碳钢耐大气腐蚀性的影响具有重要的现实意义。此外,早期文献中稀土对碳钢锈层保护性的影响缺乏论述,因而开展稀土对碳钢锈层作用的系统研究同样具有一定的理论价值。
本文通过实验室周期浸润加速腐蚀试验和实地大气暴晒试验考察了在工业及海洋大气环境中稀土对低碳结构钢耐腐蚀性能的改善效果。借助物理化学相分析、夹杂物研究、微区pH值原位观察以及电化学等手段系统探讨了钢中稀土的不同存在形式对钢基体及锈层耐蚀性能改善作用的影响规律及机理。
试验钢夹杂物的扫描电镜观察及热力学计算的研究结果表明,稀土在碳钢中能以多种形式存在,主要包括稀土硫化物、稀土氧化物、稀土氧硫化物、RE-Fe金属间化合物以及固溶稀土。除稀土总量以外,RE/S对钢中稀土的夹杂物性质及合金化量具有显著影响。对本文中研究的试验钢(RE～0.030wt%,O～0.0030wt%)而言,控制RE/S值在2.35-4.62之间时,钢中夹杂物球化完全,且数量最少；而当RE/S≥8.57时,钢中稀土的合金化量将占稀土总量的50%左右。此外,试验钢珠光体片间距随RE/S的升高而减小；且在较高RE/S试验钢中,珠光体的片层形貌有退化趋势。
试验钢的周浸加速腐蚀试验和实地大气暴晒试验结果均显示,碳钢中添加适量稀土能够有效改善基体的耐工业及海洋大气腐蚀性能。在模拟大气环境中,随RE/S数值增大,试验钢的耐蚀效果逐渐提高。
微区pH的原位分析结果显示,碳钢夹杂物引起的严重局部腐蚀能使其表面薄液膜的pH明显降低；与此相比,钢中的稀土硫化物和合金化稀土有利于抑制材料表面薄液膜的酸化。由腐蚀动力学方程可知,随碳钢表面薄液膜的pH的升高,基体的腐蚀电流将呈降低趋势。稀土硫化物和合金化稀土对薄液膜酸化效应的抑制作用,不仅使稀土钢在工业大气环境中的阳极溶解速率较低,还有利于其锈层中保护性腐蚀产物α-FeOOH的形成,并能减少稀土钢锈层中的缺陷数量。
裸钢在0.2%NaCl溶液中的极化曲线结果表明,随着RE/S值的提高,试验钢的自腐蚀电位及腐蚀电流均呈降低趋势,阴极极化特征逐渐明显；此外,RE/S较高的试验钢极化曲线阳极区出现较为明显的钝化平台。点蚀源的微观观察发现,在含有氯离子的腐蚀溶液中,钢中的不同类型的夹杂物在腐蚀初期的点蚀行为有所不同。随着稀土的加入及RE/S的升高,试验钢的点蚀形貌发生变化。与碳钢夹杂物相比,稀土夹杂物的影响范围较大,由稀土夹杂物离解产生的Ce3+可以作为试验钢在Cl-溶液中的阴极沉淀型缓蚀剂,使钢基体体现出对Cl-腐蚀更强的抵御作用。同时,结合试验钢点蚀的微观形貌及电化学特征,本工作分别建立并比较了钢中四类不同夹杂物在海洋大气环境中的诱发点蚀模型。
实地大气暴晒试验表明,在真实的工业大气环境中,试验钢暴晒两年的腐蚀产物均由α-FeOOH,γ-FeOOH,δ-FeOOH、Fe3O4以及非晶态锈组成。碳钢锈层疏松,与基体的结合力不强,且其中存在较多的裂纹和孔洞,且锈层中活性组元比例较大；而稀土可以促进锈层中保护性腐蚀产物的生成,并降低锈层中导电相Fe3O4的比例,从而可以有效保护基体,降低钢的腐蚀速率。在海洋大气环境下,稀土在锈层中不均匀分布,并能与Cl-和SO42-结合,进而有效阻止环境中的腐蚀性阴离子向基体的迁移,削弱了锈层阴离子选择性的倾向。同时,稀土能能细化锈颗粒,提高铁锈中非晶相比例和致密性,增强试验钢锈层的物理及化学保护性。
大气暴晒试验带锈试样的电化学研究结果表明,稀土可以减缓钢基体的电化学腐蚀。在热力学方面,稀土钢自腐蚀电位高于对比碳钢,降低了基体离子化的倾向；在动力学方面,稀土钢的腐蚀电流密度较小,且随着暴晒时间延长,其锈层趋于钝化。结合锈层EIS谱的演化结果可知,经过两年的大气暴晒,稀土钢锈层电阻和电荷传输电阻均远大于碳钢,腐蚀产物对钢基体耐电化学腐蚀能力显著增强。
In order to extend the service life of the steel material, the excellent corrosion resistance apart from outstanding strength-toughness matching is required of the low carbon-structural steel (carbon steel) used in atmospheric environment. However, the usage of weathering steel is restricted by the increasing cost of alloying elements. Therefore, the research on economical weathering steel has gradually become a new focus of advanced steel. In general, most of the research was carried out by adding the low-cost alloying elements. It is conformed to the conditions of our country to develop high performance RE-bearing low carbon steel with better weatherability, which also possesses important significance in saving resource and for sustainable development of steel material.
The early literatures showed that RE/S was an important parameters which could characterize the function of RE in steel, besides total RE contant. And the RE/S value could influence directly the existing form of RE and improvement effect on mechanical properties of RE-bearing steel. However, research reports on the relationships between the RE/S value and anti-atmospheric corrosion properties of carbon steel were few. Meanwhile, with the development of the metallurgical technology, the purity of the steel has been raised. The existing form and corrosion resistance mechanism of RE in the new carbon steel will certainly be corresponding changed. Therefore, it is practical significance to carry out the further study of the effect of the RE/S value and RE in different forms on carbon steel and the underlying mechanisms. In addition, since the influence of RE on the protection of rust layer of the carbon steel is not yet well understood, it is beneficial to engaged in systematically study in the contribution of RE to the rust layer of the carbon steel.
The influence of RE on the industry and marine environmental corrosion resistance of low carbon-structural steel was studied by means of cycle immersion corrosion tests and atmospheric exposure tests. Meanwhile, considering the characteristics of the corrosive medium in different atmospheric environment, the rules and mechanisms of the different RE phase in improving atmospheric corrosion resistance of the steel substrate and the rust layer had been investigated by physical chemistry phase analysis, investigation of inclusions, in-situ observation of micro-area pH value as well as electrochemical methods.
Based on the results of the SEM observation and the thermodynamic calculation, we found that RE could exist in low carbon steel in different forms, mainly including sulfides, oxides, oxysulfide, RE-Fe intermetallic and solid soluble RE. The properties of RE-inclusion and the RE alloying quantity were remarkably related to the RE/S value apart from the total RE. As far as experimental steel(RE-0.030wt%, O～0.0030wt%) was concerned, the amount of the inclusion was elevated and the shape of the inclusion was completely deteriorated, when the RE/S value was controlled in the range of 2.35 to 4.62. And the RE alloying quantity would account for about 50% of the total RE, while the RE/S value was higher than 8.57. Besides, the interval between pearlite slice was decreased with the increase of RE/S value. Moreover, the pearlite slice tended to degenerate in the steel with high RE/S value.
As shown by the cycle immersion corrosion test and atmospheric exposure test, the addition of RE to low carbon-structural steel could effectively improve the industrial and marine atmospheric corrosion resistance. In the simulated atmospheric environment, the corrosion resistant effect of experimental steel was gradually improved with the increasing of the RE/S value.
The in-situ observation result of micro-area pH value showed that a serious localized corrosion caused by the inclusion in the carbon steel could decrease the pH value of the thin liquid film of the carbon steel significantly. By contrast, RE sulfides and RE-Fe intermetallic as well as solid soluble RE were helpful to the inhibition of the acidification of the thin liquid film on RE-bearing steel. According to the corrosion kinetics, the corrosion current of the substrate was decreased with the increasing of the pH value of the thin liquid film of the steel. The inhibition of the acidizing caused by RE sulfides, RE-Fe intermetallic and solid soluble RE were not only able to decrease the anodic dissolution rate of RE-bearing steel in the industrial atmospheric environment, but also able to promote the formation ofα-FeOOH which was a steady protective corrosion product and make the rust layer more compact.
Polarization curves of the bare steel were investigated in 0.2% NaCl solution. Experimental results revealed that both self-corrosion potential and corrosion current of experimental steels decreased with the increasing of the RE/S value, showing the developing trends of the characteristics of the cathodic polarization. Moreover, an obvious passivation phenomenon was found in the anode region of the polarization curves of high RE/S steel. As shown by the microscopic observation of pitting initiation, the initial pitting corrosion behaviors with various types of inclusion were different in chloride solution. The pitting morphologies of the experimental steel would be changed by adding RE and increasingthe RE/S value. Compared with the carbon steel, the corrosion influence scope of inclusion in RE-bearing steel had a much wider range. The dissociated Ce3+ form inclusion could be used as cathodal depositing inhibitor in NaCl solution with neutral pH value, and thus leaded to a much stronger corrosion resistance of the RE-bearing steel to Cl-Furthermore, based on the pitting micro-morphologies and electrochemical characteristics of experimental steel, the marine atmospheric pitting initiation models of four types inclusions were also established, respectively.
The result of the industrial atmospheric exposure test showed that the rust phase of the experimental steels were quite similar, which were composed ofα-FeOOH,γ-FeOOH,δ-FeOOH, Fe3O4 and amorphous rust. Binding weakly with the steel matrix, the rust layer of the carbon steel was loose and porous, which contained a large percentage of active components. Whereas, RE could promote the formation of the steady protective corrosion products, decrease the ratio of conductive phase Fe3O4, which could inhibit the corrosion effectively. On the other hand, the result of the marine atmospheric exposure test showed that RE distributed unevenly in the rust layer and could be combined with Cl- and SO42-. Thus, in the presence of RE, the electromigration of corrosive anion in the corrosion product would be prevented effectively and the anion-selective tendency of rust layer was weakened. Meanwhile, RE had the capability to refine the rust particles and raise the ratio of amorphous in the rust.
The measurement results of electrochemical studies showed that RE could inhibit the electrochemical reaction of corrosion of the carbon steel exposed in Jiangjin area. Based on the thermodynamics analysis, the introduction of RE in the carbon steel could cause the free corrosion potential shift positively, and reduce the ionization tendency of the steel matrix. On the other hand, kinetics analysis indicated that RE in the steel could reduce corrosion current, and make the rust layer tend to be passivated with the extending of the exposure time. The equivalent circuit of the electrochemical reaction was obtained by analyzing EIS of the experimental steel. The parameters of Rr and Rct could characterize the anti-corrosion of the rust layer. After 2 years exposure test, both Rr and Rct of RE-bearing steel were much bigger than those of carbon steel. The test indicated that the rust layer on the surface of RE-bearing steel had strong ability to lower the corrosion rate.
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