摘要
随着人们对海洋资源的深入开发和有效利用,海洋环境中金属结构建筑物的微生物腐蚀(microbiologically influenced corrosion, MIC)已引起了人们的高度重视和广泛研究。在众多的微生物中,硫酸盐还原菌(sulfate-reducing bacteria, SRB)是最主要的腐蚀性细菌之一。
本文从青岛附近海域的海泥中分离纯化得到SRB菌株,采用调整过的Postgate’s C培养基培育细菌并以此作为腐蚀介质。监测了SRB的生长过程对海水介质性质的影响,并重点利用电化学方法(如腐蚀电位Ecorr~t曲线,电化学阻抗谱以及极化曲线)和表面分析手段(如扫描电镜,原子力显微镜以及光电子能谱等)研究了海水介质中SRB对碳素结构钢(Q235)、低镍合金高强度钢(简称“高强钢”)以及18-8不锈钢(18-8SS)腐蚀行为的影响,探讨了SRB介质中铁的阳极活性溶出机制和不锈钢钝化层表面点蚀萌发与生长机制。
研究表明,对于SRB介质中的碳钢,在浸泡初期碳钢表面会生成一层保护性硫化亚铁层(FeS),它使腐蚀速度大大降低;随着浸泡时间的延长,保护性FeS层会出现局部破裂,此后,局部破裂处将以很快的活性溶出速度发生腐蚀。而浸泡在SRB介质中的高强钢,虽然在腐蚀形貌上与碳钢有所差异,但腐蚀电化学特征几乎相同,表明腐蚀机制与碳钢一致。进一步研究表明,SRB的含硫代谢产物是加速碳钢阳极活性溶解的主要因素,据此,本文提出“SRB的含硫代谢产物通过对铁的吸附加速了碳钢/高强钢阳极活性溶解”的腐蚀机制,并在理论上依据吸附态E—pH图判断:在很宽泛的pH值和电位范围内,硫在铁上都能以稳定的吸附态存在。
SRB介质中18-8SS的点蚀过程则异常复杂,很多因素都会影响到点蚀的萌发与生长。18-8SS在SRB介质中很快就会萌发点蚀,由不锈钢表面钝化层在SRB介质中发生硫化转变所形成的局部自由氧是导致钝化层发生破坏而萌发点蚀的主要因素,因为18-8SS在SRB介质中的点蚀电位Epit比SRB介质的氧化-还原电位Eh正;微观腐蚀孔的扩展深度随浸泡时间大致呈线性增加。从腐蚀过程的阴极去极化行为看,很多因素都会影响18-8SS点蚀的生长,然而受18-8SS再钝化行为的影响(18-8SS在SRB介质中的再钝化电位Erep比氢电极的平衡电位正),SRB介质中的单质硫或多态硫的还原是促使点蚀生长的主要因素。此外,由于SRB的代谢活动能明显改变介质的性质,所以它不仅随时会影响18-8SS点蚀的萌发与生长,还会改变处于SRB介质中的18-8SS表面钝化层的结构与性能,进而影响18-8SS的点蚀行为。
本文就SRB介质中钝化层的硫化转变及其对18-8SS点蚀行为的影响进行了详细的研究。研究表明,钝化层的硫化转变降低了18-8SS的钝化性能,而短期硫化对钝化层的危害比长期硫化更大;但是,硫化转变却在一定程度上增大了阴极极化,从而也能阻碍点蚀的生长。18-8SS表面钝化层的性质分析表明,主要是铁的氧化物发生了硫化转变,转变后主要以FeS和FeS_2的形态存在,而元素Cr和Ni则仍然以氧化物/氢氧化物的形态存在,这可以明确地解释为什么短期硫化对钝化层的危害比长期硫化更大,因为,钝化层中铁的氧化物在短时间内发生硫化转变后形成的自由氧在一段时间后可能与其他合金元素重新结合形成不能发生硫化转变的其他金属氧化物/氢氧化物。另一方面,研究中还发现,18-8SS表面在SRB介质中能形成一层具有一定保护性能的生物膜,因此它能在一定程度上阻碍点蚀的萌发和生长。
With increasingly intensive exploitation and effective utilization of marine resources, problems due to microbiologically influenced corrosion (MIC) of metal constructions/components had aroused people’s high concern and extensive study, and among them sulfate-reducing bacteria (SRB) are of the most dangerous culprits.
In this thesis, SRB strain was isolated from seamud in Qingdao nearby, incubated in the modified Postgate's C culture medium which was also prepared for the corrosion medium. Changes of seawater-based medium state due to bacterial activities were detected. As the main objectives, effects of SRB on the corrosion behaviors of carbon steel, low-nickel alloyed high-strength steel and 18-8 stainless steel (18-8SS) in seawater-based media were investigated by electrochemical methods (Ecorr~t curve, electrochemical impedance spectroscopy and polarization curve) and surface analyses techniques (scanning electronic microscopy, atomic force microscopy and X-ray photoelectron spectroscopy). Mechanisms related to both anodic active dissolution of iron and pit-initiation/pit-growth of stainless steel were discussed in detail.
Specifically, when carbon steel is immersed in the cultures of SRB, a protective surface ferrous sulfide (FeS) film would form during the early days of immersion; but some time later the protective FeS film would suffer breakdown locally, and then the localized corrosion rate would be very high in a mode of active dissolution. In the case of high-strength steel immersed in the culture of SRB, the electrochemical nature of corrosion is almost the same as carbon steel although the corrosion morphology is a little different. With further investigation, it was found that sulfur-containing metabolites by SRB are the main factor enhancing the anodic active dissolution of carbon steel. Thus, such a corrosion mechanism was proposed that sulfur-containing bacterial metabolites in the form of adsorbed sulfur on iron enhance anodic active dissolution of carbon steel or high-strength steel. Thereticaly, judged from the E—pH diagrams for adsorbed sulfur on iron, adsorbed sulfur on iron remains very stable in a wide range of pH values as well as potentials values.
As for 18-8SS, pitting corrosion of 18-8SS in the cultures of SRB is very complex process, in which many factors affect pit-initiation/pit-growth. Pit-initiation of 18-8SS can occur in a very short term, and the localized free oxygen resulted from sulfidation of passive film should be the main factor that cause the breakdown of passive film because Epit of 18-8SS in the cultures of SRB is more positive than Eh of the media; Meanwhile, the depth of micro-pits increases approximately linearly with the immersion time. From standing point of cathodic depolarization of corrosion, there are many factors that affect the pit-growth of 18-8SS in the cultures of SRB; However, controlled by the repassivation behaviors of 18-8SS (Erep is more positive than the equilibrium potential of hydrogen electrode), sulfur element or polysulfide is the main factor that sustains the pit-growth instead. Additionally, due to the changes of the medium state parameters under influences of SRB, bacterial activities not only instantaneously affect the pit-initiation and the pit-growth, but also induce the modification of passive film in structure/properties and in turn affect the pitting corrosion as well.
In this thesis, sulfidation of passive film of 18-8SS in the cultures of SRB and its effects on the pitting corrosion were thorougly investigated. Results shows that sulfidation of passive film in the cultures of SRB causes a loss of passivity of 18-8SS, but sulfidation happened in the short term is more detrimental to the passive film than that in the long term. However, sulfidation polarizes the cathodic reactions to a greater extent, indicating that sulfidation can impede the pit-growth. Surface properties analyses of 18-8SS show that almost only iron oxides in the passive film were converted into sulfides in forms of FeS or FeS_2, while element Cr and Ni still remained essentially as oxides/hydroxides, which can explain definitely why sulfidation happened in the short term is more detrimental to the passive film than that in the long term, because the free oxygen resulted from sulfidation of iron oxides in the passive film probably can later recombine with other alloy elements to form other forms of unsulfidable oxides/hydroxides. On the other hand, it was also found that protective SRB biofilms can be formed in the cultures of SRB, which can impede pit-initiation /pit-growth of 18-8SS to some extent.
引文
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