低熔点金属与不锈钢表面交互作用的研究
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摘要
随着核电的快速发展,核电装备的国产化制造成为影响核电自主创新的关键环节。核电装备具有高可靠性和长寿命的特点,因此构件在加工制造过程中,对材料表面洁净度提出更高的要求。低熔点金属作为表面污染形式之一,尽管ASME和RCC-M标准明确禁止低熔点金属与过流部件表面接触,然而对低熔点金属如何与材料表面交互作用以及低熔点金属粘附后如何影响材料性能等问题的理解还不够深入。不锈钢是核电装备制造中广泛应用的材料,钝化是不锈钢的重要特性。但是,低熔点金属与不锈钢交互作用的研究还未见相关报道。因此本文研究低熔点金属与不锈钢之间的交互作用,分析不锈钢表面钝化状态对交互作用的影响规律并揭示交互作用机制,将对核电不锈钢装备的高洁净度制造提供理论依据和技术支持。
本文以低熔点金属Sn和Zn为对象,研究Sn、Zn与新鲜表面、空气自钝化及化学钝化等典型不锈钢表面的交互作用,分析了交互作用后形成的Fe-Sn禾(?)Fe-Zn化合物组织结构演变特征,基于组织结构特征提出了钝化影响交互作用的评估方法,结合不锈钢钝化膜质量的显色检测表征,揭示了钝化对交互作用的影响机制,探讨了低熔点金属Sn、Zn与不锈钢交互作用后,形成的化合物对不锈钢常温腐蚀性能和高温腐蚀性能的影响。主要结论如下：
(1)明确了低熔点金属Sn、Zn与不锈钢的交互作用。结果表明：当液相Sn与新鲜表面的不锈钢交互作用时,以形成片状和长条状的(Fe,Cr)Sn2化合物的方式发生冶金结合,固相Sn与不锈钢在220℃接触54h,不发生冶金结合作用；当液相和固相Zn与不锈钢交互作用时,以形成细小颗粒状的δ-(Fe,Cr)Zn10相和块状的ζ-(Fe,Cr)Zn13化合物的方式发生冶金结合。
(2)阐明了不锈钢表面钝化状态对交互作用的影响规律。结果表明：对于不同钝化状态的304不锈钢与低熔点金属Sn、Zn的交互作用,空气自钝化使Fe-Sn冶金结合层不均匀生长,化学钝化进一步抑制Fe-Sn化合物的形成；而钝化处理不能有效抑制Zn在不锈钢表面的冶金结合作用。对于不同种类的不锈钢与低熔点金属Sn的交互作用,420不锈钢表面完全被Fe-Sn化合物覆盖,钝化处理降低了化合物的生长速率但不能抑制化合物的形成；Fe-Sn化合物在钝化的316不锈钢表面局部生长,不锈钢空气自钝化的时间越长,生长化合物的覆盖率越小,厚度越低；液相Sn与空气自钝化和化学钝化的2205不锈钢未发生冶金结合作用。
(3)揭示了邻菲罗啉显色值—不锈钢钝化膜完整性—低熔点金属粘附程度之间的关系。结果表明：利用邻菲罗啉检测不锈钢表面,发现从新鲜表面到空气自钝化再到化学钝化,邻菲罗啉显色值逐渐降低,说明邻菲罗啉能够检测钝化膜的完整性,对比空气自钝化处理,化学钝化不锈钢表面生长相对较完整的钝化膜；不同钝化状态的不锈钢与低熔点金属Sn、Zn交互作用,发现形成化合物的粘附程度存在差异,从而提出表面覆盖率因子评价钝化膜对Sn、Zn与不锈钢交互作用的影响,建立覆盖率因子与显色值之间的关系,发现表面覆盖率因子与邻菲罗啉显色值之间存在线性关系,较大的邻菲罗啉显色值,钝化膜的完整性相对较低,钝化膜对低熔点金属Sn、Zn与不锈钢交互作用的阻碍能力降低,生长化合物的表面覆盖率增加。不锈钢表面钝化膜完整性是影响低熔点金属Sn、Zn与不锈钢交互作用的重要因素。
(4)研究了交互作用形成的Fe-Sn和Fe-Zn化合物对不锈钢常温腐蚀性能和高温腐蚀性能的影响。结果表明：在常温腐蚀条件下,Fe-Sn化合物粘附区域易于形成点蚀坑,进而加速了不锈钢的点蚀,并且化合物粘附的比例越大,不锈钢点蚀的数量越多。在高温高压水腐蚀条件下,Fe-Sn和Fe-Zn化合物粘附使腐蚀产物由不规则颗粒状的α-(Fe,Cr)2O3和多面体块状的(Fe, Cr)3O4向SnO2、ZnO和大块状Fe的氧化物转变,在长时间高温氧化条件下,低熔点金属氧化物的剥落,进一步降低不锈钢基体的耐腐蚀性能。
With the rapid development of nuclear power, the equipment manufacturing in localization has become the key factor for the independent innovation. Nuclear power equipment should have the characteristics of high reliability and long service life. Therefore, the quality assurance requirements for cleanness of nuclear power equipment during manufacturing are proposed. Low melting point metal contamination is one of the surface contaminations during manufacturing. Though the contact of low melting point metal is strongly prohibited by ASME and RCC-M international standards; the phenomena associated with the influence of low melting point metal on the material as well as the interactions between them can be considered as the issues requiring an in-depth study. Stainless steel is a widely used construction material in nuclear power plant. Passivation is an important characterization for stainless steel. However, the interaction of low melting point metal with stainless steel has not been studied till now. Therefore, the interaction of low melting point metal with stainless steel was investigated in the study. The effect of passivation on the interaction was analyzed and the interaction mechanism was revealed. The results could provide a theoretical basis and technical supports to the cleanness manufacturing for stainless steel equipment in nuclear power plant.
In the study, taking low melting point metals Sn and Zn as research object, the interaction of low melting point metal with stainless steel after passivation free, exposure in air and passivation in nitric acid was investigated. The microstructure evolution during the interaction was analyzed, and then the assessment method for the effect of passivation on the interaction was proposed. Combined with the chromaticity inspection of passive film on stainless steel, the interaction mechanism was revealed. The effect of low melting point metal on corrosion property at room temperature and corrosion property in high temperature water of stainless steel was discussed. The main conclusions are as follows:
(1) The interaction of low melting point metal with stainless steel was identified. Liquid Sn reacted with stainless steel by the formation of interfacial (Fe, Cr)Sn2layer with plated-type and block-type morphology, while there was no metallurgical intermetallics layer formation for the contact of solid Sn with stainless steel at220℃for54h. Liquid Zn and solid Zn reacted with stainless steel by the formation of interfacial columnar8phase (Fe, Cr)Zn10with tiny granule ζ phase (Fe, Cr)Zn13intermetallics.
(2) The effect of passivation on the interaction between low melting point metals and stainless steel was clarified. For the interaction of low melting point metal with passivation304stainless steel, the native oxide film grown in air resulted in the non-uniform growth of Fe-Sn intermetallics layer. The chemical passive film grown in nitric acid prevented the formation of Fe-Sn layer. Passivation did not effectively hinder the metallurgical adherence of Zn with stainless steel. For the interaction of Sn with stainless steels, liquid Sn was prone to metallurgically interact with420stainless steel by the formation of (Fe, Cr)Sn2intermetallics. Passivation decreased the growth rate of the intermetallics but can not prevent the intermetallics formation. Fe-Sn intermetallics grown on passivation316stainless steel were non-uniform, and the thickness and coverage ratio of the intermetallics decreased with the increasing exposure time in air. The metallurgical interaction of2205stainless steel with liquid Sn was prevented by passivation in air and chemical passivation.
(3) The relationship for pheanthroline colouration measurement—integrity of passive film grown on stainless steel—adherence degree of low melting point metal was revealed. The pheanthroline colouration measurement was employed to detect the stainless steel surface. Pheanthroline colouration value decreased with the increasing exposure time in air, but the pheanthroline solution did not change colour when it contacted with chemical passivation stainless steel. The integrity of passive film could be evaluated by the pheanthroline colouration measurement. Compared to the native film grown on stainless steel exposure air, the relative integrity passivation film grew on chemical passivation stainless steel. It is different for the adherence degree of Fe-Sn and Fe-Zn intermetallics on various passivation stainless steel. The coverage ratio factor was proposed to characterize the effect of passivation on the interaction between low melting point metal and stainless steel. The relationship of coverage ratio factor with pheanthroline colouration value was built. There was a linear relationship for the coverage ratio factor with the colouration value. The larger the colouration value of pheanthroline was, the lower the integrity of passive film was. The inhibition of passive film to the interaction between low melting point metal and stainless steel was decreased, so the coverage ratio of intermetallics increased. The integrity of passive film was an important factor for the interaction between low melting point metals with stainless steels.
(4) The effect of Fe-Sn and Fe-Zn intermetallics adherence on corrosion property at room temperature and corrosion property in high temperature water of stainless steel was investigated. For corrosion property at room temperature, Fe-Sn intermetallics adherence accelerated the pitting formation on stainless steel, and the pittings increased with the increasing amount of Fe-Sn intermetallics. For corrosion property in high temperature water, Fe-Sn and Fe-Zn intermetallics adherence changed the oxide scale from the irregularly shaped (Fe, Cr)2O3and faced (Fe, Cr)3O4particles to SnO2, ZnO and the faced substrate oxides. By increasing the oxide time, the corrosion resistance of stainless steel decreased because the SnO2and ZnO particles gradually fell off.
本文以低熔点金属Sn和Zn为对象,研究Sn、Zn与新鲜表面、空气自钝化及化学钝化等典型不锈钢表面的交互作用,分析了交互作用后形成的Fe-Sn禾(?)Fe-Zn化合物组织结构演变特征,基于组织结构特征提出了钝化影响交互作用的评估方法,结合不锈钢钝化膜质量的显色检测表征,揭示了钝化对交互作用的影响机制,探讨了低熔点金属Sn、Zn与不锈钢交互作用后,形成的化合物对不锈钢常温腐蚀性能和高温腐蚀性能的影响。主要结论如下：
(1)明确了低熔点金属Sn、Zn与不锈钢的交互作用。结果表明：当液相Sn与新鲜表面的不锈钢交互作用时,以形成片状和长条状的(Fe,Cr)Sn2化合物的方式发生冶金结合,固相Sn与不锈钢在220℃接触54h,不发生冶金结合作用；当液相和固相Zn与不锈钢交互作用时,以形成细小颗粒状的δ-(Fe,Cr)Zn10相和块状的ζ-(Fe,Cr)Zn13化合物的方式发生冶金结合。
(2)阐明了不锈钢表面钝化状态对交互作用的影响规律。结果表明：对于不同钝化状态的304不锈钢与低熔点金属Sn、Zn的交互作用,空气自钝化使Fe-Sn冶金结合层不均匀生长,化学钝化进一步抑制Fe-Sn化合物的形成；而钝化处理不能有效抑制Zn在不锈钢表面的冶金结合作用。对于不同种类的不锈钢与低熔点金属Sn的交互作用,420不锈钢表面完全被Fe-Sn化合物覆盖,钝化处理降低了化合物的生长速率但不能抑制化合物的形成；Fe-Sn化合物在钝化的316不锈钢表面局部生长,不锈钢空气自钝化的时间越长,生长化合物的覆盖率越小,厚度越低；液相Sn与空气自钝化和化学钝化的2205不锈钢未发生冶金结合作用。
(3)揭示了邻菲罗啉显色值—不锈钢钝化膜完整性—低熔点金属粘附程度之间的关系。结果表明：利用邻菲罗啉检测不锈钢表面,发现从新鲜表面到空气自钝化再到化学钝化,邻菲罗啉显色值逐渐降低,说明邻菲罗啉能够检测钝化膜的完整性,对比空气自钝化处理,化学钝化不锈钢表面生长相对较完整的钝化膜；不同钝化状态的不锈钢与低熔点金属Sn、Zn交互作用,发现形成化合物的粘附程度存在差异,从而提出表面覆盖率因子评价钝化膜对Sn、Zn与不锈钢交互作用的影响,建立覆盖率因子与显色值之间的关系,发现表面覆盖率因子与邻菲罗啉显色值之间存在线性关系,较大的邻菲罗啉显色值,钝化膜的完整性相对较低,钝化膜对低熔点金属Sn、Zn与不锈钢交互作用的阻碍能力降低,生长化合物的表面覆盖率增加。不锈钢表面钝化膜完整性是影响低熔点金属Sn、Zn与不锈钢交互作用的重要因素。
(4)研究了交互作用形成的Fe-Sn和Fe-Zn化合物对不锈钢常温腐蚀性能和高温腐蚀性能的影响。结果表明：在常温腐蚀条件下,Fe-Sn化合物粘附区域易于形成点蚀坑,进而加速了不锈钢的点蚀,并且化合物粘附的比例越大,不锈钢点蚀的数量越多。在高温高压水腐蚀条件下,Fe-Sn和Fe-Zn化合物粘附使腐蚀产物由不规则颗粒状的α-(Fe,Cr)2O3和多面体块状的(Fe, Cr)3O4向SnO2、ZnO和大块状Fe的氧化物转变,在长时间高温氧化条件下,低熔点金属氧化物的剥落,进一步降低不锈钢基体的耐腐蚀性能。
With the rapid development of nuclear power, the equipment manufacturing in localization has become the key factor for the independent innovation. Nuclear power equipment should have the characteristics of high reliability and long service life. Therefore, the quality assurance requirements for cleanness of nuclear power equipment during manufacturing are proposed. Low melting point metal contamination is one of the surface contaminations during manufacturing. Though the contact of low melting point metal is strongly prohibited by ASME and RCC-M international standards; the phenomena associated with the influence of low melting point metal on the material as well as the interactions between them can be considered as the issues requiring an in-depth study. Stainless steel is a widely used construction material in nuclear power plant. Passivation is an important characterization for stainless steel. However, the interaction of low melting point metal with stainless steel has not been studied till now. Therefore, the interaction of low melting point metal with stainless steel was investigated in the study. The effect of passivation on the interaction was analyzed and the interaction mechanism was revealed. The results could provide a theoretical basis and technical supports to the cleanness manufacturing for stainless steel equipment in nuclear power plant.
In the study, taking low melting point metals Sn and Zn as research object, the interaction of low melting point metal with stainless steel after passivation free, exposure in air and passivation in nitric acid was investigated. The microstructure evolution during the interaction was analyzed, and then the assessment method for the effect of passivation on the interaction was proposed. Combined with the chromaticity inspection of passive film on stainless steel, the interaction mechanism was revealed. The effect of low melting point metal on corrosion property at room temperature and corrosion property in high temperature water of stainless steel was discussed. The main conclusions are as follows:
(1) The interaction of low melting point metal with stainless steel was identified. Liquid Sn reacted with stainless steel by the formation of interfacial (Fe, Cr)Sn2layer with plated-type and block-type morphology, while there was no metallurgical intermetallics layer formation for the contact of solid Sn with stainless steel at220℃for54h. Liquid Zn and solid Zn reacted with stainless steel by the formation of interfacial columnar8phase (Fe, Cr)Zn10with tiny granule ζ phase (Fe, Cr)Zn13intermetallics.
(2) The effect of passivation on the interaction between low melting point metals and stainless steel was clarified. For the interaction of low melting point metal with passivation304stainless steel, the native oxide film grown in air resulted in the non-uniform growth of Fe-Sn intermetallics layer. The chemical passive film grown in nitric acid prevented the formation of Fe-Sn layer. Passivation did not effectively hinder the metallurgical adherence of Zn with stainless steel. For the interaction of Sn with stainless steels, liquid Sn was prone to metallurgically interact with420stainless steel by the formation of (Fe, Cr)Sn2intermetallics. Passivation decreased the growth rate of the intermetallics but can not prevent the intermetallics formation. Fe-Sn intermetallics grown on passivation316stainless steel were non-uniform, and the thickness and coverage ratio of the intermetallics decreased with the increasing exposure time in air. The metallurgical interaction of2205stainless steel with liquid Sn was prevented by passivation in air and chemical passivation.
(3) The relationship for pheanthroline colouration measurement—integrity of passive film grown on stainless steel—adherence degree of low melting point metal was revealed. The pheanthroline colouration measurement was employed to detect the stainless steel surface. Pheanthroline colouration value decreased with the increasing exposure time in air, but the pheanthroline solution did not change colour when it contacted with chemical passivation stainless steel. The integrity of passive film could be evaluated by the pheanthroline colouration measurement. Compared to the native film grown on stainless steel exposure air, the relative integrity passivation film grew on chemical passivation stainless steel. It is different for the adherence degree of Fe-Sn and Fe-Zn intermetallics on various passivation stainless steel. The coverage ratio factor was proposed to characterize the effect of passivation on the interaction between low melting point metal and stainless steel. The relationship of coverage ratio factor with pheanthroline colouration value was built. There was a linear relationship for the coverage ratio factor with the colouration value. The larger the colouration value of pheanthroline was, the lower the integrity of passive film was. The inhibition of passive film to the interaction between low melting point metal and stainless steel was decreased, so the coverage ratio of intermetallics increased. The integrity of passive film was an important factor for the interaction between low melting point metals with stainless steels.
(4) The effect of Fe-Sn and Fe-Zn intermetallics adherence on corrosion property at room temperature and corrosion property in high temperature water of stainless steel was investigated. For corrosion property at room temperature, Fe-Sn intermetallics adherence accelerated the pitting formation on stainless steel, and the pittings increased with the increasing amount of Fe-Sn intermetallics. For corrosion property in high temperature water, Fe-Sn and Fe-Zn intermetallics adherence changed the oxide scale from the irregularly shaped (Fe, Cr)2O3and faced (Fe, Cr)3O4particles to SnO2, ZnO and the faced substrate oxides. By increasing the oxide time, the corrosion resistance of stainless steel decreased because the SnO2and ZnO particles gradually fell off.
引文
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