Ⅰ.Cu薄膜与机械研磨处理Fe表面的腐蚀与扩散行为研究 Ⅱ.X-65钢表面高性能复合涂层缺陷处的局部腐蚀行为研究
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摘要
本文采用双课题形式,以第一部分为主体内容。
第一部分:
腐蚀与扩散是材料的两个重要性能。在纳米材料的制备、工艺、失效分析及可靠性评估等领域中,均涉及到材料的腐蚀与扩散问题。然而,到目前为止,纳米材料方面的研究工作内容,主要集中在制备工艺,结构表征,组织结构与力学、电学、磁学、热学,光学及催化性能等方面的关系。腐蚀与扩散方面的研究较少涉及。澄清纳米材料中的腐蚀与扩散规律,对可控纳米结构的实现、纳米材料的稳定性、材料应用与失效分析及纳米化技术的产业应用等都具有重要意义。
本文选取了两种典型工艺所制备的纳米材料作为研究对象,一个是真空蒸发方法所制备的纳米尺度金属Cu薄膜。研究了氧化传质前后薄膜组分、结构和形貌变化。建立了两种新的氧化传质表征方法,即透射光谱法与方块电阻法。着重研究了不同厚度体系下的Cu薄膜氧化传质的实验规律及其理论模型,发现极薄膜情况下由隧穿控制的快速场致迁移规律。另一个是表面机械研磨处理(SMAT)技术所制备的表面纳米化纯Fe。研究了表面纳米化处理对纯Fe的电化学腐蚀行为的影响,揭示了电化学腐蚀速率随纳米化程度加深而增加的特殊规律,并与表面纳米化316不锈钢进行了对比。利用二次离子质谱技术(SIMS)研究了Al在SMAT纯Fe纳米结构表层中的低温扩散性能,获取了相关扩散参数,发现Al在纳米晶表层中的加速扩散行为。
主要研究结果如下:
1.研究了140℃下7～25 nm厚度范围内Cu薄膜的氧化行为。采用真空蒸发法以不同沉积速率制备一系列Cu薄膜,利用原子力显微镜(AFM)观察其微观形貌,选取形貌良好的Cu薄膜样品。采用方块电阻和透射光谱两种方法为表征手段,得到7～25 nm范围内不同厚度Cu薄膜的氧化反应动力学曲线。结果表明,厚度极薄(d_(Cu)<14 nm)的Cu薄膜在140℃恒温下氧化反应出现异常加速,其动力学行为满足反对数生长规律。
2.建立了基于方块电阻测量的原位表征Cu薄膜氧化反应动力学规律的方法。利用Cu薄膜方块电阻随氧化时间的变化情况,得到氧化产物厚度与氧化时间的关系。结果发现,当Cu膜较厚时,氧化反应动力学结果符合抛物线规律。还利用不同的氧化反应温度条件和对应的抛物线常数之间的关系得到体系的扩散激活能,并利用激活能推测其微观扩散机制。结果表明,该方法适用于表征纳米尺度薄膜的氧化反应体系。
3.经SMAT处理后,纯Fe与316不锈钢的耐腐蚀性能均下降。晶粒细化是纯Fe耐蚀性能下降的主要原因。对316不锈钢样品而言,除晶粒细化因素外,表面纳米化后,316不锈钢发生马氏体相变,这种奥氏体和马氏体不同相的存在也会导致材料耐腐蚀性能的下降。
4.在300～380℃温度范围内,Al在SMAT制备的纯Fe纳米晶表层中的扩散系数比Al在粗晶纯Fe中的扩散系数高6～7个量级,扩散激活能为1.40 eV,明显低于文献报道的Al在a-Fe中的扩散激活能(2.28 eV)。分析表明,扩散性能的提高源于纳米晶表层中大量高密度位错和高晶界储能的非平衡晶界,以及在随后的热处理过程中高密度位错的运动、湮灭过程。
5.经SMAT处理的纯Fe样品在400℃低温固体粉末渗铝处理后,即可获得一定Al元素渗入。而通过低温结合中高温的接续渗铝法,可进一步显著改善渗层的质量,渗铝层的厚度更厚(约为20μm)且分布十分均匀连续。经过渗铝处理后,SMAT纯Fe样品的阳极腐蚀电流密度显著下降,且经低温接续渗铝处理的样品出现了明显的钝化行为,表明低温渗铝处理可显著改善SMAT样品的抗腐蚀性能。
第二部分:
电化学阻抗谱(EIS)技术被广泛应用于表征涂层性能以及钢铁基体在涂层下所发生的腐蚀反应。然而,传统的EIS测量所得的电化学阻抗信号来自于整个工作电极,它反映的是宏观电极的一个平均行为。这就会导致钢铁在涂层的一些微小缺陷,如针孔处所发生的局部电化学腐蚀反应过程“淹没”在平均信号之中。局部电化学阻抗谱(LEIS)技术的出现为研究涂层在局部的退化行为以及钢铁基体在涂层缺陷处所发生的局部腐蚀行为提供了广泛的可能性。目前,涂层/基底钢铁体系的电化学腐蚀行为研究,大多采用传统的整体阻抗分析,鲜有研究报道关注于电极表面的局部电化学阻抗特性。
因此,本部分的工作采用局部电化学阻抗(LEIS)技术研究了涂覆有高性能复合涂层(HPCC)的管线钢样品,在涂层缺陷处的局部腐蚀过程与机制。考虑管线钢实际使用环境,实验介质为近中性pH的NS4溶液。并与针对整个工作电极测量所得的传统电化学阻抗谱结果进行了对比。该工作对揭示近中性pH溶液中,管线钢在涂层缺陷处的局部腐蚀行为有重要科学意义和实践意义。
主要研究结果如下:
1.涂层缺陷处的局部电化学阻抗信号与缺陷尺寸有密切联系。局部电化学阻抗谱结果表明:小尺寸缺陷(例如直径小于200μm)处所发生的局部腐蚀反应过程与机制随着时间发生变化。由于腐蚀产物的沉积以及大的涂层厚度/缺陷比例,使得扩散过程最终控制了界面的腐蚀反应。当涂层含有较大尺寸的缺陷时(如直径1000μm),低频处的局部电化学阻抗信号始终表现为缺陷处,基底金属界面所发生的电荷转移反应。由于缺陷的尺寸较大,体系较为开放,因此并没有观察到腐蚀产物沉积所带来的阻塞效应。
2.通过与局部电化学阻抗谱结果对比,发现传统的针对整个含缺陷涂层的工作电极测量所得的电化学阻抗信号同时来自于涂层与缺陷处的信号,难以精确反映在小尺寸缺陷处所发生的局部电化学腐蚀过程与机制等信息。
Part 1:
Corrosion and diffusion are two important properties of materials.They are involved in many fields,including preparation,application,failure analysis and reliability evaluation of nanomaterials.Up to date,majority studies on nanomaterials have been mainly focused on the preparation of nanomaterials,characterization of nanostructure and the properties of nanomaterials including mechanical,electric, optical,magnetic and catalytic properties.However,few studies have been concerned with corrosion and diffusion properties of nanomaterials.It is of significant importance to clarify the corrosion and diffusion behaviour of nanomaterials both in a scientifical and practical way.
In this paper,two different typical nanomaterials were selected to investigate the corrosion and diffusion behaviour in nanomaterials.One is nanoscale Cu thin film prepared by vacuum deposition.The structure,composition and surface morphology change of Cu thin film after oxidation were studied.Two new methods for characterizing oxidation kinetics of thin films were established by using sheet resistance measurement or optical transmittance measurement.The oxidation behaviour of Cu thin films with different thicknesses was investigated,and an abnormal accelerated transport phenomenon controlled by tunneling effect was observed.Another is surface nanocrystallized Fe prepared by surface mechanical attrition treatment(SMAT).The effect of SMAT on the electrochemical corrosion behaviour of Fe was investigated,and the results showed that the corrosion rate increased with the increasing degree of nanocrystallization.The diffusion behaviour of A1 in SMAT Fe in low temperatures was studied by secondary ion mass spectroscopy(SIMS).The relevant diffusion parameters were obtained and accelerated diffusion behaviour of A1 in nanocrystalline surface layer of Fe was observed.
The main results are as follows:
1.The oxidation behaviour of Cu thin films with 7～25 nm thicknesses at 140℃was investigated.Cu thin films with smooth surface morphology were prepared by vacuum deposition with controlled evaporation rate.The oxidation kinetics of Cu thin films was characterized by using the sheet resistance and optical transmittance measurements.The results showed that the oxidation behaviour of Cu films was accelerated obviously when the thickness of Cu film was ultra thin(dcu＜14 nm) and the oxidation kinetics followed inverse logarithm law.
2.The oxidation kinetics of Cu thin films was also characterized by measuring the sheet resistance of Cu films during oxidation.It was found that when the film was relatively thick,the oxidation kinetics followed traditional parabolic law.Furthermore, the diffusion mechanism in Cu film during oxidation was discussed based on the value of the diffusion energy.The results showed that the method was effective for characterizing oxidation kinetics of nanoscale thin films.
3.The corrosion resistances of both Fe and 316 stainless steels were decreased after surface mechanical attrition treatment(SMAT).Grain refinement was the main reason for decreasing corrosion resistance of Fe.For 316 stainless steels,besides the reason of grain refinement,the martensitic transformation during SMAT was another reason for deterioration of corrosion resistance.
4.Within a temperature range of 300～380℃,the diffusivity of A1 in the nanocrystalline Fe prepared by SMAT was 6-7 orders of magnitude higher than that in coarse-grained Fe.The diffusion activation energy of A1 diffusion in nanocrystalline Fe was 1.40 eV,which was much smaller than that for the A1 diffusion inα-Fe (2.28eV).The enhanced diffusivity of A1 was originated from high density dislocations and a large volume fraction of nonequilibrium grain boundaries in nanocrystalline surface layer of Fe.
5.Powder aluminizing could be achieved at a much lower temperature,i.e.,400℃,for SMAT sample.Furthermore,a much thicker(about 20μm) and more continuous aluminized layer was obtained by an optimized successive aluminizing process.The current density of the aluminized SMAT sample decreased significantly, and obvious passivation behaviour was found for the SMAT sample processed by successive aluminizing.The results suggested that lower aluminizing treatment of SMAT sample could significantly improve the corrosion resistance of SMAT sample.
Part 2:
Electrochemical impedance spectroscopy(EIS) technique has been used extensively to characterize the coating performance and the corrosion of steel under the coating.However,EIS measurement is associated with a major shortcoming,i.e., the measured impedance result is attributed to the electrochemical response of the whole electrode,reflecting an“averaged”behaviour of the macroscopic electrode.As a consequence,local electrochemical process occurring at micro-defect such as pinhole in the coating is“averaged”out.Therefore,analysis of EIS data is incapable of revealing the process and mechanism of localized electrochemical corrosion reaction of steel under coating with micro-scaled defects.Without such information,it will be impossible to develop a complete understanding of localized coating degradation and the resultant corrosion of the steel.
Localized EIS(LEIS) measurements provide a promising alternative to investigate microscopically the coating degradation and localized corrosion of steel under coating.To date,there has been very limited work to characterize electrochemically the coating property for prevention of corrosion of steel,especially the localized corrosion process normally occurring at microdefects,such as pinholes in the coating.
Therefore,in this work,LEIS measurements were performed on HPCC-coated pipe steel to investigate the localized corrosion process and mechanism of steel under the defected coating in a near-neutral pH solution.LEIS plots were measured either directly above the defect over a certain frequency range or by mapping the defected area at a single measurement frequency.For comparison,conventional EIS measurements were also conducted on the macroscopic electrode.It is anticipated that this research provides an essential insight into the mechanism of localized corrosion of steel under defected coating in near-neutral pH solution.
The main results are as follows:
1.The LEIS responses measured at the defected coating is dependent on the size of the defect.For small defects,e.g.,less than 200μm diameter,localized corrosion process and mechanism of steel,as indicated by the measured LEIS plots,change with time.The diffusion process dominates the interfacial corrosion reaction,which is due to the block effect of the deposited corrosion product combined with the geometrical factor of a large coating thickness/defect width ratio.In the presence of a big defect, e.g.,up to 1000μm,the LEIS responses measured at the defect are always featured by a coating impedance in the high-frequency range and an interfacial corrosion reaction in the low-frequency range.The block effect of corrosion product does not apply due to the relatively open geometry associated with the big defect.
2.Conventional EIS measurements on a macroscopic-coated electrode reflect the“averaged”impedance results from both coating and defect.The information of the localized electrochemical corrosion processes and mechanisms at the small defect is lost,and the coating impedance information is“averaged”out when a big defect is contained.
第一部分:
腐蚀与扩散是材料的两个重要性能。在纳米材料的制备、工艺、失效分析及可靠性评估等领域中,均涉及到材料的腐蚀与扩散问题。然而,到目前为止,纳米材料方面的研究工作内容,主要集中在制备工艺,结构表征,组织结构与力学、电学、磁学、热学,光学及催化性能等方面的关系。腐蚀与扩散方面的研究较少涉及。澄清纳米材料中的腐蚀与扩散规律,对可控纳米结构的实现、纳米材料的稳定性、材料应用与失效分析及纳米化技术的产业应用等都具有重要意义。
本文选取了两种典型工艺所制备的纳米材料作为研究对象,一个是真空蒸发方法所制备的纳米尺度金属Cu薄膜。研究了氧化传质前后薄膜组分、结构和形貌变化。建立了两种新的氧化传质表征方法,即透射光谱法与方块电阻法。着重研究了不同厚度体系下的Cu薄膜氧化传质的实验规律及其理论模型,发现极薄膜情况下由隧穿控制的快速场致迁移规律。另一个是表面机械研磨处理(SMAT)技术所制备的表面纳米化纯Fe。研究了表面纳米化处理对纯Fe的电化学腐蚀行为的影响,揭示了电化学腐蚀速率随纳米化程度加深而增加的特殊规律,并与表面纳米化316不锈钢进行了对比。利用二次离子质谱技术(SIMS)研究了Al在SMAT纯Fe纳米结构表层中的低温扩散性能,获取了相关扩散参数,发现Al在纳米晶表层中的加速扩散行为。
主要研究结果如下:
1.研究了140℃下7～25 nm厚度范围内Cu薄膜的氧化行为。采用真空蒸发法以不同沉积速率制备一系列Cu薄膜,利用原子力显微镜(AFM)观察其微观形貌,选取形貌良好的Cu薄膜样品。采用方块电阻和透射光谱两种方法为表征手段,得到7～25 nm范围内不同厚度Cu薄膜的氧化反应动力学曲线。结果表明,厚度极薄(d_(Cu)<14 nm)的Cu薄膜在140℃恒温下氧化反应出现异常加速,其动力学行为满足反对数生长规律。
2.建立了基于方块电阻测量的原位表征Cu薄膜氧化反应动力学规律的方法。利用Cu薄膜方块电阻随氧化时间的变化情况,得到氧化产物厚度与氧化时间的关系。结果发现,当Cu膜较厚时,氧化反应动力学结果符合抛物线规律。还利用不同的氧化反应温度条件和对应的抛物线常数之间的关系得到体系的扩散激活能,并利用激活能推测其微观扩散机制。结果表明,该方法适用于表征纳米尺度薄膜的氧化反应体系。
3.经SMAT处理后,纯Fe与316不锈钢的耐腐蚀性能均下降。晶粒细化是纯Fe耐蚀性能下降的主要原因。对316不锈钢样品而言,除晶粒细化因素外,表面纳米化后,316不锈钢发生马氏体相变,这种奥氏体和马氏体不同相的存在也会导致材料耐腐蚀性能的下降。
4.在300～380℃温度范围内,Al在SMAT制备的纯Fe纳米晶表层中的扩散系数比Al在粗晶纯Fe中的扩散系数高6～7个量级,扩散激活能为1.40 eV,明显低于文献报道的Al在a-Fe中的扩散激活能(2.28 eV)。分析表明,扩散性能的提高源于纳米晶表层中大量高密度位错和高晶界储能的非平衡晶界,以及在随后的热处理过程中高密度位错的运动、湮灭过程。
5.经SMAT处理的纯Fe样品在400℃低温固体粉末渗铝处理后,即可获得一定Al元素渗入。而通过低温结合中高温的接续渗铝法,可进一步显著改善渗层的质量,渗铝层的厚度更厚(约为20μm)且分布十分均匀连续。经过渗铝处理后,SMAT纯Fe样品的阳极腐蚀电流密度显著下降,且经低温接续渗铝处理的样品出现了明显的钝化行为,表明低温渗铝处理可显著改善SMAT样品的抗腐蚀性能。
第二部分:
电化学阻抗谱(EIS)技术被广泛应用于表征涂层性能以及钢铁基体在涂层下所发生的腐蚀反应。然而,传统的EIS测量所得的电化学阻抗信号来自于整个工作电极,它反映的是宏观电极的一个平均行为。这就会导致钢铁在涂层的一些微小缺陷,如针孔处所发生的局部电化学腐蚀反应过程“淹没”在平均信号之中。局部电化学阻抗谱(LEIS)技术的出现为研究涂层在局部的退化行为以及钢铁基体在涂层缺陷处所发生的局部腐蚀行为提供了广泛的可能性。目前,涂层/基底钢铁体系的电化学腐蚀行为研究,大多采用传统的整体阻抗分析,鲜有研究报道关注于电极表面的局部电化学阻抗特性。
因此,本部分的工作采用局部电化学阻抗(LEIS)技术研究了涂覆有高性能复合涂层(HPCC)的管线钢样品,在涂层缺陷处的局部腐蚀过程与机制。考虑管线钢实际使用环境,实验介质为近中性pH的NS4溶液。并与针对整个工作电极测量所得的传统电化学阻抗谱结果进行了对比。该工作对揭示近中性pH溶液中,管线钢在涂层缺陷处的局部腐蚀行为有重要科学意义和实践意义。
主要研究结果如下:
1.涂层缺陷处的局部电化学阻抗信号与缺陷尺寸有密切联系。局部电化学阻抗谱结果表明:小尺寸缺陷(例如直径小于200μm)处所发生的局部腐蚀反应过程与机制随着时间发生变化。由于腐蚀产物的沉积以及大的涂层厚度/缺陷比例,使得扩散过程最终控制了界面的腐蚀反应。当涂层含有较大尺寸的缺陷时(如直径1000μm),低频处的局部电化学阻抗信号始终表现为缺陷处,基底金属界面所发生的电荷转移反应。由于缺陷的尺寸较大,体系较为开放,因此并没有观察到腐蚀产物沉积所带来的阻塞效应。
2.通过与局部电化学阻抗谱结果对比,发现传统的针对整个含缺陷涂层的工作电极测量所得的电化学阻抗信号同时来自于涂层与缺陷处的信号,难以精确反映在小尺寸缺陷处所发生的局部电化学腐蚀过程与机制等信息。
Part 1:
Corrosion and diffusion are two important properties of materials.They are involved in many fields,including preparation,application,failure analysis and reliability evaluation of nanomaterials.Up to date,majority studies on nanomaterials have been mainly focused on the preparation of nanomaterials,characterization of nanostructure and the properties of nanomaterials including mechanical,electric, optical,magnetic and catalytic properties.However,few studies have been concerned with corrosion and diffusion properties of nanomaterials.It is of significant importance to clarify the corrosion and diffusion behaviour of nanomaterials both in a scientifical and practical way.
In this paper,two different typical nanomaterials were selected to investigate the corrosion and diffusion behaviour in nanomaterials.One is nanoscale Cu thin film prepared by vacuum deposition.The structure,composition and surface morphology change of Cu thin film after oxidation were studied.Two new methods for characterizing oxidation kinetics of thin films were established by using sheet resistance measurement or optical transmittance measurement.The oxidation behaviour of Cu thin films with different thicknesses was investigated,and an abnormal accelerated transport phenomenon controlled by tunneling effect was observed.Another is surface nanocrystallized Fe prepared by surface mechanical attrition treatment(SMAT).The effect of SMAT on the electrochemical corrosion behaviour of Fe was investigated,and the results showed that the corrosion rate increased with the increasing degree of nanocrystallization.The diffusion behaviour of A1 in SMAT Fe in low temperatures was studied by secondary ion mass spectroscopy(SIMS).The relevant diffusion parameters were obtained and accelerated diffusion behaviour of A1 in nanocrystalline surface layer of Fe was observed.
The main results are as follows:
1.The oxidation behaviour of Cu thin films with 7～25 nm thicknesses at 140℃was investigated.Cu thin films with smooth surface morphology were prepared by vacuum deposition with controlled evaporation rate.The oxidation kinetics of Cu thin films was characterized by using the sheet resistance and optical transmittance measurements.The results showed that the oxidation behaviour of Cu films was accelerated obviously when the thickness of Cu film was ultra thin(dcu＜14 nm) and the oxidation kinetics followed inverse logarithm law.
2.The oxidation kinetics of Cu thin films was also characterized by measuring the sheet resistance of Cu films during oxidation.It was found that when the film was relatively thick,the oxidation kinetics followed traditional parabolic law.Furthermore, the diffusion mechanism in Cu film during oxidation was discussed based on the value of the diffusion energy.The results showed that the method was effective for characterizing oxidation kinetics of nanoscale thin films.
3.The corrosion resistances of both Fe and 316 stainless steels were decreased after surface mechanical attrition treatment(SMAT).Grain refinement was the main reason for decreasing corrosion resistance of Fe.For 316 stainless steels,besides the reason of grain refinement,the martensitic transformation during SMAT was another reason for deterioration of corrosion resistance.
4.Within a temperature range of 300～380℃,the diffusivity of A1 in the nanocrystalline Fe prepared by SMAT was 6-7 orders of magnitude higher than that in coarse-grained Fe.The diffusion activation energy of A1 diffusion in nanocrystalline Fe was 1.40 eV,which was much smaller than that for the A1 diffusion inα-Fe (2.28eV).The enhanced diffusivity of A1 was originated from high density dislocations and a large volume fraction of nonequilibrium grain boundaries in nanocrystalline surface layer of Fe.
5.Powder aluminizing could be achieved at a much lower temperature,i.e.,400℃,for SMAT sample.Furthermore,a much thicker(about 20μm) and more continuous aluminized layer was obtained by an optimized successive aluminizing process.The current density of the aluminized SMAT sample decreased significantly, and obvious passivation behaviour was found for the SMAT sample processed by successive aluminizing.The results suggested that lower aluminizing treatment of SMAT sample could significantly improve the corrosion resistance of SMAT sample.
Part 2:
Electrochemical impedance spectroscopy(EIS) technique has been used extensively to characterize the coating performance and the corrosion of steel under the coating.However,EIS measurement is associated with a major shortcoming,i.e., the measured impedance result is attributed to the electrochemical response of the whole electrode,reflecting an“averaged”behaviour of the macroscopic electrode.As a consequence,local electrochemical process occurring at micro-defect such as pinhole in the coating is“averaged”out.Therefore,analysis of EIS data is incapable of revealing the process and mechanism of localized electrochemical corrosion reaction of steel under coating with micro-scaled defects.Without such information,it will be impossible to develop a complete understanding of localized coating degradation and the resultant corrosion of the steel.
Localized EIS(LEIS) measurements provide a promising alternative to investigate microscopically the coating degradation and localized corrosion of steel under coating.To date,there has been very limited work to characterize electrochemically the coating property for prevention of corrosion of steel,especially the localized corrosion process normally occurring at microdefects,such as pinholes in the coating.
Therefore,in this work,LEIS measurements were performed on HPCC-coated pipe steel to investigate the localized corrosion process and mechanism of steel under the defected coating in a near-neutral pH solution.LEIS plots were measured either directly above the defect over a certain frequency range or by mapping the defected area at a single measurement frequency.For comparison,conventional EIS measurements were also conducted on the macroscopic electrode.It is anticipated that this research provides an essential insight into the mechanism of localized corrosion of steel under defected coating in near-neutral pH solution.
The main results are as follows:
1.The LEIS responses measured at the defected coating is dependent on the size of the defect.For small defects,e.g.,less than 200μm diameter,localized corrosion process and mechanism of steel,as indicated by the measured LEIS plots,change with time.The diffusion process dominates the interfacial corrosion reaction,which is due to the block effect of the deposited corrosion product combined with the geometrical factor of a large coating thickness/defect width ratio.In the presence of a big defect, e.g.,up to 1000μm,the LEIS responses measured at the defect are always featured by a coating impedance in the high-frequency range and an interfacial corrosion reaction in the low-frequency range.The block effect of corrosion product does not apply due to the relatively open geometry associated with the big defect.
2.Conventional EIS measurements on a macroscopic-coated electrode reflect the“averaged”impedance results from both coating and defect.The information of the localized electrochemical corrosion processes and mechanisms at the small defect is lost,and the coating impedance information is“averaged”out when a big defect is contained.
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