金属腐蚀研究中具有时间—空间分辨的电化学技术
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摘要
随着腐蚀电化学研究的不断深化，研究人员已不再满足于应用传统的腐蚀电化学技术手段，各种具有时间-空间分辨能力的电化学技术手段正逐渐受到广泛关注。这些技术包括：各种原位(in situ)和非原位(ex situ)的扫描探针显微技术、光谱探针技术、电子探针技术、电化学噪音技术以及多种技术的联用等。
本文工作主要由两部分内容组成：(1)应用多种现有已商品化的具有时间-空间分辨能力的电化学新技术和方法，包括超高景深共聚焦光学显微镜、原位原子力显微镜、电子探针、电化学噪音技术及扫描Kelvin探针显微镜技术等，对不锈钢局部腐蚀过程进行综合研究，深入探讨不锈钢在不同环境介质中的腐蚀特征及本质机理；(2)侧重发展新的时间-空间分辨的电化学仪器方法，并应用这些仪器方法对相应的实际腐蚀体系进行研究。取得主要研究进展和成果如下：
1．运用超高景深共焦光学显微镜对18-8不锈钢在不同溶液介质中的腐蚀过程进行了原位实时观测。在连续的原位光学显微图像数据采集基础上，运用Photoshop图像处理软件实现了光学示差图像分析，通过图像示差分析，极大地提高了原位光学显微观测腐蚀过程的灵敏度，可捕捉不同腐蚀阶段金属表面形貌结构的细微变化。实验发现，不锈钢在HCl溶液中的腐蚀过程存在诱导期、发展期和稳定期三个不同阶段，诱导期为不锈钢表面钝化膜的局部破裂溶解而导致亚稳态腐蚀点的诱导产生；发展期则表现为大量亚稳态腐蚀点的形成与再钝化；稳定期表现为腐蚀活性点的持续溶解或宏观点腐蚀的形成与稳定生长；
2．运用原位原子力显微镜技术对18-8不锈钢在HCl溶液中腐蚀的早期过程进行研究，发现在腐蚀的早期过程存在明显的表面钝化膜的溶解和亚稳态腐蚀点的形成；对不锈钢表面腐蚀前后进行SEM形貌分析和表面元素分布的电子探针测量，结果表明18-8不锈钢表面TiN颗粒的边界是腐蚀优先发生的位点，小尺寸的TiN颗粒边界更易于生成腐蚀活性点；采用扫描Kelvin探针显微技术，对18-8不锈钢表面形貌与Volta电位分布进行了关联研究，发现TiN颗粒边界位点与金属基底间存在明显的电位差异，由于“微电偶”和“微缝隙”的作用，从而导致在腐蚀性介质中形成腐蚀微电池，诱发局部腐蚀在TiN颗粒边界位点优先发生；
3．研究了18-8不锈钢在不同溶液介质中的电化学噪音，并运用小波分析方法对噪音数据进行解析，通过综合分析电化学噪音小波系数能量分布图的变化趋势，并综合应用光学显微镜、电子探针、原位原子力显微镜的联合研究，首次对电化学噪音数据中各小波系数所对应的腐蚀事件及物理意义进行了指认；
4．进一步建立了扫描微电极／扫描隧道显微镜联用系统，成功实现了两种技术的联用。研制了一系列电化学扫描微探针，包括金属Pt电位探针、Cl~-选择性微探针、pH选择性微探针和电位／形貌复合PtIr合金微探针，这些探针经过相应的性能测试和实验测试，证明可有效地应用于各种腐蚀体系关键性腐蚀参数的实际测量。运用所建立的SMET／STM联用测量仪器，并基于隧道电流的可控制探针尖端与样品表面距离的强大功能，大大提高了金属表面腐蚀过程电位分布、Cl~-浓度分布及pH分布等测量的空间灵敏度和空间分辨度。对表面点腐蚀位点和非腐蚀活性位点进行了纵向电位分布测量，结果表明纵向电位分布图可直接反映表面腐蚀发生发展过程的变化，不锈钢表面腐蚀活性点和非腐蚀活性点的金属／溶液界面电位分布特征存在明显差异，利用仪器的距离-电位曲线测量功能，可对金属／溶液界面双电层结构进行深入研究。成功地获得了18-8不锈钢表面腐蚀过程电位分布图和局部腐蚀点区域的形貌结构，从而实现局部腐蚀的原位构-性研究，为金属／溶液界面电化学研究提供了又一有力工具。
Traditional electrochemical techniques have become more and more insufficientfor deeply studying complicated corrosion systems. Various novel electrochemicaltechniques with time/spatial resolutions have aroused a great deal of attention in thepast decades, such as scanning probes microscope (SPM), scanning electrochemicalprobes, electron probe micro-analyzer (EPMA), spectroscopic image, electrochemicalnoise (ECN) and some combined electrochemical techniques.
In this paper, we made our focus on two main components: (1) applicationvarious the state of the art electrochemical techniques with time/spatial resolution,including in-situ optical microscope, in-situ AFM, EPMA, ECN and scanning Kelvinprobe force microscope (SKPFM), in investigations of corrosion of stainless steel indifferent environments; (2) home-establishment of a hybrid system of STM and SRETwhich is able to map both potential distribution in micro scale and atomic or nanotopographies of metals in aqueous solutions, and its applications in corrosion studies.The main results and progresses of this work are outlined as following:
1.The morphological varieties of stainless steel during corrosion processes indifferent media have been in situ observed through an optical microscope with afield depth at least 20 times greater than the traditional optical microscopes. TheDifference Viewer Imaging Technique (DVIT) has been successfully achieved byusing the Photoshop software to deal with optical images which are collected inthe corrosion process. Accordingly, it is found that, there are three corrosion stageswhen the 18-8 stainless steel is immersed in HCl solution, including initiation,development and stable propagation respectively. These stages are wellcharacterized by the different dominant corrosion events. The local breakdown of passive film and metastable pitting nucleus occur during the initial stage. Somemetastable pitting continues and someone repassivate in the development. Finallyin the stage of stable pitting, some active pitting sites keep growth and form macropitting.
2. In-situ AFM has been employed to investigate the initiation corrosion of 18-8stainless steel in HCl solution. It is found that an oxide film dissolves firstly andthen metastable pitting occurs at preferred sites. By using EPMA, the boundarysites of TiN intermetallic particle are recognized the corrosion susceptive sites.From results of SKPFM, it is concluded that a distinct difference of Volta potentialexist between the bulk matrix and the boundary sites of TiN particles in 18-8stainless steel, which is possible to result in micro galvanic corrosion.
3. The ECN technique has been applied to the investigation of corrosion initiation inan early stage of 18-8 SS immersed in different solution, and the electrochemicalcurrent noise data has been analyzed using discrete wavelet transform (DWT).The ECN data have been decomposed according to the DWT to different waveletcoefficients (d_1, d_2,…,d_8) with corresponding time scales, which are associatedwith different electrochemical transient events. For the first time, the origin ofwavelet coefficients is discussed based on the correlation between the evolution ofthe energy distribution plot(EDP)of wavelet coefficients and topographic changesfrom OM, EPMA and AFM.
4. A home-made hybrid instrument of SMET/STM has been successfully establishedin lab, and it has been applied to the studies of localized corrosion of 18-8 SS inFeCl_3 solution. A series scanning probes have also been developed, involving thePt metallic potential probe, Cl~- selective microprobe, pH selective microprobe andintegrated potential/topographic PtIr microprobe. Based on the accuratelycontrollable distance of sample-probe by STM function, the spatial resolution ofSMET on imaging for corrosion potential, Cl~- concentration and pH at interface ofmatel/solution is remarkably improved. The novel instrument has been employed,for the fist time, to detect the potential distribution in vertical range to electrodes, it is found that there is obviously different distribution on pitting site and onnonactive site. It is implied that the hybrid instrument is possible to image theinterfacial potential distribution for the corrosion system. Using the hybridinstrument, the integrated topography-activity images of 18-8 SS in FeCl_3 solutionhave been successfully recorded, which demonstrates that the hybrid instrument ofSMET/STM is able to become a powerful technique for in situ correlation studyon the surface structure and the electrochemical activity.
本文工作主要由两部分内容组成：(1)应用多种现有已商品化的具有时间-空间分辨能力的电化学新技术和方法，包括超高景深共聚焦光学显微镜、原位原子力显微镜、电子探针、电化学噪音技术及扫描Kelvin探针显微镜技术等，对不锈钢局部腐蚀过程进行综合研究，深入探讨不锈钢在不同环境介质中的腐蚀特征及本质机理；(2)侧重发展新的时间-空间分辨的电化学仪器方法，并应用这些仪器方法对相应的实际腐蚀体系进行研究。取得主要研究进展和成果如下：
1．运用超高景深共焦光学显微镜对18-8不锈钢在不同溶液介质中的腐蚀过程进行了原位实时观测。在连续的原位光学显微图像数据采集基础上，运用Photoshop图像处理软件实现了光学示差图像分析，通过图像示差分析，极大地提高了原位光学显微观测腐蚀过程的灵敏度，可捕捉不同腐蚀阶段金属表面形貌结构的细微变化。实验发现，不锈钢在HCl溶液中的腐蚀过程存在诱导期、发展期和稳定期三个不同阶段，诱导期为不锈钢表面钝化膜的局部破裂溶解而导致亚稳态腐蚀点的诱导产生；发展期则表现为大量亚稳态腐蚀点的形成与再钝化；稳定期表现为腐蚀活性点的持续溶解或宏观点腐蚀的形成与稳定生长；
2．运用原位原子力显微镜技术对18-8不锈钢在HCl溶液中腐蚀的早期过程进行研究，发现在腐蚀的早期过程存在明显的表面钝化膜的溶解和亚稳态腐蚀点的形成；对不锈钢表面腐蚀前后进行SEM形貌分析和表面元素分布的电子探针测量，结果表明18-8不锈钢表面TiN颗粒的边界是腐蚀优先发生的位点，小尺寸的TiN颗粒边界更易于生成腐蚀活性点；采用扫描Kelvin探针显微技术，对18-8不锈钢表面形貌与Volta电位分布进行了关联研究，发现TiN颗粒边界位点与金属基底间存在明显的电位差异，由于“微电偶”和“微缝隙”的作用，从而导致在腐蚀性介质中形成腐蚀微电池，诱发局部腐蚀在TiN颗粒边界位点优先发生；
3．研究了18-8不锈钢在不同溶液介质中的电化学噪音，并运用小波分析方法对噪音数据进行解析，通过综合分析电化学噪音小波系数能量分布图的变化趋势，并综合应用光学显微镜、电子探针、原位原子力显微镜的联合研究，首次对电化学噪音数据中各小波系数所对应的腐蚀事件及物理意义进行了指认；
4．进一步建立了扫描微电极／扫描隧道显微镜联用系统，成功实现了两种技术的联用。研制了一系列电化学扫描微探针，包括金属Pt电位探针、Cl~-选择性微探针、pH选择性微探针和电位／形貌复合PtIr合金微探针，这些探针经过相应的性能测试和实验测试，证明可有效地应用于各种腐蚀体系关键性腐蚀参数的实际测量。运用所建立的SMET／STM联用测量仪器，并基于隧道电流的可控制探针尖端与样品表面距离的强大功能，大大提高了金属表面腐蚀过程电位分布、Cl~-浓度分布及pH分布等测量的空间灵敏度和空间分辨度。对表面点腐蚀位点和非腐蚀活性位点进行了纵向电位分布测量，结果表明纵向电位分布图可直接反映表面腐蚀发生发展过程的变化，不锈钢表面腐蚀活性点和非腐蚀活性点的金属／溶液界面电位分布特征存在明显差异，利用仪器的距离-电位曲线测量功能，可对金属／溶液界面双电层结构进行深入研究。成功地获得了18-8不锈钢表面腐蚀过程电位分布图和局部腐蚀点区域的形貌结构，从而实现局部腐蚀的原位构-性研究，为金属／溶液界面电化学研究提供了又一有力工具。
Traditional electrochemical techniques have become more and more insufficientfor deeply studying complicated corrosion systems. Various novel electrochemicaltechniques with time/spatial resolutions have aroused a great deal of attention in thepast decades, such as scanning probes microscope (SPM), scanning electrochemicalprobes, electron probe micro-analyzer (EPMA), spectroscopic image, electrochemicalnoise (ECN) and some combined electrochemical techniques.
In this paper, we made our focus on two main components: (1) applicationvarious the state of the art electrochemical techniques with time/spatial resolution,including in-situ optical microscope, in-situ AFM, EPMA, ECN and scanning Kelvinprobe force microscope (SKPFM), in investigations of corrosion of stainless steel indifferent environments; (2) home-establishment of a hybrid system of STM and SRETwhich is able to map both potential distribution in micro scale and atomic or nanotopographies of metals in aqueous solutions, and its applications in corrosion studies.The main results and progresses of this work are outlined as following:
1.The morphological varieties of stainless steel during corrosion processes indifferent media have been in situ observed through an optical microscope with afield depth at least 20 times greater than the traditional optical microscopes. TheDifference Viewer Imaging Technique (DVIT) has been successfully achieved byusing the Photoshop software to deal with optical images which are collected inthe corrosion process. Accordingly, it is found that, there are three corrosion stageswhen the 18-8 stainless steel is immersed in HCl solution, including initiation,development and stable propagation respectively. These stages are wellcharacterized by the different dominant corrosion events. The local breakdown of passive film and metastable pitting nucleus occur during the initial stage. Somemetastable pitting continues and someone repassivate in the development. Finallyin the stage of stable pitting, some active pitting sites keep growth and form macropitting.
2. In-situ AFM has been employed to investigate the initiation corrosion of 18-8stainless steel in HCl solution. It is found that an oxide film dissolves firstly andthen metastable pitting occurs at preferred sites. By using EPMA, the boundarysites of TiN intermetallic particle are recognized the corrosion susceptive sites.From results of SKPFM, it is concluded that a distinct difference of Volta potentialexist between the bulk matrix and the boundary sites of TiN particles in 18-8stainless steel, which is possible to result in micro galvanic corrosion.
3. The ECN technique has been applied to the investigation of corrosion initiation inan early stage of 18-8 SS immersed in different solution, and the electrochemicalcurrent noise data has been analyzed using discrete wavelet transform (DWT).The ECN data have been decomposed according to the DWT to different waveletcoefficients (d_1, d_2,…,d_8) with corresponding time scales, which are associatedwith different electrochemical transient events. For the first time, the origin ofwavelet coefficients is discussed based on the correlation between the evolution ofthe energy distribution plot(EDP)of wavelet coefficients and topographic changesfrom OM, EPMA and AFM.
4. A home-made hybrid instrument of SMET/STM has been successfully establishedin lab, and it has been applied to the studies of localized corrosion of 18-8 SS inFeCl_3 solution. A series scanning probes have also been developed, involving thePt metallic potential probe, Cl~- selective microprobe, pH selective microprobe andintegrated potential/topographic PtIr microprobe. Based on the accuratelycontrollable distance of sample-probe by STM function, the spatial resolution ofSMET on imaging for corrosion potential, Cl~- concentration and pH at interface ofmatel/solution is remarkably improved. The novel instrument has been employed,for the fist time, to detect the potential distribution in vertical range to electrodes, it is found that there is obviously different distribution on pitting site and onnonactive site. It is implied that the hybrid instrument is possible to image theinterfacial potential distribution for the corrosion system. Using the hybridinstrument, the integrated topography-activity images of 18-8 SS in FeCl_3 solutionhave been successfully recorded, which demonstrates that the hybrid instrument ofSMET/STM is able to become a powerful technique for in situ correlation studyon the surface structure and the electrochemical activity.
引文
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