铜及青铜合金在静态和动态薄液膜下的腐蚀行为研究
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摘要
铜及其合金青铜具有优良的机械性能,导电导热性能和腐蚀防护性能。自古以来就常常被用于大型雕塑、房屋屋顶,古器皿或者艺术品的构建材料。当暴露在湿润的大气或轻微的腐蚀环境时,铜及青铜表面会钝化形成一层保护性的氧化膜。但是当它们暴露在强腐蚀性环境中,特别是含氯的腐蚀环境中,青铜将遭受严重的腐蚀过程,这种腐蚀叫“青铜病”或“青铜癌症”。到目前为止,“青铜病”仍然是文物保护过程中最难以解决的问题,其根本原因在于腐蚀机制的复杂性。金属的大气腐蚀是发生在薄液膜下的电化学过程。在过去,对铜和青铜大气腐蚀机制的研究主要集中在腐蚀产物膜的物理表征,但物理表征得到的并不是直接的电化学信息,导致铜和青铜在含氯大气环境下的腐蚀机制仍然不清楚。本文在改进的薄液膜装置上,成功实现了电化学方法对铜及青铜在静态和动态薄液膜条件下的大气腐蚀行为研究。本文的主要研究工作包括：
1.采用电化学阻抗谱(EIS),阴极极化曲线(Cathodic polarization curve)等电化学手段并结合SEM/EDS和XRD考察了纯铜在不同厚度的含氯静态薄液膜下的腐蚀行为。结果表明在最初的2h内,铜的腐蚀行为受氧的扩散控制,腐蚀速率随着薄液膜的厚度减薄而加速,但是当浸泡时间增加至192h后,由于在300μm以上薄液膜下铜的腐蚀过程受阴极控制,300μm以下腐蚀过程受阳极控制,腐蚀速率的排序变为：300μm>402μm>199μm>本体溶液>101μm。铜在静态含氯薄液膜条件下的腐蚀行为和在本体溶液中的腐蚀行为有很大的差异。在薄液膜条件下,主要发生均匀腐蚀过程,而在本体溶液中为点蚀过程。最初所形成的腐蚀产物主要为Cu2O,且腐蚀产物量随着薄液膜的厚度减薄而增加；长时间浸泡后,表面一层Cu2O在氯离子的作用下转化成了Cu2(OH)3Cl和Cu2(OH)2CO3,形成双层腐蚀结构。内层靠近金属基底为Cu2O,外层为Cu2(OH)3Cl和Cu2(OH)2CO3的混合层
2.应用电化学方法如OCP、EIS和阴极极化技术考察了单相α-青铜在不同厚度的静态含氯薄液膜下的腐蚀行为,发现单相α-青铜和纯铜的电化学腐蚀行为类似,但是并不完全等同,单相α-青铜发生铜的优先溶解和含锡腐蚀产物富聚的过程,主要为局部腐蚀过程,而非均匀腐蚀。采用阳极极化曲线考察了单相α-青铜经过腐蚀后产生的含锡腐蚀产物膜对基底溶解行为影响。实验表明含锡腐蚀产物膜对基底有一定的保护作用。
3.考察了微观相结构和组成对青铜在不同液膜下的初期腐蚀行为的影响。结果表明阴极过程和电化学腐蚀速率和微观相结构有关。在同样厚度的薄液膜条件下,三相青铜76Cu在初期的腐蚀速率比两相青铜86Cu,85Cu的腐蚀速率小,含铅相的两相青铜86Cu的腐蚀速率比同样是两相但不含铅相的85Cu青铜的腐蚀速率小。而在本体溶液中,其腐蚀速率排序为76Cu>86Cu>85Cu。采用扫描开尔文探针显微镜(SKPFM)考察了具有不同微观相结构的青铜表面伏打电位分布,明晰了其腐蚀行为。
4.采用EIS和线性极化考察了Na2SO4和NaCl对青铜大气腐蚀行为的协同效应,并利用XRD、Raman光谱和SEM/EDS对腐蚀产物进行表征。在腐蚀初期,少量Na2SO4的加入能降低青铜在含NaCl的动态薄液膜下的腐蚀速率,表现为逆协同效应。而在中后期,青铜在只含NaCl的动态薄液膜下的腐蚀速率小于其暴露在含Na2SO4和NaCl的动态薄液膜下的腐蚀速率,表现为协同效应。协同效应归因为Na2SO4的加入使Pb相在NaCl的动态薄液膜下发生优先溶解过程,而在只含NaCl的动态薄液膜下Pb腐蚀生成一层具有保护性能的PbCl(OH)钝化膜。
Copper and bronze alloys, due to their good mechanic properties, electronic and heat conductivity, and good anti-corrosion resistance property, have long been used as constructive materials such as sculptures, building roof, household utensils and work of art. Copper and bronze alloys tend to be passivated in humid atmospheres or in light corrosive environments. However, in aggressive environments, especially in chloride containing environments, they suffered severe corrosion, which is called "bronze disease" or "bronze cancer". Up to now, bronze disease is still a challenge for the protection of cultural relic, due to the complication of the corrosion mechanism in chloride containing environment. Atmospheric corrosion can be regarded as wet corrosion of material under the thin electrolyte layer (TEL) formed on the surface of the material. This kind of corrosion is usually considered to be of an electrochemical nature. The past studies dealt with atmospheric corrosion of copper and bronze alloys were focused on the characterization of the patina, which caused much debate for the corrosion mechanisms because the physical characterization is unable to get the direct electrochemical information. In this dissertation, the copper and bronze corrosion behavior under TELs was successfully in-situ monitored via electrochemical methods with the aid of modified equipment. The main contents are listed as follows:
1. The corrosion behavior of pure copper under chloride-containing TEL with various thicknesses was investigated using cathodic polarization and EIS. The results show that at the initial immersion stage (in2h), copper corrosion rate under TEL increases with the thinning of the thickness of TEL because the corrosion is under the control of O2diffusion process during the first2h. As the immersion time increases to192h, the corrosion rate ranks as300μm>402μm>199μm> bulk solution>101μm due to the fact that the corrosion is under the control of cathodic process when the thickness of TEL is larger than300μm, while less than300μm, the corrosion is under the control of anodic process. The morphology study performed by SEM reveals that uniform corrosion is the main corrosion behavior for the copper under chloride-containing TEL. This corrosion behavior was significantly different from that of copper in bulk solution. In the bulk solution, pitting was the main corrosion behavior. At initial immersion time (in2h), the corrosion product on the copper surface was mainly Cu2O, and its amount increases with the decreasing of the covered electrolyte layers. After long time immersion the protective layer Cu2O suffers destruction and transferred into Cu2(OH)3Cl and Cu2(OH)2CO3in the presence of chloride ions. The formed corrosion layer can be defined with a duplex structure, i.e., an inner layer adhere to the substrate corresponding to cuprite (Cu2O) and an outer layer a mixture of atacamite (Cu2(OH)3Cl) and malachite (Cu2(OH)2CO3).
2. The corrosion behavior of single-phase α-bronze under chloride-containing static TEL with various thicknesses was investigated using electrochemical methods including OCP, EIS and cathodic polarization. The results indicate that the corrosion behavior of a-bronze is similar, but not identical to that of copper. The corrosion behavior of a-bronze proceeds through a preferential dissolution of Cu and a concentration of corrosion products containing Sn, further, a localized corrosion process is occurred on its surface. Anodic polarization curve shows that the corrosion products of Sn present protection to the substrate.
3. The effect of microstructure and composition of bronze alloys on the bronze corrosion behavior under TEL was also investigated. The results indicate that the cathodic polarization behavior and corrosion rate are dependent on the phase microstruture. The corrosion rate of76Cu with three phases is higher than that of86Cu and85Cu with two phases at the same thickness of TEL during the initial stage, and the corrosion rate of two-phase86Cu containing Pb is higher than that of two-phase85Cu without Pb. However, in the bulk solution, the corrosion rates rank as76Cu>86Cu>85Cu。 The potential maps of bronze alloys with different phase structures was investigated by SKPFM, and the corrosion behavior was further determined.
4. The synthetic effect of Na2SO4and NaCl on the bronze atmospheric corrosion was investigated during the initial stage and corrosion products were characterized using XRD、Raman spectroscopy and SEM/EDS. The results indicate that the addition of a small amount of Na2SO4into NaCl solution reduces the corrosion rate of bronze under chloride-containing dynamic TEL, representing a inverse synthetic effect during the initial stage, whereas, after long time of exposure, the corrosion rate of bronze under NaCl containing TEL is lower than that of under NaCl and Na2SO4TEL, which is manifested as synthetic effect. The synthetic effect can be ascribed to the preferential dissolution of Pb caused by the NaaSO4, while in the only NaCl-containing dynamic TEL, a passivative film PbCl(OH) is formed on the bronze surface.
1.采用电化学阻抗谱(EIS),阴极极化曲线(Cathodic polarization curve)等电化学手段并结合SEM/EDS和XRD考察了纯铜在不同厚度的含氯静态薄液膜下的腐蚀行为。结果表明在最初的2h内,铜的腐蚀行为受氧的扩散控制,腐蚀速率随着薄液膜的厚度减薄而加速,但是当浸泡时间增加至192h后,由于在300μm以上薄液膜下铜的腐蚀过程受阴极控制,300μm以下腐蚀过程受阳极控制,腐蚀速率的排序变为：300μm>402μm>199μm>本体溶液>101μm。铜在静态含氯薄液膜条件下的腐蚀行为和在本体溶液中的腐蚀行为有很大的差异。在薄液膜条件下,主要发生均匀腐蚀过程,而在本体溶液中为点蚀过程。最初所形成的腐蚀产物主要为Cu2O,且腐蚀产物量随着薄液膜的厚度减薄而增加；长时间浸泡后,表面一层Cu2O在氯离子的作用下转化成了Cu2(OH)3Cl和Cu2(OH)2CO3,形成双层腐蚀结构。内层靠近金属基底为Cu2O,外层为Cu2(OH)3Cl和Cu2(OH)2CO3的混合层
2.应用电化学方法如OCP、EIS和阴极极化技术考察了单相α-青铜在不同厚度的静态含氯薄液膜下的腐蚀行为,发现单相α-青铜和纯铜的电化学腐蚀行为类似,但是并不完全等同,单相α-青铜发生铜的优先溶解和含锡腐蚀产物富聚的过程,主要为局部腐蚀过程,而非均匀腐蚀。采用阳极极化曲线考察了单相α-青铜经过腐蚀后产生的含锡腐蚀产物膜对基底溶解行为影响。实验表明含锡腐蚀产物膜对基底有一定的保护作用。
3.考察了微观相结构和组成对青铜在不同液膜下的初期腐蚀行为的影响。结果表明阴极过程和电化学腐蚀速率和微观相结构有关。在同样厚度的薄液膜条件下,三相青铜76Cu在初期的腐蚀速率比两相青铜86Cu,85Cu的腐蚀速率小,含铅相的两相青铜86Cu的腐蚀速率比同样是两相但不含铅相的85Cu青铜的腐蚀速率小。而在本体溶液中,其腐蚀速率排序为76Cu>86Cu>85Cu。采用扫描开尔文探针显微镜(SKPFM)考察了具有不同微观相结构的青铜表面伏打电位分布,明晰了其腐蚀行为。
4.采用EIS和线性极化考察了Na2SO4和NaCl对青铜大气腐蚀行为的协同效应,并利用XRD、Raman光谱和SEM/EDS对腐蚀产物进行表征。在腐蚀初期,少量Na2SO4的加入能降低青铜在含NaCl的动态薄液膜下的腐蚀速率,表现为逆协同效应。而在中后期,青铜在只含NaCl的动态薄液膜下的腐蚀速率小于其暴露在含Na2SO4和NaCl的动态薄液膜下的腐蚀速率,表现为协同效应。协同效应归因为Na2SO4的加入使Pb相在NaCl的动态薄液膜下发生优先溶解过程,而在只含NaCl的动态薄液膜下Pb腐蚀生成一层具有保护性能的PbCl(OH)钝化膜。
Copper and bronze alloys, due to their good mechanic properties, electronic and heat conductivity, and good anti-corrosion resistance property, have long been used as constructive materials such as sculptures, building roof, household utensils and work of art. Copper and bronze alloys tend to be passivated in humid atmospheres or in light corrosive environments. However, in aggressive environments, especially in chloride containing environments, they suffered severe corrosion, which is called "bronze disease" or "bronze cancer". Up to now, bronze disease is still a challenge for the protection of cultural relic, due to the complication of the corrosion mechanism in chloride containing environment. Atmospheric corrosion can be regarded as wet corrosion of material under the thin electrolyte layer (TEL) formed on the surface of the material. This kind of corrosion is usually considered to be of an electrochemical nature. The past studies dealt with atmospheric corrosion of copper and bronze alloys were focused on the characterization of the patina, which caused much debate for the corrosion mechanisms because the physical characterization is unable to get the direct electrochemical information. In this dissertation, the copper and bronze corrosion behavior under TELs was successfully in-situ monitored via electrochemical methods with the aid of modified equipment. The main contents are listed as follows:
1. The corrosion behavior of pure copper under chloride-containing TEL with various thicknesses was investigated using cathodic polarization and EIS. The results show that at the initial immersion stage (in2h), copper corrosion rate under TEL increases with the thinning of the thickness of TEL because the corrosion is under the control of O2diffusion process during the first2h. As the immersion time increases to192h, the corrosion rate ranks as300μm>402μm>199μm> bulk solution>101μm due to the fact that the corrosion is under the control of cathodic process when the thickness of TEL is larger than300μm, while less than300μm, the corrosion is under the control of anodic process. The morphology study performed by SEM reveals that uniform corrosion is the main corrosion behavior for the copper under chloride-containing TEL. This corrosion behavior was significantly different from that of copper in bulk solution. In the bulk solution, pitting was the main corrosion behavior. At initial immersion time (in2h), the corrosion product on the copper surface was mainly Cu2O, and its amount increases with the decreasing of the covered electrolyte layers. After long time immersion the protective layer Cu2O suffers destruction and transferred into Cu2(OH)3Cl and Cu2(OH)2CO3in the presence of chloride ions. The formed corrosion layer can be defined with a duplex structure, i.e., an inner layer adhere to the substrate corresponding to cuprite (Cu2O) and an outer layer a mixture of atacamite (Cu2(OH)3Cl) and malachite (Cu2(OH)2CO3).
2. The corrosion behavior of single-phase α-bronze under chloride-containing static TEL with various thicknesses was investigated using electrochemical methods including OCP, EIS and cathodic polarization. The results indicate that the corrosion behavior of a-bronze is similar, but not identical to that of copper. The corrosion behavior of a-bronze proceeds through a preferential dissolution of Cu and a concentration of corrosion products containing Sn, further, a localized corrosion process is occurred on its surface. Anodic polarization curve shows that the corrosion products of Sn present protection to the substrate.
3. The effect of microstructure and composition of bronze alloys on the bronze corrosion behavior under TEL was also investigated. The results indicate that the cathodic polarization behavior and corrosion rate are dependent on the phase microstruture. The corrosion rate of76Cu with three phases is higher than that of86Cu and85Cu with two phases at the same thickness of TEL during the initial stage, and the corrosion rate of two-phase86Cu containing Pb is higher than that of two-phase85Cu without Pb. However, in the bulk solution, the corrosion rates rank as76Cu>86Cu>85Cu。 The potential maps of bronze alloys with different phase structures was investigated by SKPFM, and the corrosion behavior was further determined.
4. The synthetic effect of Na2SO4and NaCl on the bronze atmospheric corrosion was investigated during the initial stage and corrosion products were characterized using XRD、Raman spectroscopy and SEM/EDS. The results indicate that the addition of a small amount of Na2SO4into NaCl solution reduces the corrosion rate of bronze under chloride-containing dynamic TEL, representing a inverse synthetic effect during the initial stage, whereas, after long time of exposure, the corrosion rate of bronze under NaCl containing TEL is lower than that of under NaCl and Na2SO4TEL, which is manifested as synthetic effect. The synthetic effect can be ascribed to the preferential dissolution of Pb caused by the NaaSO4, while in the only NaCl-containing dynamic TEL, a passivative film PbCl(OH) is formed on the bronze surface.
引文
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