金属包装材料的腐蚀失效过程和腐蚀检测
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摘要
金属包装材料其缺点之一就是容易发生腐蚀，其腐蚀机制尚未探明，而金属包装实罐产品的腐蚀检测也存在困难。本文针对金属包装材料镀锡薄钢板在功能饮料和氯化钠溶液中的腐蚀实效过程与机制以及金属包装实罐的腐蚀检测而开展的。
采用电化学阻抗谱技术，结合扫描电镜（SEM）、能量散射X射线谱（EDS）、X射线光电子能谱（XPS）、扫描探针显微镜（SPM）等表面分析技术，研究了镀锡薄钢板平板试样在功能饮料和氯化钠溶液中的腐蚀行为并探讨了腐蚀机制。结果表明，两者腐蚀机制完全不同。在功能饮料中主要是有机酸对镀锡薄钢板的腐蚀，镀锡薄钢板在功能饮料中浸泡24天后其表面的腐蚀产物膜由外层的富锡层和内层的富铁层组成，XPS结果表明其成分主要是Sn(II)/Sn(IV)与柠檬酸阴离子及Fe(III)与柠檬酸阴离子组成的化合物；而在氯化钠溶液中主要是对镀锡层缺陷处暴露的基底金属碳钢的腐蚀，其腐蚀产物主要是γ-FeOOH。
根据涂覆镀锡薄钢板在氯化钠溶液和功能饮料中的EIS特征和EN特征，利用低频阻抗模值和噪声电阻值评价了涂覆镀锡薄钢板的耐蚀性能，并探讨了涂覆镀锡薄钢板在氯化钠溶液和功能饮料中的腐蚀机制。结果表明，其腐蚀过程主要分为涂层的润湿和涂层下金属的腐蚀两个阶段，而润湿过程通常只有几天。
发展了快速评价涂层失效程度的方法，提出了利用电化学阻抗谱（EIS）中Bode图中频区（1—100Hz）阻抗模值的变化率为切入点，提取特征参数p作为表征涂层失效程度的参数。实验结果表明该方法可以用来快速评价有机涂层的失效程度而无需建立等效电路模型。
研制了适用于饮料金属包装实罐腐蚀检测的电化学传感器，并对不同实罐进行了EIS和电化学噪声（EN）检测。采用电感耦合离子质谱仪（ICP-MS）技术检测实罐容器中的金属离子含量，结果表明随着服役期的延长，饮料实罐中的金属离子Fe和Sn的含量增加，而EIS和EN结果表明随着服役期的延长，涂层电阻、电荷转移电阻、噪声电阻则不断减小，表明腐蚀引发了离子的溢出，ICP-MS结果与电化学参数具有直接的关联性。研究结果表明，研制的传感器可以用于实罐耐蚀性能检测，并为评估金属包装产品的货架寿命提供科学依据。
将混沌分析引入了电化学噪声的数据分析之中，并针对304不锈钢、316L不锈钢、涂覆镀锡薄钢板腐蚀过程的电化学电位噪声进行了初步分析。结果表明：利用电位噪声的关联维数可以判断腐蚀类型，局部腐蚀对应的关联维数较大而钝化过程对应的关联维数较小。
One disadvantage of metal packaging materials is that it is more likely to becorroded, but its corrosion mechanism and corrosion detection of metal cans stilltroubled the researchers. This paper focus on the deterioration process and corrosionmechanism of tinplate in functional drink and NaCl solution, the corroson detection ofbeverage cans.
The corrosion process of a tinplate in functional beverage and NaCl solution wasinvestigated using electrochemical impedance spectroscope (EIS), scanning electronmicroscopy (SEM), energy dispersive X-ray spectroscopy (EDS), scanning probemicroscopy (SPM), and X-ray photoelectron spectroscopy (XPS), and a corrosionmechanism is proposed. The results show that the corrosion mechanism under twoconditons are different. We propose that the tinplate is mainly corroded by the organicacids that exist in functional beverages. X-ray photoelectron spectroscopy (XPS)results show that the corrosion product is mainly composed of a Sn(II)/Sn(IV) citratecomplex or an Fe(III) citrate complex. Furthermore, the corrosion product film is firstenriched with Sn and then enriched with Fe after immersion in functional beverage for24d. The corrosion of tinplate in0.5mol/L NaCl solution was mainly the dissolutionof carbon steel substrate because of the defects in the tin layer and the corrosionproduct was mainly γ-FeOOH.
The anti-corrosion performance of lacquered-tinplate were evaluated usingimpedance modulus at low frequency and noise resistance, obtained from EIS and ENdata, respectively. Furthermore, the corrosion mechanism of lacquered-tinplate inenergy drink and NaCl solution was discussed. The results showed that the corrosionprocess could be divided into2stages: wetting of the organic coating and thecorrosion of the tinplate beneath the coating, and the wetting process was only acouple of days.
The degradation coefficient is proposed to evaluate the degradation degree oforganic coatings by directly analyzing the Bode plots of the electrochemicalimpedance spectroscopy (EIS) data (1—100Hz). We investigated the degradation ofphenolic epoxy coating/tinplate system by EIS and the degradation coefficient value,which correlates well with the results of breakpoint frequency and variation of phase angle at10Hz. It is concluded that degradation coefficient can be used for the fastevaluation of degradation degree of organic coatings without constructingelectrochemical equivalent circuits in practical applications.
An electrochemical sensor was designed to detect the corrosion degree of metalcans for beverage packaging, and the effective testing area of the sensor wasdetermined. Electrochemical impedance spectroscopy (EIS) and electrochemical noise(EN) were performed to detect the corrosion degree of beverage cans. ICP-MS resultsshowed that tin and iron release increased with storage time while EIS and EN resultsshowed that coating resistance, charge transfer resistance and noise resistancedecreased with the increase in storage time, thus indicating that the corrosion beneaththe organic coating induced a metal release. A clear and direct relationship wasobtained between ICP-MS and electrochemical data. The designed electrochemicalsensor was successfully applied to detect the performance of beverage cans andfurther provided scientific proof to evaluate the shelf life of metal cans for packaging.
Chaos theory and the use of phase space reconstruction produce a novelmethodology to study electrochemical noise (EN) signals, obtaining novelinformation to distinguish corrosion types. To evaluate the chaotic nature ofelectrochemical noise, phase space is reconstructed and the embedding parameter isobtained by the mutual information and Cao's methods. Subsequently, the correlationdimension is calculated. From the correlation dimension, we can conclude that localcorrosion shows a higher correlation dimension while passivation shows a lowercorrelation dimension.
采用电化学阻抗谱技术，结合扫描电镜（SEM）、能量散射X射线谱（EDS）、X射线光电子能谱（XPS）、扫描探针显微镜（SPM）等表面分析技术，研究了镀锡薄钢板平板试样在功能饮料和氯化钠溶液中的腐蚀行为并探讨了腐蚀机制。结果表明，两者腐蚀机制完全不同。在功能饮料中主要是有机酸对镀锡薄钢板的腐蚀，镀锡薄钢板在功能饮料中浸泡24天后其表面的腐蚀产物膜由外层的富锡层和内层的富铁层组成，XPS结果表明其成分主要是Sn(II)/Sn(IV)与柠檬酸阴离子及Fe(III)与柠檬酸阴离子组成的化合物；而在氯化钠溶液中主要是对镀锡层缺陷处暴露的基底金属碳钢的腐蚀，其腐蚀产物主要是γ-FeOOH。
根据涂覆镀锡薄钢板在氯化钠溶液和功能饮料中的EIS特征和EN特征，利用低频阻抗模值和噪声电阻值评价了涂覆镀锡薄钢板的耐蚀性能，并探讨了涂覆镀锡薄钢板在氯化钠溶液和功能饮料中的腐蚀机制。结果表明，其腐蚀过程主要分为涂层的润湿和涂层下金属的腐蚀两个阶段，而润湿过程通常只有几天。
发展了快速评价涂层失效程度的方法，提出了利用电化学阻抗谱（EIS）中Bode图中频区（1—100Hz）阻抗模值的变化率为切入点，提取特征参数p作为表征涂层失效程度的参数。实验结果表明该方法可以用来快速评价有机涂层的失效程度而无需建立等效电路模型。
研制了适用于饮料金属包装实罐腐蚀检测的电化学传感器，并对不同实罐进行了EIS和电化学噪声（EN）检测。采用电感耦合离子质谱仪（ICP-MS）技术检测实罐容器中的金属离子含量，结果表明随着服役期的延长，饮料实罐中的金属离子Fe和Sn的含量增加，而EIS和EN结果表明随着服役期的延长，涂层电阻、电荷转移电阻、噪声电阻则不断减小，表明腐蚀引发了离子的溢出，ICP-MS结果与电化学参数具有直接的关联性。研究结果表明，研制的传感器可以用于实罐耐蚀性能检测，并为评估金属包装产品的货架寿命提供科学依据。
将混沌分析引入了电化学噪声的数据分析之中，并针对304不锈钢、316L不锈钢、涂覆镀锡薄钢板腐蚀过程的电化学电位噪声进行了初步分析。结果表明：利用电位噪声的关联维数可以判断腐蚀类型，局部腐蚀对应的关联维数较大而钝化过程对应的关联维数较小。
One disadvantage of metal packaging materials is that it is more likely to becorroded, but its corrosion mechanism and corrosion detection of metal cans stilltroubled the researchers. This paper focus on the deterioration process and corrosionmechanism of tinplate in functional drink and NaCl solution, the corroson detection ofbeverage cans.
The corrosion process of a tinplate in functional beverage and NaCl solution wasinvestigated using electrochemical impedance spectroscope (EIS), scanning electronmicroscopy (SEM), energy dispersive X-ray spectroscopy (EDS), scanning probemicroscopy (SPM), and X-ray photoelectron spectroscopy (XPS), and a corrosionmechanism is proposed. The results show that the corrosion mechanism under twoconditons are different. We propose that the tinplate is mainly corroded by the organicacids that exist in functional beverages. X-ray photoelectron spectroscopy (XPS)results show that the corrosion product is mainly composed of a Sn(II)/Sn(IV) citratecomplex or an Fe(III) citrate complex. Furthermore, the corrosion product film is firstenriched with Sn and then enriched with Fe after immersion in functional beverage for24d. The corrosion of tinplate in0.5mol/L NaCl solution was mainly the dissolutionof carbon steel substrate because of the defects in the tin layer and the corrosionproduct was mainly γ-FeOOH.
The anti-corrosion performance of lacquered-tinplate were evaluated usingimpedance modulus at low frequency and noise resistance, obtained from EIS and ENdata, respectively. Furthermore, the corrosion mechanism of lacquered-tinplate inenergy drink and NaCl solution was discussed. The results showed that the corrosionprocess could be divided into2stages: wetting of the organic coating and thecorrosion of the tinplate beneath the coating, and the wetting process was only acouple of days.
The degradation coefficient is proposed to evaluate the degradation degree oforganic coatings by directly analyzing the Bode plots of the electrochemicalimpedance spectroscopy (EIS) data (1—100Hz). We investigated the degradation ofphenolic epoxy coating/tinplate system by EIS and the degradation coefficient value,which correlates well with the results of breakpoint frequency and variation of phase angle at10Hz. It is concluded that degradation coefficient can be used for the fastevaluation of degradation degree of organic coatings without constructingelectrochemical equivalent circuits in practical applications.
An electrochemical sensor was designed to detect the corrosion degree of metalcans for beverage packaging, and the effective testing area of the sensor wasdetermined. Electrochemical impedance spectroscopy (EIS) and electrochemical noise(EN) were performed to detect the corrosion degree of beverage cans. ICP-MS resultsshowed that tin and iron release increased with storage time while EIS and EN resultsshowed that coating resistance, charge transfer resistance and noise resistancedecreased with the increase in storage time, thus indicating that the corrosion beneaththe organic coating induced a metal release. A clear and direct relationship wasobtained between ICP-MS and electrochemical data. The designed electrochemicalsensor was successfully applied to detect the performance of beverage cans andfurther provided scientific proof to evaluate the shelf life of metal cans for packaging.
Chaos theory and the use of phase space reconstruction produce a novelmethodology to study electrochemical noise (EN) signals, obtaining novelinformation to distinguish corrosion types. To evaluate the chaotic nature ofelectrochemical noise, phase space is reconstructed and the embedding parameter isobtained by the mutual information and Cao's methods. Subsequently, the correlationdimension is calculated. From the correlation dimension, we can conclude that localcorrosion shows a higher correlation dimension while passivation shows a lowercorrelation dimension.
引文
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