316L不锈钢表面电镀钯合金膜层工艺及其在非氧化性介质中耐蚀行为研究
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摘要
不锈钢表面的钝化膜使得不锈钢在很多介质中有着良好的耐蚀性，但是在非氧化性介质，比如高温稀硫酸、高温醋酸中，不锈钢表面的钝化膜会发生溶解，且无法再自修复，使得不锈钢发生腐蚀。对于不锈钢在醋酸中的腐蚀行为，前人进行了大量的研究，但是对于不锈钢在PTA（对苯二甲酸）浆料中的腐蚀行为尚不明确。对不锈钢表面电沉积钯或者钯合金膜层能够提高不锈钢在非氧化性介质中的耐蚀性，但是，如何进一步提高钯膜合金膜层在高温醋酸中的耐蚀性，以及钯合金膜层在高温醋酸、高温稀硫酸中的耐蚀机制前人研究较少。
本文基于316L不锈钢在高温含溴离子醋酸中的腐蚀行为规律，模拟了PTA浆料（PTA粉末+含溴离子醋酸）干燥过程中浆料湿度对不锈钢腐蚀行为的影响，研究发现，加热不锈钢能够降低界面湿度，显著减小腐蚀速率。在温度恒定的条件下，不锈钢在PTA浆料中的腐蚀速率随湿度的变化呈抛物线变化，在PTA浆料的固液比为25：4时，不锈钢的腐蚀速率最大，在过湿或者过干的PTA浆料中的腐蚀速率均较小。
为了进一步提高钯合金膜层在醋酸中耐蚀性，本文采用了在钯膜层中添加Cu、Ni、Mo合金元素，对纯Pd膜层进行热处理，在不锈钢表面制备Pd-Ni/Pd-Cu复合膜层三种改进方法，并研究了以上三种工艺制备的膜层在还原性介质中的耐蚀性。
通过电沉积的方法能够在304L不锈钢表面沉积一层钯铜镍钼合金膜层，膜层均匀致密，结合力良好，硬度较高。钯铜镍钼膜层性能与沉积电流密切相关，沉积电流密度越小，膜层越平整致密，硬度越高，耐蚀性能也越好。当沉积电流密度为1.2A/dm~2时，膜层在含溴离子沸腾醋酸中的腐蚀速率为0.61g·m~(-2)·h~(-1)，而当沉积电流密度降低至0.8A/dm~2时，膜层在含溴离子醋酸中的腐蚀速率降低至0.05g·m~(-2)·h~(-1)。铜含量对膜层的耐蚀性能有较大的影响，当膜层中铜含量为5.03wt%时，膜层耐蚀性达到最佳，为0.02g·m~(-2)·h~(-1)。
对不锈钢表面镀钯试样进行热处理，可以除去钯膜层中的氢，使膜层的电化学性能可以得到较大程度的恢复，提高了膜层的自腐蚀电位，从而增强膜层耐蚀性。200℃/4h、400℃/4h的热处理条件对膜层元素百分含量以及晶格结构没有明显影响，200℃/4h热处理镀钯膜层中的钯是金属态，400℃/4h热处理镀钯膜层中的钯是氧化态。热处理后，镀钯试样表面的显微硬度明显提高。
通过电沉积能够在316L不锈钢表面制备约3μm的Pd-Ni/Pd-Cu复合膜层。与单层Pd-Cu膜层相比较，该膜层具有更高的硬度，弹性模量和附着力。膜层的孔隙率也明显降低。Pd-Ni/Pd-Cu复合膜层较低的孔隙率可以阻止氯离子渗透膜层到达不锈钢基体。同时复合膜层高硬度、高弹性模量以及更好的附着力的特点，可以提高膜层的耐冲蚀能力，以上因素使得Pd-Ni/Pd-Cu复合膜层能够明显地提高316L不锈钢的耐蚀性能。特别是在既有冲刷腐蚀又有氯离子的复杂环境中，复合膜层表现出了优异的耐蚀性能。在搅拌速率为900r/min并含有0.005mol/LCl~-的沸腾甲乙混合酸中，表面镀有Pd-Ni/Pd-Cu复合膜层的不锈钢试样的腐蚀速率比表面镀有单层Pd-Cu膜层不锈钢试样小了一个数量级。
在80℃0.5mol L-1H_2SO_4+2ppm F-溶液中，在316L不锈钢表面电镀钯能够促进不锈钢基体自发钝化。当316L不锈钢与钯连接之后，在试样表面形成了一层钝化膜，比不锈钢本身的空气氧化膜相比，钝化膜的耐蚀性能明显提高。这可能是因为钝化膜中含有更多的Cr，更高含量的Cr(OH)_3与Fe_3O_4，并且钝化膜有着更小的点缺陷浓度。
最后，本文研究了在316L不锈钢表面沉积Pd，Cr-Pd膜层在PEM燃料电池双极板上的应用。与316L不锈钢相比，电镀钯或者Cr-Pd试样的腐蚀速率降低了三个数量级；电镀钯或者Cr-Pd试样的表面接触电阻同样也显著降低。
Due to the passive film on the surface of stainless steel, stainlesssteel have excellent corrosion resistance in lots of corrosive mediums.However, in reductive corrosion mediums such as boiling dilute sulfuricacid solutions or boiling acetic and formic acids, passive film can notremain stable and active corrosion may happen. The corrosion behaviourof stainless steel in acetic acid with or without halide ions has beenstudied by many authors. However, few researches were focused on thecorrosion behaviour of stainless steel in purified terephthalic acid (PTA)slurry which is important to industrial production. Different techniqueswere reported for palladium deposition on316L stainless steel, and Pdand Pd alloy films show good corrosion resistant in boiling dilute sulfuricacid solutions or boiling acetic and formic acids. However, to improve thecorrosion resistance of the film, and understand the mechanism of theanti-corrosion rensistance in reductive corrosion mediums, it is necessaryto carry on further reaserch on Pd alloy film deposition technology andcorrosion behavior of Pd alloy film.
In this research, the corrosion behaviour of316L stainless steel insimulated drying process of PTA slurry was studied. Pd film, Cr-Pd film,PdCuNiMo film and Pd-Ni/Pd-Cu double coating were deposited onstainless steel, and corrosion behavior of the films were investigated. Themechanism of anti-corrosion resistance for Pd film in0.5mol L-1H_2SO_4+2ppm F-solution at80℃was studied.
The corrosion behaviour of316L stainless steel in acetic-10%formicacid mixture containing Br-and in simulated PTA slurry was investigated,to understand the corrosion mechanism of316L stainless steel in dryingprocess of PTA slurry. The results show that in acetic-10%formic acidmixture containing Br-, corrosion rate of316L stainless steel increaseswith the increase of Br-concentration and temperature. In PTA slurry, thecorrosion rate of316L stainless steel changes in a parabolic form withincrease of the solid to liquid ratio of the slurry. The slurry has thestrongest corrosivity when the solid to liquid ratio of the slurry reachesabout6.25. In a half dry-half wet PTA slurry, when the316L steel surfaceis remained at a suitable temperature to avoid continuous liquid film onthe surface, corrosion rate of the steel will be greatly reduced.
PdCuNiMo alloy film can be deposited on304L stainless steel byelectroplating. The property of film closely related to deposition current.With smaller deposition current, the film is more smooth and dense, andthe hardness of film is higher. So correspondingly, the property of corrosion resistance is better. As the deposite current density decreases, Inboling acetic and formic acids containing200ppm Br-, the corrosion rateof the films prepared with1.2A/dm~2current density is0.61g·m~(-2)·h~(-1). Butthe corrosion rate of film drops to0.05g·m~(-2)·h~(-1)once the current densityreduce to0.8A/dm~2. The influence of Cu content was also investigated.When the content of CuSO_4is1.5g/L, the film prepared with0.8A/dm~2current density has the best corrosion resintance, and the corrosion rate isonly0.02g·m~(-2)·h~(-1).
The codeposition hydrogen in the film can be removed by heattreatment, hence the electrochemical performance can be greatlyrecovered, which leads to higher corrosion potential and better corrosionresistance. After heat treatment, the micro-hardness is obviouslyimproved, in addition, the lattice structure and element content remain thesame. XPS analysis indicated that Pd is metallic state after200℃treatment, However, after treating at400℃，oxidation reaction happenedto Pd.
A Pd-Ni/Pd-Cu double coating with a thickness of about3μm wasdeposited on stainless steel surface by electroplating. The double coatingshows obviously higher hardness, modulus of elasticity and adhesivestrength to the substrate in contrast to single Pd-Cu coating. The porosityof the deposited coating also decreased evidently. The lower porosity ofthe double coating may reduce chloride migration through the deposited film. The higher hardness, modulus and adhesive strength would increasethe erosion resistance. All these factors result in better corrosionresistance. The Pd-Ni/Pd-Cu double coating significantly improved thecorrosion resistance of316L stainless steel in strong corrosive medium.Particularly, the double coating exhibits better resistance in complicatedcorrosive environment including erosion and chloride ions. In boilingacetic and formic acids mixture containing0.005mol/L Cl~-with900r/min stir, the corrosion rate of the double coating coated316L stainlesssteel is about one order of magnitude lower than that of Pd-Cu coatedsamples.
A thin layer of Pd deposition on the surface significantly improves thecorrosion resistance of316L stainless steel in0.5mol L-1H_2SO_4+2ppmF-solution at80℃. The Pd film promotes spontaneous passivition andthe corrosion rate of the Pd plated specimen decreases by three orders ofmagnitude in contrast to that of the original316L specimens. When316Lstainless steel specimen is coupled with Pd electrode, the passive filmformed on stainless steel shows much better corrosion resistance than theair-formed passive film. After the disconnection of the stainless/Pd couple,the stainless steel specimen still remains passivated for a relatively longtime. The Mott-Schottky measurements show that compared with theair-formed passive films, there are less point defects in the passive filmon the specimens coupled with Pd. XPS measurements show that the main difference between the compositions of the two films is theenrichment of Cr and the presence of Cr(OH)_3and Fe_3O_4in the passivefilms coupled with palladium. These differences lead to the bettercorrosion resistance of the passive film formed under the effect ofpalladium film.
Last but important, As a potential material for bipolar plates in protonexchange membrane (PEM) fuel cells, Pd and Cr-Pd film was depositedon316L stainless steel. Corrosion resistance and interface contactresistance were studued. Comared with original316L stainless steel, thecorrosion rate of specimen with Pd or Cr-Pd film decrease by three ordersof magnitude, and the interface contact resistance is also obviouslydecreased. Adding Cr in Pd film can further improve the corrosionresistance for Cr(OH)_3exsits in Cr-Pd film as a beneficial component. Inaddition, adding Cr can lower the cost of the films.
本文基于316L不锈钢在高温含溴离子醋酸中的腐蚀行为规律，模拟了PTA浆料（PTA粉末+含溴离子醋酸）干燥过程中浆料湿度对不锈钢腐蚀行为的影响，研究发现，加热不锈钢能够降低界面湿度，显著减小腐蚀速率。在温度恒定的条件下，不锈钢在PTA浆料中的腐蚀速率随湿度的变化呈抛物线变化，在PTA浆料的固液比为25：4时，不锈钢的腐蚀速率最大，在过湿或者过干的PTA浆料中的腐蚀速率均较小。
为了进一步提高钯合金膜层在醋酸中耐蚀性，本文采用了在钯膜层中添加Cu、Ni、Mo合金元素，对纯Pd膜层进行热处理，在不锈钢表面制备Pd-Ni/Pd-Cu复合膜层三种改进方法，并研究了以上三种工艺制备的膜层在还原性介质中的耐蚀性。
通过电沉积的方法能够在304L不锈钢表面沉积一层钯铜镍钼合金膜层，膜层均匀致密，结合力良好，硬度较高。钯铜镍钼膜层性能与沉积电流密切相关，沉积电流密度越小，膜层越平整致密，硬度越高，耐蚀性能也越好。当沉积电流密度为1.2A/dm~2时，膜层在含溴离子沸腾醋酸中的腐蚀速率为0.61g·m~(-2)·h~(-1)，而当沉积电流密度降低至0.8A/dm~2时，膜层在含溴离子醋酸中的腐蚀速率降低至0.05g·m~(-2)·h~(-1)。铜含量对膜层的耐蚀性能有较大的影响，当膜层中铜含量为5.03wt%时，膜层耐蚀性达到最佳，为0.02g·m~(-2)·h~(-1)。
对不锈钢表面镀钯试样进行热处理，可以除去钯膜层中的氢，使膜层的电化学性能可以得到较大程度的恢复，提高了膜层的自腐蚀电位，从而增强膜层耐蚀性。200℃/4h、400℃/4h的热处理条件对膜层元素百分含量以及晶格结构没有明显影响，200℃/4h热处理镀钯膜层中的钯是金属态，400℃/4h热处理镀钯膜层中的钯是氧化态。热处理后，镀钯试样表面的显微硬度明显提高。
通过电沉积能够在316L不锈钢表面制备约3μm的Pd-Ni/Pd-Cu复合膜层。与单层Pd-Cu膜层相比较，该膜层具有更高的硬度，弹性模量和附着力。膜层的孔隙率也明显降低。Pd-Ni/Pd-Cu复合膜层较低的孔隙率可以阻止氯离子渗透膜层到达不锈钢基体。同时复合膜层高硬度、高弹性模量以及更好的附着力的特点，可以提高膜层的耐冲蚀能力，以上因素使得Pd-Ni/Pd-Cu复合膜层能够明显地提高316L不锈钢的耐蚀性能。特别是在既有冲刷腐蚀又有氯离子的复杂环境中，复合膜层表现出了优异的耐蚀性能。在搅拌速率为900r/min并含有0.005mol/LCl~-的沸腾甲乙混合酸中，表面镀有Pd-Ni/Pd-Cu复合膜层的不锈钢试样的腐蚀速率比表面镀有单层Pd-Cu膜层不锈钢试样小了一个数量级。
在80℃0.5mol L-1H_2SO_4+2ppm F-溶液中，在316L不锈钢表面电镀钯能够促进不锈钢基体自发钝化。当316L不锈钢与钯连接之后，在试样表面形成了一层钝化膜，比不锈钢本身的空气氧化膜相比，钝化膜的耐蚀性能明显提高。这可能是因为钝化膜中含有更多的Cr，更高含量的Cr(OH)_3与Fe_3O_4，并且钝化膜有着更小的点缺陷浓度。
最后，本文研究了在316L不锈钢表面沉积Pd，Cr-Pd膜层在PEM燃料电池双极板上的应用。与316L不锈钢相比，电镀钯或者Cr-Pd试样的腐蚀速率降低了三个数量级；电镀钯或者Cr-Pd试样的表面接触电阻同样也显著降低。
Due to the passive film on the surface of stainless steel, stainlesssteel have excellent corrosion resistance in lots of corrosive mediums.However, in reductive corrosion mediums such as boiling dilute sulfuricacid solutions or boiling acetic and formic acids, passive film can notremain stable and active corrosion may happen. The corrosion behaviourof stainless steel in acetic acid with or without halide ions has beenstudied by many authors. However, few researches were focused on thecorrosion behaviour of stainless steel in purified terephthalic acid (PTA)slurry which is important to industrial production. Different techniqueswere reported for palladium deposition on316L stainless steel, and Pdand Pd alloy films show good corrosion resistant in boiling dilute sulfuricacid solutions or boiling acetic and formic acids. However, to improve thecorrosion resistance of the film, and understand the mechanism of theanti-corrosion rensistance in reductive corrosion mediums, it is necessaryto carry on further reaserch on Pd alloy film deposition technology andcorrosion behavior of Pd alloy film.
In this research, the corrosion behaviour of316L stainless steel insimulated drying process of PTA slurry was studied. Pd film, Cr-Pd film,PdCuNiMo film and Pd-Ni/Pd-Cu double coating were deposited onstainless steel, and corrosion behavior of the films were investigated. Themechanism of anti-corrosion resistance for Pd film in0.5mol L-1H_2SO_4+2ppm F-solution at80℃was studied.
The corrosion behaviour of316L stainless steel in acetic-10%formicacid mixture containing Br-and in simulated PTA slurry was investigated,to understand the corrosion mechanism of316L stainless steel in dryingprocess of PTA slurry. The results show that in acetic-10%formic acidmixture containing Br-, corrosion rate of316L stainless steel increaseswith the increase of Br-concentration and temperature. In PTA slurry, thecorrosion rate of316L stainless steel changes in a parabolic form withincrease of the solid to liquid ratio of the slurry. The slurry has thestrongest corrosivity when the solid to liquid ratio of the slurry reachesabout6.25. In a half dry-half wet PTA slurry, when the316L steel surfaceis remained at a suitable temperature to avoid continuous liquid film onthe surface, corrosion rate of the steel will be greatly reduced.
PdCuNiMo alloy film can be deposited on304L stainless steel byelectroplating. The property of film closely related to deposition current.With smaller deposition current, the film is more smooth and dense, andthe hardness of film is higher. So correspondingly, the property of corrosion resistance is better. As the deposite current density decreases, Inboling acetic and formic acids containing200ppm Br-, the corrosion rateof the films prepared with1.2A/dm~2current density is0.61g·m~(-2)·h~(-1). Butthe corrosion rate of film drops to0.05g·m~(-2)·h~(-1)once the current densityreduce to0.8A/dm~2. The influence of Cu content was also investigated.When the content of CuSO_4is1.5g/L, the film prepared with0.8A/dm~2current density has the best corrosion resintance, and the corrosion rate isonly0.02g·m~(-2)·h~(-1).
The codeposition hydrogen in the film can be removed by heattreatment, hence the electrochemical performance can be greatlyrecovered, which leads to higher corrosion potential and better corrosionresistance. After heat treatment, the micro-hardness is obviouslyimproved, in addition, the lattice structure and element content remain thesame. XPS analysis indicated that Pd is metallic state after200℃treatment, However, after treating at400℃，oxidation reaction happenedto Pd.
A Pd-Ni/Pd-Cu double coating with a thickness of about3μm wasdeposited on stainless steel surface by electroplating. The double coatingshows obviously higher hardness, modulus of elasticity and adhesivestrength to the substrate in contrast to single Pd-Cu coating. The porosityof the deposited coating also decreased evidently. The lower porosity ofthe double coating may reduce chloride migration through the deposited film. The higher hardness, modulus and adhesive strength would increasethe erosion resistance. All these factors result in better corrosionresistance. The Pd-Ni/Pd-Cu double coating significantly improved thecorrosion resistance of316L stainless steel in strong corrosive medium.Particularly, the double coating exhibits better resistance in complicatedcorrosive environment including erosion and chloride ions. In boilingacetic and formic acids mixture containing0.005mol/L Cl~-with900r/min stir, the corrosion rate of the double coating coated316L stainlesssteel is about one order of magnitude lower than that of Pd-Cu coatedsamples.
A thin layer of Pd deposition on the surface significantly improves thecorrosion resistance of316L stainless steel in0.5mol L-1H_2SO_4+2ppmF-solution at80℃. The Pd film promotes spontaneous passivition andthe corrosion rate of the Pd plated specimen decreases by three orders ofmagnitude in contrast to that of the original316L specimens. When316Lstainless steel specimen is coupled with Pd electrode, the passive filmformed on stainless steel shows much better corrosion resistance than theair-formed passive film. After the disconnection of the stainless/Pd couple,the stainless steel specimen still remains passivated for a relatively longtime. The Mott-Schottky measurements show that compared with theair-formed passive films, there are less point defects in the passive filmon the specimens coupled with Pd. XPS measurements show that the main difference between the compositions of the two films is theenrichment of Cr and the presence of Cr(OH)_3and Fe_3O_4in the passivefilms coupled with palladium. These differences lead to the bettercorrosion resistance of the passive film formed under the effect ofpalladium film.
Last but important, As a potential material for bipolar plates in protonexchange membrane (PEM) fuel cells, Pd and Cr-Pd film was depositedon316L stainless steel. Corrosion resistance and interface contactresistance were studued. Comared with original316L stainless steel, thecorrosion rate of specimen with Pd or Cr-Pd film decrease by three ordersof magnitude, and the interface contact resistance is also obviouslydecreased. Adding Cr in Pd film can further improve the corrosionresistance for Cr(OH)_3exsits in Cr-Pd film as a beneficial component. Inaddition, adding Cr can lower the cost of the films.
引文
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