电化学合成聚吡咯膜的电学性能与应用
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摘要
聚吡咯(polypyrrole, PPy)不仅具有优异的电性能和电化学性能,而且具有合成容易、价格低廉和环境友好等优势,被认为是一种具有广阔应用前景的电子导电高分子(Electronically Conductive Polymer, ECP)材料。大量研究表明,PPy性能容易通过制备条件进行“剪裁”,在各种制备方法中,电化学法兼具原位成膜的便利和膜厚易控制的优势。本文在多种电极(钽、铜和铝阳极体)表面原位电合成PPy膜,着重研究聚合条件对PPy的结构和电化学性能的影响,探索其在超级电容器、防腐和聚合物铝电解电容器的应用。
在钽电极上实现了0℃下高密度PPy(High Density PPy,HD-PPy)的大电流(10 mA·cm~（-2）)制备,获得的PPy膜的密度为1.42 g·cm~(-3)。该密度值和目前报道的在-40℃用低电流密度(0.02～0.05 mA·cm~（-2）)时得到的值相当,而本文的制备方法具有容易实现、周期短和成本低的优势,因此更具有应用价值。结构研究表明,HD-PPy的形成机理是高电流密度导致了平面型二维分子链结构的形成。其室温电导率高达200 S·cm-1,比通常的PPy膜具有更优异的热稳定性和能显著地阻碍离子传输,因此将是优异的电极材料和金属防腐材料。
为了实现无模板法合成特殊微/纳结构的PPy,研究了溶液pH值和电流密度对PPy结构和形貌的影响。在pH=9的溶液中采用大电流密度(>3mA·cm~（-2）)首次合成了具有微/纳结构羊角状的PPy(horn-like PPy, h-PPy),其形成机理可能是在高电流密度下形成了一种非平面型的二维分子链结构。h-PPy不仅具有高比表面积和高结晶度,并且室温电导率达到90 S·cm-1,与之相比在该pH下用小电流密度合成的常见椰菜花形状PPy的室温电导率<10 S·cm-1。
为了提高PPy电极材料的充放电速率和电位窗,采用了聚(3,4-乙撑二氧噻吩)(PEDOT)表面修饰PPy。由于协同效应,PEDOT/PPy复合物具有比单一材料更高的比容量和充放电速率,并具有PEDOT的高电位窗(1V)。特别是在h-PPy表面获得的多孔PEDOT/h-PPy双层复合物,由于多孔结构有利于电解液的扩散,其比容量达到290 F·g~（-1）并具有快速的充放电性能。在浓硫酸/浓硝酸中超声振荡单壁碳纳米管(SWNTs),获取长度小于100 nm并高度离子化的功能化单壁碳纳米管(F-SWNTs),进一步电化学制备了颗粒尺寸约为100 nm的PPy/F-SWNTs复合物。其比容量达到230 F·g~（-1）,电荷转移电阻极低(小于0.05Ω),且在电位窗0.8 V下具有稳定的循环性能。通过正交实验优化制备条件,获得了多孔的PPy膜,其电化学性能可以进一步通过掺杂离子剪裁:PPy-Cl具有高比容量,可达到270 F·g~（-1）, PPy-TOS(对甲基苯磺酸根)具有快速充放电能力,并都具有稳定的循环性能。为了提高基于PPy的多孔电极的面积比容量,提出了用多次聚合法制备多孔PPy-Cl和PPy-TOS厚膜,其面积比容量高达5 F·cm~（-2）,且质量比容量未随膜厚增加而明显降低。因此这四种基于PPy的材料都将是优异的超级电容器电极材料。
在金属铜电极表面预先电合成PPy-C2O4衬底层,实现了在铜电极上电化学制备HD-PPy和PPy-DBS膜。在3.5wt% NaCl溶液中防腐性能测试表明,由于有效的物理阻隔作用,HD-PPy电极的腐蚀电流比LD-PPy低一个数量级。与PPy-C2O4和PPy-TOS相比,PPy-DBS的有效保护时间为三倍以上,腐蚀电流低两个数量级。其原因在于DBS-体积较大而固定在PPy网格内,通过对腐蚀离子(Cl-)和C_2O_4~(2-)的静电排斥作用,既可以阻碍Cl-穿透PPy膜而腐蚀金属基底,也可以阻碍C_2O_4~(2-)从膜中逃逸而长时间维持电极的“自愈”能力。
通过在铝阳极体表面用高锰酸钾氧化吡咯单体制备一层导电衬底层以及控制氧化剂浓度和相应的浸渍次数,掌握了在绝缘铝阳极体表面均匀现场电化学被覆PPy的关键技术,采用有效的阻隔材料和优化的电流方案缩短电化学聚合时间突破了该类电容器漏电流大的瓶颈问题。在中试线上,通过引入热处理和后期补形成工艺,进一步降低了该电容器的漏电流,研制出具有自主知识产权的高性能片式化铝固体电解电容器,并通过教育部组织的专家组鉴定,性能达到国际先进水平,目前正在福建国光电子股份有限公司进行工业规模化生产。
Polypyrrole (PPy) has been extensively investigated and was considered as the promising Electronically Conductive polymers (ECP), due to its excellent properties and advantages including environmentally friendly feature, low cost and facile synthesis.
In the studies, the high density PPy films (HD-PPy), doped by p-toluenesulfonate (TOS-), were prepared on tatanum electrodes at the current density of 10 mA?cm-2 at 0℃. Its density was up to 1.42 g?cm-3, which was slightly larger than the maximum reported value abtained on glass carbon electrodes by 0.02～0.05 mA?cm-2 at -40℃. The method in the studies was of more practical value from the view of application, because it is easy to perform, low cost, time saving, and especially independent of the electrode surface. Its high density was resulted from the formation of plane-type two dimensional (2D) structure of molecular chains. The conductivity of HD-PPy was up to 200 S?cm-1. Furthermore, the thermal stability of HD-PPy films was significantly superior to that of conventional PPy films. In additional, HD-PPy could hinder ions insertion more effectively. It can be concluded that HD-PPy would be an excellent electrode material and anticorrosion material.
Aiming to explore free-template method to relize micro/nano-PPy, the effects of pH and current density of polymerization on the morphology and structure of PPy were investigated. The horn-like PPy films (h-PPy) with horns in micro/nano size were obtained at pH=9 with current density larger than 3mA?cm-2. The horn might be a kind of non-plane 2D structure of molecure chains resulted from high current density in polymerizaiton. Furthermore, h-PPy was characterized as great specific area, highly ordering, and attractive conductivity up to 90 S?cm-1.
To improve the charge/discharge rate and cycling stability of PPy-based electode of supercapacitor, the PEDOT/h-PPy composites and the composites of PPy and functionalized single-walled carbon nanotubes (F-SWNTs) were prepared by electrochemical methods. The two kinds of composites were characterized with highly porous structure, which leads to their specific capacitance up to 290 and 230 F?g-1 in 1M KCl aqueous solutions, respectively. Furthermore, they have very fast charge/ discharge rate and good cycle stability at potential window of 1V and 0.8 V, respectively.The porous PPy films were also obtained in the optimized conditions, whose electrochemical properties can be tailored by doping ions. By trying several ions, PPy-Cl had high specific capacitance up to 270 F?g-1, while PPy-TOS had very rapid charge/discharge ability. To achieve PPy with high area specific capacitance, we proposed the multi-step method to prepare porous thick PPy films. The results showed that two kinds of even porous PPy films, PPy-Cl and PPy-TOS with area specific capacitance up to 5 F?cm-2 were obtained by the method. Moreover, their mass specific capacitance could reach 330 F?g-1 and 191 F?g-1 at discharge current of 1 mA?cm-2. In concusion, PEDOT/h-PPy, PPy/F-SWNTs, PPy-Cl and PPy-TOS will be promissing electrode materials for supercapacitors.
HD-PPy and PPy doped with dodecylbenzenesulfonate (PPy-DBS) were prepared on an underlayer of PPy doped with oxalate (PPy-C2O4) by galvanostatical method for effective copper protection, because PPy-TOS and PPy-DBS could not be obtained directly on copper surface by electrochemical methods. Their anticorrosion performance in 3.5% NaCl solution was signifanctly superior to that of conventional PPy-TOS and the bilayer PPy-C2O4, coatings with equal thickness. The reason is that HD-PPy and PPy-DBS could obstruct the corrosion ions (Cl-) from penetrating the PPy films and hinder the oxalate from escaping so that the healing ability of PPy could be maintained for a long term. The results demonstrate that HD-PPy and PPy-DBS films on an underlayer of PPy-C2O4 have potential application to protect copper.
The PPy aluminum solid electrolytic capacitors (PA-Cap) were realized by electropolymerization of PPy on the underlayer of PPy/MnO2 prepared by chemical method. The leakage current can be effectively decreased by using coating silicon rubber and shortening polymerization, and can be further dereased by thermal treatment during pilot production. The aluminum electrolytic capacitors with high performance were achieved by optimizing oxidant concentration, dip numbers and current density of polymerization, and had been put into manufacture.
在钽电极上实现了0℃下高密度PPy(High Density PPy,HD-PPy)的大电流(10 mA·cm~（-2）)制备,获得的PPy膜的密度为1.42 g·cm~(-3)。该密度值和目前报道的在-40℃用低电流密度(0.02～0.05 mA·cm~（-2）)时得到的值相当,而本文的制备方法具有容易实现、周期短和成本低的优势,因此更具有应用价值。结构研究表明,HD-PPy的形成机理是高电流密度导致了平面型二维分子链结构的形成。其室温电导率高达200 S·cm-1,比通常的PPy膜具有更优异的热稳定性和能显著地阻碍离子传输,因此将是优异的电极材料和金属防腐材料。
为了实现无模板法合成特殊微/纳结构的PPy,研究了溶液pH值和电流密度对PPy结构和形貌的影响。在pH=9的溶液中采用大电流密度(>3mA·cm~（-2）)首次合成了具有微/纳结构羊角状的PPy(horn-like PPy, h-PPy),其形成机理可能是在高电流密度下形成了一种非平面型的二维分子链结构。h-PPy不仅具有高比表面积和高结晶度,并且室温电导率达到90 S·cm-1,与之相比在该pH下用小电流密度合成的常见椰菜花形状PPy的室温电导率<10 S·cm-1。
为了提高PPy电极材料的充放电速率和电位窗,采用了聚(3,4-乙撑二氧噻吩)(PEDOT)表面修饰PPy。由于协同效应,PEDOT/PPy复合物具有比单一材料更高的比容量和充放电速率,并具有PEDOT的高电位窗(1V)。特别是在h-PPy表面获得的多孔PEDOT/h-PPy双层复合物,由于多孔结构有利于电解液的扩散,其比容量达到290 F·g~（-1）并具有快速的充放电性能。在浓硫酸/浓硝酸中超声振荡单壁碳纳米管(SWNTs),获取长度小于100 nm并高度离子化的功能化单壁碳纳米管(F-SWNTs),进一步电化学制备了颗粒尺寸约为100 nm的PPy/F-SWNTs复合物。其比容量达到230 F·g~（-1）,电荷转移电阻极低(小于0.05Ω),且在电位窗0.8 V下具有稳定的循环性能。通过正交实验优化制备条件,获得了多孔的PPy膜,其电化学性能可以进一步通过掺杂离子剪裁:PPy-Cl具有高比容量,可达到270 F·g~（-1）, PPy-TOS(对甲基苯磺酸根)具有快速充放电能力,并都具有稳定的循环性能。为了提高基于PPy的多孔电极的面积比容量,提出了用多次聚合法制备多孔PPy-Cl和PPy-TOS厚膜,其面积比容量高达5 F·cm~（-2）,且质量比容量未随膜厚增加而明显降低。因此这四种基于PPy的材料都将是优异的超级电容器电极材料。
在金属铜电极表面预先电合成PPy-C2O4衬底层,实现了在铜电极上电化学制备HD-PPy和PPy-DBS膜。在3.5wt% NaCl溶液中防腐性能测试表明,由于有效的物理阻隔作用,HD-PPy电极的腐蚀电流比LD-PPy低一个数量级。与PPy-C2O4和PPy-TOS相比,PPy-DBS的有效保护时间为三倍以上,腐蚀电流低两个数量级。其原因在于DBS-体积较大而固定在PPy网格内,通过对腐蚀离子(Cl-)和C_2O_4~(2-)的静电排斥作用,既可以阻碍Cl-穿透PPy膜而腐蚀金属基底,也可以阻碍C_2O_4~(2-)从膜中逃逸而长时间维持电极的“自愈”能力。
通过在铝阳极体表面用高锰酸钾氧化吡咯单体制备一层导电衬底层以及控制氧化剂浓度和相应的浸渍次数,掌握了在绝缘铝阳极体表面均匀现场电化学被覆PPy的关键技术,采用有效的阻隔材料和优化的电流方案缩短电化学聚合时间突破了该类电容器漏电流大的瓶颈问题。在中试线上,通过引入热处理和后期补形成工艺,进一步降低了该电容器的漏电流,研制出具有自主知识产权的高性能片式化铝固体电解电容器,并通过教育部组织的专家组鉴定,性能达到国际先进水平,目前正在福建国光电子股份有限公司进行工业规模化生产。
Polypyrrole (PPy) has been extensively investigated and was considered as the promising Electronically Conductive polymers (ECP), due to its excellent properties and advantages including environmentally friendly feature, low cost and facile synthesis.
In the studies, the high density PPy films (HD-PPy), doped by p-toluenesulfonate (TOS-), were prepared on tatanum electrodes at the current density of 10 mA?cm-2 at 0℃. Its density was up to 1.42 g?cm-3, which was slightly larger than the maximum reported value abtained on glass carbon electrodes by 0.02～0.05 mA?cm-2 at -40℃. The method in the studies was of more practical value from the view of application, because it is easy to perform, low cost, time saving, and especially independent of the electrode surface. Its high density was resulted from the formation of plane-type two dimensional (2D) structure of molecular chains. The conductivity of HD-PPy was up to 200 S?cm-1. Furthermore, the thermal stability of HD-PPy films was significantly superior to that of conventional PPy films. In additional, HD-PPy could hinder ions insertion more effectively. It can be concluded that HD-PPy would be an excellent electrode material and anticorrosion material.
Aiming to explore free-template method to relize micro/nano-PPy, the effects of pH and current density of polymerization on the morphology and structure of PPy were investigated. The horn-like PPy films (h-PPy) with horns in micro/nano size were obtained at pH=9 with current density larger than 3mA?cm-2. The horn might be a kind of non-plane 2D structure of molecure chains resulted from high current density in polymerizaiton. Furthermore, h-PPy was characterized as great specific area, highly ordering, and attractive conductivity up to 90 S?cm-1.
To improve the charge/discharge rate and cycling stability of PPy-based electode of supercapacitor, the PEDOT/h-PPy composites and the composites of PPy and functionalized single-walled carbon nanotubes (F-SWNTs) were prepared by electrochemical methods. The two kinds of composites were characterized with highly porous structure, which leads to their specific capacitance up to 290 and 230 F?g-1 in 1M KCl aqueous solutions, respectively. Furthermore, they have very fast charge/ discharge rate and good cycle stability at potential window of 1V and 0.8 V, respectively.The porous PPy films were also obtained in the optimized conditions, whose electrochemical properties can be tailored by doping ions. By trying several ions, PPy-Cl had high specific capacitance up to 270 F?g-1, while PPy-TOS had very rapid charge/discharge ability. To achieve PPy with high area specific capacitance, we proposed the multi-step method to prepare porous thick PPy films. The results showed that two kinds of even porous PPy films, PPy-Cl and PPy-TOS with area specific capacitance up to 5 F?cm-2 were obtained by the method. Moreover, their mass specific capacitance could reach 330 F?g-1 and 191 F?g-1 at discharge current of 1 mA?cm-2. In concusion, PEDOT/h-PPy, PPy/F-SWNTs, PPy-Cl and PPy-TOS will be promissing electrode materials for supercapacitors.
HD-PPy and PPy doped with dodecylbenzenesulfonate (PPy-DBS) were prepared on an underlayer of PPy doped with oxalate (PPy-C2O4) by galvanostatical method for effective copper protection, because PPy-TOS and PPy-DBS could not be obtained directly on copper surface by electrochemical methods. Their anticorrosion performance in 3.5% NaCl solution was signifanctly superior to that of conventional PPy-TOS and the bilayer PPy-C2O4, coatings with equal thickness. The reason is that HD-PPy and PPy-DBS could obstruct the corrosion ions (Cl-) from penetrating the PPy films and hinder the oxalate from escaping so that the healing ability of PPy could be maintained for a long term. The results demonstrate that HD-PPy and PPy-DBS films on an underlayer of PPy-C2O4 have potential application to protect copper.
The PPy aluminum solid electrolytic capacitors (PA-Cap) were realized by electropolymerization of PPy on the underlayer of PPy/MnO2 prepared by chemical method. The leakage current can be effectively decreased by using coating silicon rubber and shortening polymerization, and can be further dereased by thermal treatment during pilot production. The aluminum electrolytic capacitors with high performance were achieved by optimizing oxidant concentration, dip numbers and current density of polymerization, and had been put into manufacture.
引文
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