导电聚合物及其杂化电活性功能材料的可控制备与应用
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摘要
电活性材料(Electroactive Material, EM)是电子-离子的混合导体,其体相在氧化和还原过程中能够从溶液中可逆地置入和释放离子(离子交换或充放电过程)成为电导体。EM主要包括无机过渡金属络合物、导电高分子聚合物和有机/无机杂化材料,它们所具有的电化学属性并不随EM的体相不同而改变。EM在离子选择性电极、离子交换膜、化学/生物传感器、电催化、二次电池以及电致生色器件等新技术领域有着广阔的应用前景。因此,寻求廉价、易合成、高电子传递速率、高离子交换容量、高电催化活性和高循环稳定性的EM,是EM研究的重点。
聚苯胺是导电高分子EM中具有代表性的导电聚合物,虽然广大研究者通过不同方法合成不同形貌的聚苯胺基EM并用于不同领域,但很少人注意到不同分子构象聚苯胺的物理化学特性及分子构象对聚苯胺本质属性的影响。因此我们可以通过合成单一分子构象或一种分子构象含量多的聚苯胺材料,研究分子构象对其本质属性的影响。本论文首次通过单极脉冲自组装聚合法制备了全顺式聚苯胺纳米管膜电极,并阐明该全顺式聚苯胺纳米管的自组装聚合成长机理。该全顺式聚苯胺纳米管膜具有低的电荷传递阻力、好的润湿性、高的表观扩散系数、高的离子交换容量和良好的稳定性,这些优良的性能都归因于全顺式聚苯胺具有螺旋上升的分子结构。并将该全顺式聚苯胺成功用于超级电容器材料和电催化氧化抗坏血酸传感器,同时期待该材料应用于其他电化学领域。
在众多电控离子交换材料中,对重金属离子具有选择性的电活性材料的报道很少。因此,开发电控重金属离子交换材料来处理重金属离子废水迫在眉睫。本论文首次将聚2,6-吡啶二甲酸导电高分子EM应用于电控离子交换分离回收废液中的铜离子,并提出一种全新的电控离子交换机制。采用EQCM方法原位跟踪离子置入置出膜的过程,并通过傅立叶红外光谱(FTIR)和X-射线光电子能谱(XPS)等方法对聚2,6-吡啶二甲酸电控离子交换分离回收铜离子机理进行分析。结果表明,聚2,6-吡啶二甲酸对铜离子具有优良的选择性、高的离子交换容量和超强的循环稳定性。
本论文首次采用单极脉冲氧化法将铁氰化镍纳米颗粒锚固到碳纳米管表面,制得铁氰化镍/壳聚糖/碳纳米管复合膜电极,并通过调变氧化电位来实现对铁氰化镍的结构调控。该复合膜电极制备方法简单、结构可控,整个膜合成过程时间仅仅几分钟。该膜作为双氧水传感器,显示了优良的电催化还原活性,其归因于碳纳米管与铁氰化镍的协同催化效应。结果表明,在-0.2V电位下对双氧水的电催化活性最高,其检测双氧水的线性范围为0.04-5.6mM,敏感度为654mA-M-1·cm-2,在2s内电催化反应达到平衡,在信噪比为3时其检出限为2.8×101M。
本论文还通过一步循环伏安电沉积法在碳纳米管表面沉积得到立方体聚苯胺/铁氰化镍纳米复合颗粒。通过扫描电子显微镜(SEM)和FTIR对立方体聚苯胺/铁氰化镍纳米复合颗粒的形貌和结构进行表征,观察到立方体聚苯胺/铁氰化镍纳米复合颗粒均匀的分散在碳纳米管表面。由于羧基化碳纳米管的引入,为导电聚苯胺链上的氮原子提供了一种酸性的导电微环境,使得该复合膜电极在中性条件下具有电活性。该复合膜用于双氧水传感器显示了良好的电催化还原性能,归因于碳纳米管与铁氰化镍间的协同效应。结果表明,该复合膜作为双氧水传感器具有高的敏感度、快速的响应时间和低的检测限,其电催化双氧水的动力学常数为1.29×108cm3·mol-1·s-1。同时该复合膜具有高稳定性和重现性。
This field encompasses mixed (electron-ion) conducting materials whose bulk phases can be charged/discharged electronically from an external electric circuit or by chemical agents. To retain the electroneutrality of the phase the transferred electronic charge must be compensated by the incorporation/expulsion of ionic species. Such a phenomenon is characteristic of numerous systems with very diverse chemical natures, including redox or electronically conducting polymers, inorganic solids with mixed-valence transition metals, and lithium cation intercalation layers, placed in contact with an electrolyte solution. Despite the broad variety of underlying molecular mechanisms, the electrochemical processes occurring in these materials possess many common features. It is important that the EM with high electronic transfer rate, high ion exchange capacity and high stability, was found and synthesized.
In this paper, the all cis-polyaniline nanotube film was successfully obtained using a novel unipolar pulse electro-polymerization method. To the best our knowledge, this is the first report and confirmation of this kind promising film composed of all cis-polyaniline nanotubes. To date, although various polyaniline-based materials have been synthesized and used in different fields, little attention has been paid to these potentially important species on which the chemical and physical properties of polyaniline are based. Only a few scattered reports can be found in the literatures with respect to the molecular conformation of PANI and the effects of possible isomeric forms on the intrinsic properties of polyaniline. That may be why some conflicting results were reported even by some highly respectable research groups. Therefore, in order to understand the performance mechanism of PANI and to determine the intrinsic properties of PANI, it should be very interesting if we can synthesize PANI preferably in one isomeric form or as a mixture containing a smaller than usual number of different isomer. In the present study, we found a facile way to get the all cis-polyaniline nanotube film and its formation mechanism was also analyzed and discussed. Furthermore, many excellent performances such as less charge transfer resistance, better water wettability, higher apparent diffusion coefficient, higher redox site capacity and super-stability of all cis-polyaniline nanotube film with the unique chemical molecular conformation were identified and successfully applied for the supercapacitor and high sensitive ascorbic acid sensor. It is expected that this advanced material will be applied in many electrochemical fields based on this Study.
In this paper, the PPDC film was successfully obtained using a novel unipolar pulse electro-polymerization method and its electronic switch copper ion exchange mechanism was analyzed and discussed. The process and mechanism of copper ion exchange were characterized by electrochemical quartz crystal microbalance (EQCM), X-ray Photoelectron Spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR). The PPDC film prepared had good stability and high ion exchange capacity, and should be useful in practical heavy metal ion waste treatment.
Unipolar pulse waveforms consist of an applied anode potential during the on-period and an open-circuit potential during the off-period. Unipolar pulse electrodeposition was used to fabricate nickel hexacyanoferrate/chitosan/carbon nanotubes (NiHCF/CS/CNTs) nanocomposite films with controllable structure on electrode surface and the as-prepared films were applied in hydrogen peroxide (H2O2) sensor. One-step electrodeposition of NiHCF/CS/CNTs film with insoluble-structure NiHCF nanoparticles was performed, and the whole procedure took only several minutes. The morphology and the composition of the NiHCF/CS/CNTs film were characterized by scanning electron microscopy (SEM) and energy dispersive X-ray (EDS). With the introduction of CNTs, the formed NiHCF/CS/CNTs system showed synergy between CNTs and NiHCF with a significant improvement of redox activity of NiHCF due to the excellent electron-transfer ability of CNTs. Electrochemical experiments revealed that the modified electrode allowed low potential (-0.2V) detection of H2O2and showed high electrocatalytic activity to the reduction of H2O2. The linear range for the detection of H2O2was0.04-5.6mM with a high sensitivity of654mA M-1cm2, and the response was very fast (less than2s). A detection limit of as low as2.8×10-7M (S/N=3) for H2O2was achieved.
Electroactive hybrid films with cubic nickel hexacyanoferrate/polyaniline (NiHCF/PANI) were synthesized on carbon nanotubes (CNTs) modified platinum electrodes by a facile one-step electrosynthesis method using cyclic voltammetry (CV). The morphologies and structures of the as-prepared NiHCF/PANI/CNTs films were characterized using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR), respectively. Due to the introduction of CNTs with carboxyl groups, an acidic micro-environment was provided for the nitrogen atoms in the PANI chains, which could maintain its electroactivity in neutral aqueous solutions. The hybrid films were applied for hydrogen peroxide (H2O2) detection and showed synergy and higher electrocatalytic activity with a higher sensitivity, a faster response time and a lower detection limit. It was found that detection sensitivity could be regulated by controlling the time of CV of electrosynthesis during the preparation of the hybrid film. A catalytic rate constant of1.29×108cm3·mol-1·s-1was obtained from an investigation of the kinetics of the catalytic reaction. SEM images showed that the cubic composite nano-particles of PANI and NiHCF were formed and distributed uniformly on the CNTs. The hybrid film prepared had good stability and reproducibility in the detection of H2O2, and should be useful in practical H2O2sensors.
聚苯胺是导电高分子EM中具有代表性的导电聚合物,虽然广大研究者通过不同方法合成不同形貌的聚苯胺基EM并用于不同领域,但很少人注意到不同分子构象聚苯胺的物理化学特性及分子构象对聚苯胺本质属性的影响。因此我们可以通过合成单一分子构象或一种分子构象含量多的聚苯胺材料,研究分子构象对其本质属性的影响。本论文首次通过单极脉冲自组装聚合法制备了全顺式聚苯胺纳米管膜电极,并阐明该全顺式聚苯胺纳米管的自组装聚合成长机理。该全顺式聚苯胺纳米管膜具有低的电荷传递阻力、好的润湿性、高的表观扩散系数、高的离子交换容量和良好的稳定性,这些优良的性能都归因于全顺式聚苯胺具有螺旋上升的分子结构。并将该全顺式聚苯胺成功用于超级电容器材料和电催化氧化抗坏血酸传感器,同时期待该材料应用于其他电化学领域。
在众多电控离子交换材料中,对重金属离子具有选择性的电活性材料的报道很少。因此,开发电控重金属离子交换材料来处理重金属离子废水迫在眉睫。本论文首次将聚2,6-吡啶二甲酸导电高分子EM应用于电控离子交换分离回收废液中的铜离子,并提出一种全新的电控离子交换机制。采用EQCM方法原位跟踪离子置入置出膜的过程,并通过傅立叶红外光谱(FTIR)和X-射线光电子能谱(XPS)等方法对聚2,6-吡啶二甲酸电控离子交换分离回收铜离子机理进行分析。结果表明,聚2,6-吡啶二甲酸对铜离子具有优良的选择性、高的离子交换容量和超强的循环稳定性。
本论文首次采用单极脉冲氧化法将铁氰化镍纳米颗粒锚固到碳纳米管表面,制得铁氰化镍/壳聚糖/碳纳米管复合膜电极,并通过调变氧化电位来实现对铁氰化镍的结构调控。该复合膜电极制备方法简单、结构可控,整个膜合成过程时间仅仅几分钟。该膜作为双氧水传感器,显示了优良的电催化还原活性,其归因于碳纳米管与铁氰化镍的协同催化效应。结果表明,在-0.2V电位下对双氧水的电催化活性最高,其检测双氧水的线性范围为0.04-5.6mM,敏感度为654mA-M-1·cm-2,在2s内电催化反应达到平衡,在信噪比为3时其检出限为2.8×101M。
本论文还通过一步循环伏安电沉积法在碳纳米管表面沉积得到立方体聚苯胺/铁氰化镍纳米复合颗粒。通过扫描电子显微镜(SEM)和FTIR对立方体聚苯胺/铁氰化镍纳米复合颗粒的形貌和结构进行表征,观察到立方体聚苯胺/铁氰化镍纳米复合颗粒均匀的分散在碳纳米管表面。由于羧基化碳纳米管的引入,为导电聚苯胺链上的氮原子提供了一种酸性的导电微环境,使得该复合膜电极在中性条件下具有电活性。该复合膜用于双氧水传感器显示了良好的电催化还原性能,归因于碳纳米管与铁氰化镍间的协同效应。结果表明,该复合膜作为双氧水传感器具有高的敏感度、快速的响应时间和低的检测限,其电催化双氧水的动力学常数为1.29×108cm3·mol-1·s-1。同时该复合膜具有高稳定性和重现性。
This field encompasses mixed (electron-ion) conducting materials whose bulk phases can be charged/discharged electronically from an external electric circuit or by chemical agents. To retain the electroneutrality of the phase the transferred electronic charge must be compensated by the incorporation/expulsion of ionic species. Such a phenomenon is characteristic of numerous systems with very diverse chemical natures, including redox or electronically conducting polymers, inorganic solids with mixed-valence transition metals, and lithium cation intercalation layers, placed in contact with an electrolyte solution. Despite the broad variety of underlying molecular mechanisms, the electrochemical processes occurring in these materials possess many common features. It is important that the EM with high electronic transfer rate, high ion exchange capacity and high stability, was found and synthesized.
In this paper, the all cis-polyaniline nanotube film was successfully obtained using a novel unipolar pulse electro-polymerization method. To the best our knowledge, this is the first report and confirmation of this kind promising film composed of all cis-polyaniline nanotubes. To date, although various polyaniline-based materials have been synthesized and used in different fields, little attention has been paid to these potentially important species on which the chemical and physical properties of polyaniline are based. Only a few scattered reports can be found in the literatures with respect to the molecular conformation of PANI and the effects of possible isomeric forms on the intrinsic properties of polyaniline. That may be why some conflicting results were reported even by some highly respectable research groups. Therefore, in order to understand the performance mechanism of PANI and to determine the intrinsic properties of PANI, it should be very interesting if we can synthesize PANI preferably in one isomeric form or as a mixture containing a smaller than usual number of different isomer. In the present study, we found a facile way to get the all cis-polyaniline nanotube film and its formation mechanism was also analyzed and discussed. Furthermore, many excellent performances such as less charge transfer resistance, better water wettability, higher apparent diffusion coefficient, higher redox site capacity and super-stability of all cis-polyaniline nanotube film with the unique chemical molecular conformation were identified and successfully applied for the supercapacitor and high sensitive ascorbic acid sensor. It is expected that this advanced material will be applied in many electrochemical fields based on this Study.
In this paper, the PPDC film was successfully obtained using a novel unipolar pulse electro-polymerization method and its electronic switch copper ion exchange mechanism was analyzed and discussed. The process and mechanism of copper ion exchange were characterized by electrochemical quartz crystal microbalance (EQCM), X-ray Photoelectron Spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR). The PPDC film prepared had good stability and high ion exchange capacity, and should be useful in practical heavy metal ion waste treatment.
Unipolar pulse waveforms consist of an applied anode potential during the on-period and an open-circuit potential during the off-period. Unipolar pulse electrodeposition was used to fabricate nickel hexacyanoferrate/chitosan/carbon nanotubes (NiHCF/CS/CNTs) nanocomposite films with controllable structure on electrode surface and the as-prepared films were applied in hydrogen peroxide (H2O2) sensor. One-step electrodeposition of NiHCF/CS/CNTs film with insoluble-structure NiHCF nanoparticles was performed, and the whole procedure took only several minutes. The morphology and the composition of the NiHCF/CS/CNTs film were characterized by scanning electron microscopy (SEM) and energy dispersive X-ray (EDS). With the introduction of CNTs, the formed NiHCF/CS/CNTs system showed synergy between CNTs and NiHCF with a significant improvement of redox activity of NiHCF due to the excellent electron-transfer ability of CNTs. Electrochemical experiments revealed that the modified electrode allowed low potential (-0.2V) detection of H2O2and showed high electrocatalytic activity to the reduction of H2O2. The linear range for the detection of H2O2was0.04-5.6mM with a high sensitivity of654mA M-1cm2, and the response was very fast (less than2s). A detection limit of as low as2.8×10-7M (S/N=3) for H2O2was achieved.
Electroactive hybrid films with cubic nickel hexacyanoferrate/polyaniline (NiHCF/PANI) were synthesized on carbon nanotubes (CNTs) modified platinum electrodes by a facile one-step electrosynthesis method using cyclic voltammetry (CV). The morphologies and structures of the as-prepared NiHCF/PANI/CNTs films were characterized using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR), respectively. Due to the introduction of CNTs with carboxyl groups, an acidic micro-environment was provided for the nitrogen atoms in the PANI chains, which could maintain its electroactivity in neutral aqueous solutions. The hybrid films were applied for hydrogen peroxide (H2O2) detection and showed synergy and higher electrocatalytic activity with a higher sensitivity, a faster response time and a lower detection limit. It was found that detection sensitivity could be regulated by controlling the time of CV of electrosynthesis during the preparation of the hybrid film. A catalytic rate constant of1.29×108cm3·mol-1·s-1was obtained from an investigation of the kinetics of the catalytic reaction. SEM images showed that the cubic composite nano-particles of PANI and NiHCF were formed and distributed uniformly on the CNTs. The hybrid film prepared had good stability and reproducibility in the detection of H2O2, and should be useful in practical H2O2sensors.
引文
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