纳米二氧化锰基复合材料的制备及其电化学特性研究
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摘要
二氧化锰（MnO_2）是一种极具潜力的超级电容器用电极材料，但其较差的导电率和复杂多样的结构形貌限制了其电化学性能的发挥。本论文旨在提高MnO_2的电化学性能，通过纳米化和复合导电材料的策略，设计并制备高性能的纳米复合材料，探索材料制备工艺、微观结构和电化学特性之间的联系；并在此基础上，从非对称器件结构角度去构建兼具高功率密度和高能量密度的非对称电容器。
鉴于导电聚合物良好的电容行为和导电性，本文选择了两种导电聚合物来提高MnO_2的电化学性能，并相应地制备了MnO_2/导电聚合物纳米复合材料。首先，采用界面法合成了MnO_2/聚苯胺微纳复合球，结果表明复合物具有空心结构和介孔特性，这种独特的三维层次结构使得电解液能够贮存且离子扩散阻力小，复合材料的比电容达到262F/g。其次，首次提出采用MnO_2作为反应模板，通过原位聚合一步合成了聚吡咯纳米结构。通过调控反应摩尔比，获得了MnO_2/聚吡咯一维纳米复合管，组分间的协同作用赋予其最高318F/g的比电容量，且倍率特性和循环稳定性优异。
利用电纺纳米碳纤维无纺布作为导电基体，通过原位氧化还原法将MnO_2纳米结构均匀地沉积在纤维表面，获得了具有同轴结构的MnO_2@纳米碳纤维自支撑电极材料，避免了使用导电添加剂和粘结剂，降低了电极质量并简化了电极制备，复合材料表现出良好的电化学性能。接着从改善外层MnO_2纳米结构形貌、提高芯层纳米碳纤维导电性以及纳米复合聚吡咯等角度分别开发了三种有效的制备方式来进一步提高MnO_2的利用率，且都获得了性能更加优异的电极材料。此外，还探讨了温度对MnO_2@纳米碳纤维电化学行为的影响机理。
最后，提出并设计了基于自支撑电极材料的水系非对称电容器体系，组装了以MnO_2@纳米碳纤维为正极、活性纳米碳纤维为负极以及Na2SO4水溶液为电解液的非对称电容器，工作电压达2.0V，分析了正极和负极材料优化器件性能的措施，最终获得了兼具高功率密度（20.8kW/kg）和高能量密度（30.6Wh/kg）的非对称电容器，显示出了广阔的应用前景。
Manganese dioxides (MnO_2) hold a significant promise as electrode materials forsupercapacitors, but the electrochemical performance is ultimately limited by its poorelectrical conductivity. It is therefore the aim of this work to fully exploit the potentialof MnO_2-based electrode materials. The dissertation proposes strategic designs andfabrication of high-performance nanocomposites by incorporating MnO_2nanostructuresinto conducting materials, and then explores the close relationship between synthesistechnique, microstucture and the electrochemical properties. From a point view ofelectrode configuration based on these new electrode materials, asymmetricsupercapacitors are finally constructed to harvest both high power density and highenergy density.
In view of the good pseudocapacive behavior and good electrical conductivity ofconducting polymers, two kinds of MnO_2/conducting polymers nanocomposites wereprepared. Firstly, mesoporous MnO_2/polyaniline composites with unique morphology ofhierarchical hollow submicron spheres were prepared by modified interfacial synthesis.The three-dimentional architecture provides not only the “ion-buffering reservoirs” forrapid Faradic reactions but also the rich and uniform meso-channels for fast electrolyticdiffusion. The hierarchical nanocomposites electrode exhibits high specific capacitanceof262F/g with good rate capability. Secondly, a novel approach based on a reactivetemplate of MnO_2was proposed for the first time to in-situ polymerize polypyrrolenanostructures. By controlling the molar ratio of MnO_2and pyrrole monomers,one-dimentional nanotubular MnO_2/polypyrrole nanocomposites were prepared. Andthe synergistic effect between each component ensures a maximum specific capacitanceof318F/g with excellent rate capability and cycling stability.
Electrospun carbon nanofibers (CNF) fabric was used as conductive substrates foruniform grow MnO_2nanostructures on the surface of CNF by in-situ redox deposition.The as-prepared MnO_2@CNF nanocomposites showed unique coaxial configurationand exhibited good electrochemical performance when used as freestanding electrodes.Afterwards, three effective sythesis techniques were developed to further improve theutilization of MnO_2nanostructures, including the introduction of porous, ultrathinMnO_2nanflakes, the increase in the electrical conductivity of CNF cores by embedding carbon nanotubes and the nano-combination with polypyrrole. The three resultedfreestanding nanocomposites electrodes showed better electrochemical prepertiescompared to the counterparts. Moreover, the effect of temperature on thepseudo-capacitive behavior of the freestanding MnO_2@CNF was extensively studied.
Finally, a novel aqueous asymmetric sucapacitors was proposed and designedrationally by using two completely freestanding electrodes, i.e., MnO_2@CNF as thepositive electrode and activated CNF as the negative electrode. The influence ofpositive electrode and negative electrode on the electrochemical performance ofthe asymmetric supercapacitors was investigated. The as-assembled asymmetricsupercapacitor with optimal mass ratio can be operated reversibly over a widevoltage range of0-2.0V, and presented both high energy density of30.6Wh/kgand high power density of20.8kW/kg. The high-performance asymmetricsupercapacitors based on freestanding electrodes may find great applications inthe increasing demands on energy storage systems with high energy/powerdelivery.
鉴于导电聚合物良好的电容行为和导电性，本文选择了两种导电聚合物来提高MnO_2的电化学性能，并相应地制备了MnO_2/导电聚合物纳米复合材料。首先，采用界面法合成了MnO_2/聚苯胺微纳复合球，结果表明复合物具有空心结构和介孔特性，这种独特的三维层次结构使得电解液能够贮存且离子扩散阻力小，复合材料的比电容达到262F/g。其次，首次提出采用MnO_2作为反应模板，通过原位聚合一步合成了聚吡咯纳米结构。通过调控反应摩尔比，获得了MnO_2/聚吡咯一维纳米复合管，组分间的协同作用赋予其最高318F/g的比电容量，且倍率特性和循环稳定性优异。
利用电纺纳米碳纤维无纺布作为导电基体，通过原位氧化还原法将MnO_2纳米结构均匀地沉积在纤维表面，获得了具有同轴结构的MnO_2@纳米碳纤维自支撑电极材料，避免了使用导电添加剂和粘结剂，降低了电极质量并简化了电极制备，复合材料表现出良好的电化学性能。接着从改善外层MnO_2纳米结构形貌、提高芯层纳米碳纤维导电性以及纳米复合聚吡咯等角度分别开发了三种有效的制备方式来进一步提高MnO_2的利用率，且都获得了性能更加优异的电极材料。此外，还探讨了温度对MnO_2@纳米碳纤维电化学行为的影响机理。
最后，提出并设计了基于自支撑电极材料的水系非对称电容器体系，组装了以MnO_2@纳米碳纤维为正极、活性纳米碳纤维为负极以及Na2SO4水溶液为电解液的非对称电容器，工作电压达2.0V，分析了正极和负极材料优化器件性能的措施，最终获得了兼具高功率密度（20.8kW/kg）和高能量密度（30.6Wh/kg）的非对称电容器，显示出了广阔的应用前景。
Manganese dioxides (MnO_2) hold a significant promise as electrode materials forsupercapacitors, but the electrochemical performance is ultimately limited by its poorelectrical conductivity. It is therefore the aim of this work to fully exploit the potentialof MnO_2-based electrode materials. The dissertation proposes strategic designs andfabrication of high-performance nanocomposites by incorporating MnO_2nanostructuresinto conducting materials, and then explores the close relationship between synthesistechnique, microstucture and the electrochemical properties. From a point view ofelectrode configuration based on these new electrode materials, asymmetricsupercapacitors are finally constructed to harvest both high power density and highenergy density.
In view of the good pseudocapacive behavior and good electrical conductivity ofconducting polymers, two kinds of MnO_2/conducting polymers nanocomposites wereprepared. Firstly, mesoporous MnO_2/polyaniline composites with unique morphology ofhierarchical hollow submicron spheres were prepared by modified interfacial synthesis.The three-dimentional architecture provides not only the “ion-buffering reservoirs” forrapid Faradic reactions but also the rich and uniform meso-channels for fast electrolyticdiffusion. The hierarchical nanocomposites electrode exhibits high specific capacitanceof262F/g with good rate capability. Secondly, a novel approach based on a reactivetemplate of MnO_2was proposed for the first time to in-situ polymerize polypyrrolenanostructures. By controlling the molar ratio of MnO_2and pyrrole monomers,one-dimentional nanotubular MnO_2/polypyrrole nanocomposites were prepared. Andthe synergistic effect between each component ensures a maximum specific capacitanceof318F/g with excellent rate capability and cycling stability.
Electrospun carbon nanofibers (CNF) fabric was used as conductive substrates foruniform grow MnO_2nanostructures on the surface of CNF by in-situ redox deposition.The as-prepared MnO_2@CNF nanocomposites showed unique coaxial configurationand exhibited good electrochemical performance when used as freestanding electrodes.Afterwards, three effective sythesis techniques were developed to further improve theutilization of MnO_2nanostructures, including the introduction of porous, ultrathinMnO_2nanflakes, the increase in the electrical conductivity of CNF cores by embedding carbon nanotubes and the nano-combination with polypyrrole. The three resultedfreestanding nanocomposites electrodes showed better electrochemical prepertiescompared to the counterparts. Moreover, the effect of temperature on thepseudo-capacitive behavior of the freestanding MnO_2@CNF was extensively studied.
Finally, a novel aqueous asymmetric sucapacitors was proposed and designedrationally by using two completely freestanding electrodes, i.e., MnO_2@CNF as thepositive electrode and activated CNF as the negative electrode. The influence ofpositive electrode and negative electrode on the electrochemical performance ofthe asymmetric supercapacitors was investigated. The as-assembled asymmetricsupercapacitor with optimal mass ratio can be operated reversibly over a widevoltage range of0-2.0V, and presented both high energy density of30.6Wh/kgand high power density of20.8kW/kg. The high-performance asymmetricsupercapacitors based on freestanding electrodes may find great applications inthe increasing demands on energy storage systems with high energy/powerdelivery.
引文
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