电化学超级电容器多孔碳电极材料的研究
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摘要
电化学超级电容器是介于传统电容器和充电电池之间的一种新型储能装置,因具有高比功率和长寿命等突出优点,近年来已成为电化学储能领域的研究热点。但是,与传统的二次电池如锂离子电池相比,超级电容器的能量密度较低,因此目前有许多研究工作者都致力于提高超级电容器体系的能量密度。根据超级电容器的能量密度公式E=1/2 CV2,可以通过两种有效的方法来提高电容器的能量密度：一是增大电极材料的比电容(C),二是提高电容器的工作电压(V)。基于这种分析,为了提高多孔碳电极的能量密度,本论文的研究内容首先集中在对于多孔碳材料孔结构的优化,通过调节孔的大小、孔连接以及构建有序多级孔结构,提高多孔比表面积的利用率,从而提高电极材料的比能量。其次,从碳纳米管/线出发,采用制备简单的MnO2及天然生物表壳为模板,创新合成了具有多种新颖结构的介孔碳纳米管/线、介孔碳纳米线阵列材料,多孔结构增加了碳纳米管/线的比表面积,增大了材料的比电容；同时,管线结构减小了电极材料的内阻,提高了电容器的工作电压。具体内容介绍如下：
1.三维有序介孔碳球阵列的制备及电化学性能的研究
目前,广泛应用于电容器的活性炭材料虽然具有较高的比表面积,但是由于存在大量的封闭微孔以及无序的孔连接,比表面积利用率较低,因而对比电容的贡献甚微。由于介孔碳材料具有高度有序的孔道结构,且在中孔范围内孔径分布单一,因此引起了人们的广泛关注。我们以介孔碳孔的大小、孔连接为出发点,采用硬模板Si02与软模板P123相结合的两步模板法制备三维有序介孔碳球阵列,比表面积为601 m2/g,球内介孔孔径为10.4 nm,且碳球阵列间存在孔径为60 nm的堆积窗口。对其在有机系中进行电化学性能的测试,结果表明,其比电容为84 F/g,单位表面积比电容为14μF/cm2,相比于商业活性炭的表面积比电容有很大提高,而且倍率性能和循环性能也均有很大的改善。这是因为较大的孔径为电解液提供了更多的入口,使电极材料更易被电解液浸润,从而具有更高的表面利用率,提高了表面积比电容；此外,阵列间的窗口也提供了电解液的储存空间,更有利于电解液的渗透和离子的快速传输,石墨化结构以及阵列结构也提高了材料的导电性,从而提高了材料的倍率和循环性能。
2.有序介孔/微孔复合多级孔碳材料的制备及电化学性能的研究
有序介孔有着非常优异的倍率特性,但是其比容量一直受到比表面积的制约,而小于2 nm的微孔碳会在特定的孔径范围内拥有超反常的大比容量储能能力。我们以有序介孔碳化钛/碳的复合物为前躯体,通过氯气原位除钛反应,得到了有序介孔孔壁上拥有大量微孔结构的有序多级孔碳材料。通过调节TiC中的Ti含量、碳化温度、氯气处理温度来调节微孔、介孔的孔径大小以及微孔/介孔的比例,得到了较高的比表面积1917 m2/g,介孔孔径为3.0 nm,微孔孔径为0.69nm及1.25 nm的多级孔碳材料,从而提高了材料在有机体系中的电化学性能,表现出146 F/g较高的比电容。有序的介孔结构保证了电解液的浸润和传输,以及较高的电导率,从而提高比功率；同时接近有机电解液离子大小的微孔可以大大提高材料的储能比表面积,提高比电容。因此有序介孔/微孔复合多级孔碳材料表现出具有高能量密度以及高功率密度的双重特性。
3.天然生物前驱体制备微孔/介孔复合多级孔碳材料及其电化学性能的研究
采用模板法及氯气处理法可以制备得到多级孔碳材料,但是其操作复杂耗时,并且一定程度上对环境造成了影响。而天然生物由于其来源充足、可再生、环境友好,是一种理想的新型碳源。我们首次尝试采用天然生物(海藻)为直接前驱体,通过冷冻干燥及高温碳化的过程制备微孔/介孔复合多级孔碳材料。不同种类的海藻经过碳化处理后也形成不同多级孔结构的碳材料,并在超级电容器的应用中显示出良好的电化学性能,水系中比电容为150 F/g。同时我们通过ZnCl2的活化作用达到扩孔目的,提高多级孔碳材料的比表面积,使得电解液充分的浸润和储存,同时提供了更有效的离子传输通道,提高碳材料的比电容至194 F/g。介孔结构有利于提高材料的功率密度,介孔孔壁上的大量微孔结构也对提高材料的能量密度起到了至关重要的作用,同时通过活化扩孔处理,可以调节微孔与介孔的比例,从而优化材料的电化学性能。
4.MnO2模板法制备不同形貌的介孔碳纳米管材料及其电化学性能的研究
碳纳米管表面性质稳定,电导率高,也被应用在较高工作电压的电容器中,但由于碳纳米管材料的比表面积较小,对比电容的贡献十分有限。因此我们采用环保的,形貌可控的二氧化锰为硬模板,并结合软模板的方法制备不同形貌的有序介孔碳纳米管、介孔碳纳米管刺球、介孔碳纳米管套线。得到的介孔碳纳米管具有较高的比表面积1079 m2/g,较大的介孔孔径为9.6 nm,在有机体系中表现了较高的比电容124 F/g。二氧化锰可被盐酸羟胺简便除去,大大降低了实验的成本,提高实验操作的安全性。电化学测试结果表明,相比于活性炭材料,介孔碳纳米管的管状结构降低了材料的内阻,从而提高了电容器的实际工作电压；同时,大量的介孔也提高了碳纳米管材料的比表面积,从而使电极材料具有更高的比电容；此外,碳纳米管上的介孔以及管内较大的管径通道均为电解液提供了更多的传输通道,更有利于电解液的渗透和离子的快速传输,从而提高了材料的倍率和循环性能。同时采用形貌可控的MnO2为模板也可以运用到其它氧化物等无机材料的合成中。
5.天然生物模板法制备介孔碳纳米线阵列及其电化学性能的研究
碳纳米管/线材料由于其比表面积较低对比电容有一定的制约作用,但是将其有序排列成阵列结构,既会增加材料的比表面积,也会提高其导电性。我们首次采用天然生物螃蟹表壳(主要为碳酸钙)为模板,结合自组装软模板法,制备了高度有序介孔碳纳米线阵列。该材料具有有序的多级孔结构：大孔孔道为1μm,阵列纳米线间通道为70 nm,纳米线上高度有序的介孔为11 nm,比表面积为1270 m2/g,并表现了较高的比电容152 F/g,同时也具备了优越的倍率和循环性能。碳纳米线的阵列结构以及纳米线上的介孔结构,都大大提高材料的比表面积,并且有效的提供了电解液离子浸润和传输的通道,具有更高的比电容；微米级有序阵列结构相比于活性炭以及杂乱分散堆积的单体碳纳米管/线结构具有较高的导电性能,从而降低了内阻,提高了材料的倍率和循环性能。另外,生物模板由于其来源充足,可持续性强,成本低,环保,结构复杂有序,由此可获得多种具有多级有序结构与特殊形貌的仿生材料。
6.高温处理介孔碳纳米线阵列及其在高电位超级电容器中的应用研究
在碳纳米管制备和纯化的过程中,表面会引入有机官能团杂质,使其在高电位时与电解液发生不可逆的副反应,从而影响了电容器的充电电压和比电容。因此,我们尝试对介孔碳纳米线阵列在氮气气氛中进行进一步的高温处理,去除表面有机官能团。测试表明其表面的C=O、C-O以及O-H基团都有一定程度的减少；并且随着处理温度的进一步增高,碳材料的石墨化程度也相应的提高,从而有利于提高材料的电导率。在较高的0-4 V的电位区间对其进行充放电测试表明,其比电容及库伦效率都有了很大的提高。因此,较高的表面处理温度有效的减少了碳纳米线表面的有机杂质官能团,避免了在高电位时发生的不可逆的副反应,提高电容器的充电电压和库伦效率；同时表面基团的减少也提高了碳材料表面的浸润性,降低电极材料的内阻,从而提高双电层电容器的倍率性能和循环寿命。
Electrochemical supercapacitor is a new type of energy storage device between traditional capacitors and rechargeable batteries. Because of its high specific power and long life and other outstanding advantages, in recent years, supercapacitors have attracted great interest in energy storage applications. However, its energy density is much lower than that of secondary batteries, such as lithium-ion battery, so many researchers are committed to improve the energy density of supercapacitor system. According to the energy equation of supercapacitors E=1/2 CV2, two effective apporaches can be used to improve the energy density of supercapacitors:one is increasing the specific capacitance of electrode material (C), the other one is to promote the output voltage (V). Based on this analysis, in order to improve the energy density of the porous carbon electrode, firstly, the researches of this thesis focused on the optimization of pore structure, by adjusting the pore size, pore connectivity and building hierarchical porous structure to improve the utilization of surface area, so improve the specific energy of electrode materials. Secondly, we creatively synthesize mesoporous carbon nanotubes/nanowires with a variety of novel structure and mesoporous carbon nanofiber arrays by MnO2 and natural carb shll templates, and the porous structures increase the surface area of he carbon materials which is benefit to improving the specific capacitance. Meanwhile, the nanotube and nanofiber structures will reduce the internal resistance of the electrode material, so increase the capacitor working voltage.
1. Synthsis of three-dimensional ordered mesoporous carbon sphere arrays and its electrochemical performance in supercapacitor
Currently, activated carbon materials with a high surface area are widely used in capacitors, but because there are a lot of closed pores and disordered pore connectivity, the utilization of the surface area is low, thus it contributes little to specific capacitance. Ordered mesoporous carbon has attracted much attention due to its highly ordered pore structure and narrow pore size distribution in mesopore range. A novel three-dimensional ordered mesoporous carbon sphere arrays (MCSAs) with surface area of 601 m2/g, a large pore size of 10.4 nm and a window size of 60 nm was successfully synthesized through a two-step template method by the combination of the surfactant-templating organic resol self-assembly, colloidal crystals of polystyrene and silica hard templating routes. MCSAs deliver a larger specific area capacitance of than commercial activated carbon (14μF/cm2,84 F/g). The good performances might be owing to its large ordered pore size and the continuous connected windows between the spheres which are favorable for the penetration of electrolyte and ion transportation at high scan rates, so it shows a higher surface utilization and high specific capacitance. Also the arrays of electrode materials and the graphite structure should have better electrical conductivity, so the rate capability and cycling performance are greatly improved.
2. Synthsis of hierarchical ordered mesoporous/microporous carbon and its electrochemical performance in supercapacitor
Mesoporous carbon has excellent rate capability characteristics, but its specific energy has been subjected to its low surface area. While there is an anomalous increase in carbon capacitance at pore size smaller than 2 nm. We develop a facile approach to prepare hierarchical ordered mesoporous/microporous carbon (OMMC) by synthesizing ordered mesoporous nanocrystalline titanium-carbide/carbon composites, followed by in situ chlorination of carbides. By adjusting the content of Ti in TiC, carbonization temperature, temperature of chlorine treatment, we regulate the micropore size, the mesopore size and the microporous/mesoporous ratio. The obtained hierarchical porous carbon materials consist of a narrow mesopore with size of 3.0 nm, and micropores on the walls with size of 0.69 and 1.25 nm. The ordered mesoporous channels ensure retention and immersion of the electrolyte, serving as a favorable ion-path for electrolyte penetration and allowing for fast ionic transport into the bulk of the OMMC particles, good electronic conductivity, thus show an excellent capacitance retention at high discharge rates for pulse power applications. At the same time, the micropores drilled on the mesopore walls allow the produced OMMC to exhibit a specific surface area up to 1917 m2/g and a specific capacitance up to 146 F/g for an outstanding energy density. The unique hierarchical porous structure contributes to attractive capabilities as a promising material in energy storage with both high energy density and high power density.
3. Preparation of hierarchical mesoporous/microporous carbon from natural organism precursor and its electrochemical performance in supercapacitor
Using the template method and chlorination treatment method can prepare hierarchical porous carbon materials, but it is time-consuming, operation-complicated, and with a bad impact on the environment. However, novel carbon sources, seaweeds, are naturally occurring, simple and environmentally benign. Hierarchical mesoporous/microporous carbons are produced by freeze-drying and carbonization processes using various seaweeds as carbon sources. Different hierarchical porous carbon materials come from different type seaweed after carbonization, and the application in supercapacitor show a good electrochemical performance with a capacity of 150 F/g in 6 M KOH solution. Meanwhile, treatment with ZnCl2 as pore-enlarge activation was successfully achieved by a simple pyrolysis process. It improves the surface area, making it sufficient for electrolyte infiltration and storage, and providing a more efficient ion transmission channel, so it shows a lager specific capacitance of 194 F/g. Mesoporous materials can improve the power density, and the micropores play a crucial role in improving the energy density. We can also adjust microporous/mesoporous ratio through activation, in order to optimize the electrochemical performance.
4. Direct synthesis of different morphology mesoporous carbon nanotubes using MnO2 as template and their electrochemical performance in supercapacitors
Because of the stability of surface properties and high conductivity, carbon nanotubes are an ideal electrode material for use in high voltage capacitor. But the specific surface area of carbon nanotubes is small, so the capacitance contribution is very limited. Therefore, we use MnO2 as hard template, which is environmental friendly and morphology controllable, combined with the soft template self-assembly process, to prepare mesoporous carbon nanotubes, mesoporous carbon nano-thorn microspheres and mesoporous carbon nanowires in nanotubes. Mesoporous carbon nanotube with a high surface area of 1079 m2/g and a large pore size of 9.6 nm show a capacitance of 124 F/g. MnO2 can be easily removed by HCl, so greatly reduce the costs, improve the safety of experimental operation. Electrochemical test results show that the nanotube structure can reduce the internal resistance of carbon materials, thus improves the actual working voltage; meanwhile, a large number of mesoporous on the carbon nanotubes also contribute to the surface area, so that the material has a higher specific capacitance. In addition, the large mesopores and large inner tubes provide more channels for the electrolyte rapid penetration and ion transmission, thereby reducing the internal resistance of nanotubes, and improve the rate capability and cycling performance. At the same time, this synthesis method can be easily extended to preparation of other nano-sized mesoporous materials.
5. Synthesis of highly ordered mesoporous carbon nanofiber arrays from a crab shell biological template and its electrochemical performance in supercapacitors
The low surface area of carbon nanotubes/wires restricts the capacitance in supercapacitor. However, arranged them in an orderly array will not only increase the surface area, but also improve its conductivity. We develope a natural biological template approach for the successful synthesis of novel highly-ordered mesoporous carbon nanofiber arrays by combining surfactant-templating self-assembly of organic resols with natural crab shell hard-templating process. The obtained materials consist of a mesoporous carbon nanofiber (70 nm in mean diameter and 11 nm in mesopore), an interspacing void of 70 nm between nanofibers, and 1 micrometer of pores between nanofiber arrays. The structure of arrays and the large mesopores in the nanofiber greatly increase the surface area of materials to 1270 m2/g, and effectively provides transport channel for electrolyte ion, so it has a higher specific capacitance of 152 F/g. The micro-sized array structure also has higher electronic conductivity than activated carbon and the accumulation of single carbon nanotube/line, so it reduces the internal resistance, and ensures a higher actual working voltage, better rate capability and cycling performance. In addition, the biological templates are abundant, sustainable, low cost, environmental friendly, structural complex and ordered. Furthermore, the biomimetic strategy may present a new possibility for the synthesis of various nano-structured mesoporous materials with special morphologies.
6. High-temperature treatment of mesoporous carbon nanowire arrays and its high voltage application in supercapacitors
In the process of the preparation and purification of carbon nanutubes, the impurities of organic functional groups will be introduced on the surface, which may irreversibly reacted with the electrolyte at high voltage, thus affecting the charge voltage and specific capacitance of the capacitors. By further treatment of mesoporous carbon nanowires in nitrogen at high temperature, we remove the surface organic functional groups off. Tests show that the C=O, CO and OH groups on the carbon surface have a reduction with certain degree;and as the temperature further increased, the graphitization degree of the carbon materials increased accordingly. The above factors help to improve electrical conductivity, so it shows an improving specific capacitance at higher voltage of 4 V. Higher treatment temperatures effectively reduce the organic impurities functional groups on the surface of carbon nanowires, to avoid irreversible reaction at high voltage. So it improves the rated voltage of capacitors and the coulomb efficiency. The treatment of surface also increases the infiltration ability of electrolyte and reduces the internal resistance of the electrode material, thereby enhancing the rate capability and cycling performance of supercapacitor.
1.三维有序介孔碳球阵列的制备及电化学性能的研究
目前,广泛应用于电容器的活性炭材料虽然具有较高的比表面积,但是由于存在大量的封闭微孔以及无序的孔连接,比表面积利用率较低,因而对比电容的贡献甚微。由于介孔碳材料具有高度有序的孔道结构,且在中孔范围内孔径分布单一,因此引起了人们的广泛关注。我们以介孔碳孔的大小、孔连接为出发点,采用硬模板Si02与软模板P123相结合的两步模板法制备三维有序介孔碳球阵列,比表面积为601 m2/g,球内介孔孔径为10.4 nm,且碳球阵列间存在孔径为60 nm的堆积窗口。对其在有机系中进行电化学性能的测试,结果表明,其比电容为84 F/g,单位表面积比电容为14μF/cm2,相比于商业活性炭的表面积比电容有很大提高,而且倍率性能和循环性能也均有很大的改善。这是因为较大的孔径为电解液提供了更多的入口,使电极材料更易被电解液浸润,从而具有更高的表面利用率,提高了表面积比电容；此外,阵列间的窗口也提供了电解液的储存空间,更有利于电解液的渗透和离子的快速传输,石墨化结构以及阵列结构也提高了材料的导电性,从而提高了材料的倍率和循环性能。
2.有序介孔/微孔复合多级孔碳材料的制备及电化学性能的研究
有序介孔有着非常优异的倍率特性,但是其比容量一直受到比表面积的制约,而小于2 nm的微孔碳会在特定的孔径范围内拥有超反常的大比容量储能能力。我们以有序介孔碳化钛/碳的复合物为前躯体,通过氯气原位除钛反应,得到了有序介孔孔壁上拥有大量微孔结构的有序多级孔碳材料。通过调节TiC中的Ti含量、碳化温度、氯气处理温度来调节微孔、介孔的孔径大小以及微孔/介孔的比例,得到了较高的比表面积1917 m2/g,介孔孔径为3.0 nm,微孔孔径为0.69nm及1.25 nm的多级孔碳材料,从而提高了材料在有机体系中的电化学性能,表现出146 F/g较高的比电容。有序的介孔结构保证了电解液的浸润和传输,以及较高的电导率,从而提高比功率；同时接近有机电解液离子大小的微孔可以大大提高材料的储能比表面积,提高比电容。因此有序介孔/微孔复合多级孔碳材料表现出具有高能量密度以及高功率密度的双重特性。
3.天然生物前驱体制备微孔/介孔复合多级孔碳材料及其电化学性能的研究
采用模板法及氯气处理法可以制备得到多级孔碳材料,但是其操作复杂耗时,并且一定程度上对环境造成了影响。而天然生物由于其来源充足、可再生、环境友好,是一种理想的新型碳源。我们首次尝试采用天然生物(海藻)为直接前驱体,通过冷冻干燥及高温碳化的过程制备微孔/介孔复合多级孔碳材料。不同种类的海藻经过碳化处理后也形成不同多级孔结构的碳材料,并在超级电容器的应用中显示出良好的电化学性能,水系中比电容为150 F/g。同时我们通过ZnCl2的活化作用达到扩孔目的,提高多级孔碳材料的比表面积,使得电解液充分的浸润和储存,同时提供了更有效的离子传输通道,提高碳材料的比电容至194 F/g。介孔结构有利于提高材料的功率密度,介孔孔壁上的大量微孔结构也对提高材料的能量密度起到了至关重要的作用,同时通过活化扩孔处理,可以调节微孔与介孔的比例,从而优化材料的电化学性能。
4.MnO2模板法制备不同形貌的介孔碳纳米管材料及其电化学性能的研究
碳纳米管表面性质稳定,电导率高,也被应用在较高工作电压的电容器中,但由于碳纳米管材料的比表面积较小,对比电容的贡献十分有限。因此我们采用环保的,形貌可控的二氧化锰为硬模板,并结合软模板的方法制备不同形貌的有序介孔碳纳米管、介孔碳纳米管刺球、介孔碳纳米管套线。得到的介孔碳纳米管具有较高的比表面积1079 m2/g,较大的介孔孔径为9.6 nm,在有机体系中表现了较高的比电容124 F/g。二氧化锰可被盐酸羟胺简便除去,大大降低了实验的成本,提高实验操作的安全性。电化学测试结果表明,相比于活性炭材料,介孔碳纳米管的管状结构降低了材料的内阻,从而提高了电容器的实际工作电压；同时,大量的介孔也提高了碳纳米管材料的比表面积,从而使电极材料具有更高的比电容；此外,碳纳米管上的介孔以及管内较大的管径通道均为电解液提供了更多的传输通道,更有利于电解液的渗透和离子的快速传输,从而提高了材料的倍率和循环性能。同时采用形貌可控的MnO2为模板也可以运用到其它氧化物等无机材料的合成中。
5.天然生物模板法制备介孔碳纳米线阵列及其电化学性能的研究
碳纳米管/线材料由于其比表面积较低对比电容有一定的制约作用,但是将其有序排列成阵列结构,既会增加材料的比表面积,也会提高其导电性。我们首次采用天然生物螃蟹表壳(主要为碳酸钙)为模板,结合自组装软模板法,制备了高度有序介孔碳纳米线阵列。该材料具有有序的多级孔结构：大孔孔道为1μm,阵列纳米线间通道为70 nm,纳米线上高度有序的介孔为11 nm,比表面积为1270 m2/g,并表现了较高的比电容152 F/g,同时也具备了优越的倍率和循环性能。碳纳米线的阵列结构以及纳米线上的介孔结构,都大大提高材料的比表面积,并且有效的提供了电解液离子浸润和传输的通道,具有更高的比电容；微米级有序阵列结构相比于活性炭以及杂乱分散堆积的单体碳纳米管/线结构具有较高的导电性能,从而降低了内阻,提高了材料的倍率和循环性能。另外,生物模板由于其来源充足,可持续性强,成本低,环保,结构复杂有序,由此可获得多种具有多级有序结构与特殊形貌的仿生材料。
6.高温处理介孔碳纳米线阵列及其在高电位超级电容器中的应用研究
在碳纳米管制备和纯化的过程中,表面会引入有机官能团杂质,使其在高电位时与电解液发生不可逆的副反应,从而影响了电容器的充电电压和比电容。因此,我们尝试对介孔碳纳米线阵列在氮气气氛中进行进一步的高温处理,去除表面有机官能团。测试表明其表面的C=O、C-O以及O-H基团都有一定程度的减少；并且随着处理温度的进一步增高,碳材料的石墨化程度也相应的提高,从而有利于提高材料的电导率。在较高的0-4 V的电位区间对其进行充放电测试表明,其比电容及库伦效率都有了很大的提高。因此,较高的表面处理温度有效的减少了碳纳米线表面的有机杂质官能团,避免了在高电位时发生的不可逆的副反应,提高电容器的充电电压和库伦效率；同时表面基团的减少也提高了碳材料表面的浸润性,降低电极材料的内阻,从而提高双电层电容器的倍率性能和循环寿命。
Electrochemical supercapacitor is a new type of energy storage device between traditional capacitors and rechargeable batteries. Because of its high specific power and long life and other outstanding advantages, in recent years, supercapacitors have attracted great interest in energy storage applications. However, its energy density is much lower than that of secondary batteries, such as lithium-ion battery, so many researchers are committed to improve the energy density of supercapacitor system. According to the energy equation of supercapacitors E=1/2 CV2, two effective apporaches can be used to improve the energy density of supercapacitors:one is increasing the specific capacitance of electrode material (C), the other one is to promote the output voltage (V). Based on this analysis, in order to improve the energy density of the porous carbon electrode, firstly, the researches of this thesis focused on the optimization of pore structure, by adjusting the pore size, pore connectivity and building hierarchical porous structure to improve the utilization of surface area, so improve the specific energy of electrode materials. Secondly, we creatively synthesize mesoporous carbon nanotubes/nanowires with a variety of novel structure and mesoporous carbon nanofiber arrays by MnO2 and natural carb shll templates, and the porous structures increase the surface area of he carbon materials which is benefit to improving the specific capacitance. Meanwhile, the nanotube and nanofiber structures will reduce the internal resistance of the electrode material, so increase the capacitor working voltage.
1. Synthsis of three-dimensional ordered mesoporous carbon sphere arrays and its electrochemical performance in supercapacitor
Currently, activated carbon materials with a high surface area are widely used in capacitors, but because there are a lot of closed pores and disordered pore connectivity, the utilization of the surface area is low, thus it contributes little to specific capacitance. Ordered mesoporous carbon has attracted much attention due to its highly ordered pore structure and narrow pore size distribution in mesopore range. A novel three-dimensional ordered mesoporous carbon sphere arrays (MCSAs) with surface area of 601 m2/g, a large pore size of 10.4 nm and a window size of 60 nm was successfully synthesized through a two-step template method by the combination of the surfactant-templating organic resol self-assembly, colloidal crystals of polystyrene and silica hard templating routes. MCSAs deliver a larger specific area capacitance of than commercial activated carbon (14μF/cm2,84 F/g). The good performances might be owing to its large ordered pore size and the continuous connected windows between the spheres which are favorable for the penetration of electrolyte and ion transportation at high scan rates, so it shows a higher surface utilization and high specific capacitance. Also the arrays of electrode materials and the graphite structure should have better electrical conductivity, so the rate capability and cycling performance are greatly improved.
2. Synthsis of hierarchical ordered mesoporous/microporous carbon and its electrochemical performance in supercapacitor
Mesoporous carbon has excellent rate capability characteristics, but its specific energy has been subjected to its low surface area. While there is an anomalous increase in carbon capacitance at pore size smaller than 2 nm. We develop a facile approach to prepare hierarchical ordered mesoporous/microporous carbon (OMMC) by synthesizing ordered mesoporous nanocrystalline titanium-carbide/carbon composites, followed by in situ chlorination of carbides. By adjusting the content of Ti in TiC, carbonization temperature, temperature of chlorine treatment, we regulate the micropore size, the mesopore size and the microporous/mesoporous ratio. The obtained hierarchical porous carbon materials consist of a narrow mesopore with size of 3.0 nm, and micropores on the walls with size of 0.69 and 1.25 nm. The ordered mesoporous channels ensure retention and immersion of the electrolyte, serving as a favorable ion-path for electrolyte penetration and allowing for fast ionic transport into the bulk of the OMMC particles, good electronic conductivity, thus show an excellent capacitance retention at high discharge rates for pulse power applications. At the same time, the micropores drilled on the mesopore walls allow the produced OMMC to exhibit a specific surface area up to 1917 m2/g and a specific capacitance up to 146 F/g for an outstanding energy density. The unique hierarchical porous structure contributes to attractive capabilities as a promising material in energy storage with both high energy density and high power density.
3. Preparation of hierarchical mesoporous/microporous carbon from natural organism precursor and its electrochemical performance in supercapacitor
Using the template method and chlorination treatment method can prepare hierarchical porous carbon materials, but it is time-consuming, operation-complicated, and with a bad impact on the environment. However, novel carbon sources, seaweeds, are naturally occurring, simple and environmentally benign. Hierarchical mesoporous/microporous carbons are produced by freeze-drying and carbonization processes using various seaweeds as carbon sources. Different hierarchical porous carbon materials come from different type seaweed after carbonization, and the application in supercapacitor show a good electrochemical performance with a capacity of 150 F/g in 6 M KOH solution. Meanwhile, treatment with ZnCl2 as pore-enlarge activation was successfully achieved by a simple pyrolysis process. It improves the surface area, making it sufficient for electrolyte infiltration and storage, and providing a more efficient ion transmission channel, so it shows a lager specific capacitance of 194 F/g. Mesoporous materials can improve the power density, and the micropores play a crucial role in improving the energy density. We can also adjust microporous/mesoporous ratio through activation, in order to optimize the electrochemical performance.
4. Direct synthesis of different morphology mesoporous carbon nanotubes using MnO2 as template and their electrochemical performance in supercapacitors
Because of the stability of surface properties and high conductivity, carbon nanotubes are an ideal electrode material for use in high voltage capacitor. But the specific surface area of carbon nanotubes is small, so the capacitance contribution is very limited. Therefore, we use MnO2 as hard template, which is environmental friendly and morphology controllable, combined with the soft template self-assembly process, to prepare mesoporous carbon nanotubes, mesoporous carbon nano-thorn microspheres and mesoporous carbon nanowires in nanotubes. Mesoporous carbon nanotube with a high surface area of 1079 m2/g and a large pore size of 9.6 nm show a capacitance of 124 F/g. MnO2 can be easily removed by HCl, so greatly reduce the costs, improve the safety of experimental operation. Electrochemical test results show that the nanotube structure can reduce the internal resistance of carbon materials, thus improves the actual working voltage; meanwhile, a large number of mesoporous on the carbon nanotubes also contribute to the surface area, so that the material has a higher specific capacitance. In addition, the large mesopores and large inner tubes provide more channels for the electrolyte rapid penetration and ion transmission, thereby reducing the internal resistance of nanotubes, and improve the rate capability and cycling performance. At the same time, this synthesis method can be easily extended to preparation of other nano-sized mesoporous materials.
5. Synthesis of highly ordered mesoporous carbon nanofiber arrays from a crab shell biological template and its electrochemical performance in supercapacitors
The low surface area of carbon nanotubes/wires restricts the capacitance in supercapacitor. However, arranged them in an orderly array will not only increase the surface area, but also improve its conductivity. We develope a natural biological template approach for the successful synthesis of novel highly-ordered mesoporous carbon nanofiber arrays by combining surfactant-templating self-assembly of organic resols with natural crab shell hard-templating process. The obtained materials consist of a mesoporous carbon nanofiber (70 nm in mean diameter and 11 nm in mesopore), an interspacing void of 70 nm between nanofibers, and 1 micrometer of pores between nanofiber arrays. The structure of arrays and the large mesopores in the nanofiber greatly increase the surface area of materials to 1270 m2/g, and effectively provides transport channel for electrolyte ion, so it has a higher specific capacitance of 152 F/g. The micro-sized array structure also has higher electronic conductivity than activated carbon and the accumulation of single carbon nanotube/line, so it reduces the internal resistance, and ensures a higher actual working voltage, better rate capability and cycling performance. In addition, the biological templates are abundant, sustainable, low cost, environmental friendly, structural complex and ordered. Furthermore, the biomimetic strategy may present a new possibility for the synthesis of various nano-structured mesoporous materials with special morphologies.
6. High-temperature treatment of mesoporous carbon nanowire arrays and its high voltage application in supercapacitors
In the process of the preparation and purification of carbon nanutubes, the impurities of organic functional groups will be introduced on the surface, which may irreversibly reacted with the electrolyte at high voltage, thus affecting the charge voltage and specific capacitance of the capacitors. By further treatment of mesoporous carbon nanowires in nitrogen at high temperature, we remove the surface organic functional groups off. Tests show that the C=O, CO and OH groups on the carbon surface have a reduction with certain degree;and as the temperature further increased, the graphitization degree of the carbon materials increased accordingly. The above factors help to improve electrical conductivity, so it shows an improving specific capacitance at higher voltage of 4 V. Higher treatment temperatures effectively reduce the organic impurities functional groups on the surface of carbon nanowires, to avoid irreversible reaction at high voltage. So it improves the rated voltage of capacitors and the coulomb efficiency. The treatment of surface also increases the infiltration ability of electrolyte and reduces the internal resistance of the electrode material, thereby enhancing the rate capability and cycling performance of supercapacitor.
引文
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