纳米结构晶态碳基材料可控制备及电化学储能特性研究
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摘要
进入21世纪以来，随着传统能源的日渐耗竭与环境污染的日益严重，新型能源材料及其相应装置的研究已引起全社会的广泛关注。超级电容器作为介于传统电容器和二次电池的一种新型能量储存与转换装置，以其高的比容量、稳定的循环寿命、宽的工作电压视窗和高的功率密度等特点，在便携式仪器、动力混合汽车电源、信息技术等领域具有重要的商业前景和价值。其中，电极材料是影响超级电容器电化学性能最为关键的因素之一。在各种电极材料中，碳材料由于其优异的循环稳定性已被用作电极材料应用在商业电容器中。但传统的碳电极材料（如：活性碳，碳纳米管）低的比电容仍限制了其能量密度的提高。为了提高碳电极材料的比电容，本论文选用不同的碳的前驱体，根据基团相互作用原理设计合成出一系列的具有独特结构的纳米碳材料。本论文主要的研究内容如下：
1.采用溶液-固体路线以葡萄糖为碳源合成出高比表面积多孔晶态纳米碳材料（PGC），并对其电化学性能进行了系统的研究。电化学测试结果表明，PGC样品作为超级电容器电极材料表现出很好的电化学性能。PGC材料优异的电化学特性主要归因于其独特的微观结构。其中，多孔结构有利于电解液离子的传输，而优异的导电性有利于电子在大电流充放电过程中的传递。
2.采用一步水热的方法以氧化石墨和尿素为原材料合成出具有高含氮量的氮掺杂石墨烯（NGS），并对其电化学性能进行了测试。通过一系列实验证实NGS材料的比表面积、氮的含量和类型都可通过改变实验条件来进行调控。当水热温度为180℃、水热时间为12h、氧化石墨与尿素质量比为300:1时制备的NGS材料展示了最好的电容特性。在水系电解液（6M KOH）中，电流密度为0.2A/g时，NGS材料的比电容高达326F/g。经过5000次充放电循环后，NGS材料的比电容为保持初始电容的99.9%。当以NGS材料为电极组装成对称电容器时，在功率密度为7980kW/kg下其能量密度为25.02Wh/kg。在实验过程中，我们发现氮的掺杂类型对NGS材料的电化学性能有很重要的影响。其中，吡啶氮和吡咯氮可与电解液离子发生氧化还原反应产生法拉第准电容；而四元氮可有效的改善材料的导电性从而有利于电子的快速传输。
3.采用配位/热解碳化方法制备出氮掺杂多孔晶态纳米碳材料（NPGC），并研究了不同碳化温度和不同三聚氰胺加入量对NPGC材料微观结构和电容特性的影响。测试结果表明NPGC材料具有大的比表面积、优良的导电性、以及高的氮含量。并且NPGC材料展示了较好的电容特性。在电流密度为1A/g下，比电容值可达到293F/g。经循环5000次后，其比电容仍为初始比电容的99.5%。
4.采用水热配位-ZnCl2活化的路线以生物衍生物壳聚糖为含氮的碳源制备出硼氮分别掺杂的多孔石墨化纳米碳材料（BNGC）。在合成过程中，首先，壳聚糖与Fe3+离子（固氮剂/石墨化催化剂前驱体）进行配位得到壳聚糖-Fe前驱体，随后将硼源加入到壳聚糖-Fe溶液中在180℃进行水热反应，在此过程中，H3BO3转化为B2O3气体，它们与壳聚糖-Fe上剩余的含氧基团进行反应得到分开掺杂的硼、氮碳材料。在经过氯化锌活化和酸处理后，具有大的比表面积、优良的导电性、硼氮的分别掺杂的BNGC样品被合成出来。BNGC样品独特的微观结构和硼氮的分别掺杂使得其具有高的比电容（313F/g，1A/g）、优异的倍率特性、较好的电化学循环稳定性、库伦效率、高的能量密度和功率密度。
5.采用同步ZnCl2活化和石墨化的方法以椰壳为碳源合成了多孔层状晶态纳米碳材料（PNGS）。在合成过程中，首先将石墨催化剂前驱体（FeCl3）和活化剂（ZnCl2）同时引入到椰壳的骨架中形成椰壳-Fe3+复合体。将此复合体经过碳化和去催化剂后，得到PGNS材料。所合成的PGNS样品具有高的比表面积和较好的导电性。当其做为超级电容器电极材料时，展示了优异的电容特性。在水系电解液中，PGNS样品具有高的比电容和优异的电化学循环稳定性。而在有机系电解液中，PGNS样品同样也展示了好的电化学性能：在功率密度为10kW/kg时，PGNS样品能量密度可高达54.7Wh/kg。
With the depletion of the conventional energy sources and the severity of theenvironmental pollution in the twenty-first century, the researches of the new energymaterials and devices have been attracted considerable attentions in whole society. As akind of energy storage and conversion device, supercapacitors, which bridge the gapbetween the traditional capacitors and batteries, have received currently much interestbecause their wide range of applications in as portable electronics, hybrid electricvehicles, and pulsing techniques based on their virtues of the high specific capacitance,reliable cycle life, wide operating voltage, high energy and power density. Electrodematerial is the key that affected the electrochemical performance of supercapacitors.Among various electrode materials, carbon materials are the main electrode materialsfor commercial supercapacitors due to their high cycle stability. However, the lowcapacitance of traditional carbon-based electrode materials (activated carbons andcarbon nanotubes) still limited the improvement of their energy density. According tothe group interaction, we have designed and prepared a series of advanced carbonelectrode materials with special microstructures from different carbon resources forsupercpacitors. The main contents in this paper have been shown as follows:
1. Porous crystalline carbons (PGC) were synthesized via a simple “Solution-Solid”route and their application as advanced electrode materials for supercapacitor were alsodemonstrated. The electrochemical tests prove that the PGC sample shows capacitivebehavior. The outstanding performance of the PGC sample is attributed to its specialmicrostructure. That is, the porous structure and high conductivity are favor forion-charge transport during the high galvanostatic charge-discharge process.
2. An easy and effective one-step hydrothermal process was developed to preparenitrogen-doped grapheme (NGS) by a hydrothermal reaction of GO with urea. A seriesof experiments indicate that the surface area, nitrogen content and type of NGS materials could be controlled by adjusting the experiment conditions. The as-made NGSsample (mass ratio of urea/GO is300:1, hydrothermal temperature:180oC,hydrothermal time:12h) exhibits the best capacitive performance: high capacitance (326F/g,0.2A/g), superior cycling stability (maintaining initial capacity) after2000cycles.Most importantly, in a two-electrode symmetric capacitor, the energy density of25.02Wh/kg should be achieved at power density of7980W/kg. The experimental resultsfurther demonstrated that the types of nitrogen play an important role in the capacitivebehaviors. In detail, the pyridinic-N and pyrrolic-N could provide pseudo-capacitanceby the redox reaction, while quaternary-N could improve the conductivity of the NGSthat is favorable to the electrons transport.
3. Nitrogen-doped porous crystalline carbon (NPGC) was prepared by means of asimple coordination-pyrolysis combination route, the effect of different carbonizedtemperature and different melamine content on the microstructure was also studied. Thetests indicated that the NPGC material has large surface area, well conductivity and highnitrogen content. The unusual structure of NPGC sample endows its superior capacitiveproperty. NPGC-2-900sample has high specific capacitance of293F/g at1A/g. Afterconsecutive5000cycles, the specific capacitance of NPGC-2-900still maintains theinitial capacity.
4. The separated boron and nitrogen co-doping porous graphitic carbon (BNGC) wasfabricated though a hydrothermal coordination-ZnCl2activation process from nitrogen-containing chitosan. In this synthesis, chitosan was first coordinated with Fe3+ions toobtain the chitosan-Fe precursor. Followed by the hydrothermal reaction, H3BO3wasconverted into B2O3steam, which reacts with residual oxygen groups of chitosan-Fe.After that, the boron atoms doped into the skeleton of to get the separated B and Nco-doping polymerized carbon. After ZnCl2activation and removal of Fe catalyst withhydrochloric acid, the BNGC with high surface area was synthesized. Benefiting fromthe structure of BNGC samples and isolated boron and nitrogen co-doping, the BNGC sample exhibits high specific capacitance (313F/g,1A/g), well electrochemicalstability, high coulombic efficiency, high energy and power densities.
5. The porous layered crystalline nanocarbon (PGNS) has been synthesized throughan effective simultaneous activation-graphitization route by using a renewable andinexpensive coconut shell. In the preparation, the graphitization catalyst precursor(FeCl3) and activating agent (ZnCl2) are simultaneously introduced into the frameworkof the coconut shell to get the coconut shell-Fe precursor. Following pyrolysis andremoval of the catalyst, the PGNS material obtained. The as-prepared PNGS sample hashigh surface area and well conductivity. The PNGS exhibits excellent capacitivebehavior. In aqueous electrolyte, PNGS sample has high specific capacitance, superiorcycle durability and Coulombic efficiency. Remarkably, in an organic electrolyte, PGNSalso shows outstanding electrochemical performance: an energy density of up to54.7Wh/kg can be achieved at a high power density of10kW/kg.
1.采用溶液-固体路线以葡萄糖为碳源合成出高比表面积多孔晶态纳米碳材料（PGC），并对其电化学性能进行了系统的研究。电化学测试结果表明，PGC样品作为超级电容器电极材料表现出很好的电化学性能。PGC材料优异的电化学特性主要归因于其独特的微观结构。其中，多孔结构有利于电解液离子的传输，而优异的导电性有利于电子在大电流充放电过程中的传递。
2.采用一步水热的方法以氧化石墨和尿素为原材料合成出具有高含氮量的氮掺杂石墨烯（NGS），并对其电化学性能进行了测试。通过一系列实验证实NGS材料的比表面积、氮的含量和类型都可通过改变实验条件来进行调控。当水热温度为180℃、水热时间为12h、氧化石墨与尿素质量比为300:1时制备的NGS材料展示了最好的电容特性。在水系电解液（6M KOH）中，电流密度为0.2A/g时，NGS材料的比电容高达326F/g。经过5000次充放电循环后，NGS材料的比电容为保持初始电容的99.9%。当以NGS材料为电极组装成对称电容器时，在功率密度为7980kW/kg下其能量密度为25.02Wh/kg。在实验过程中，我们发现氮的掺杂类型对NGS材料的电化学性能有很重要的影响。其中，吡啶氮和吡咯氮可与电解液离子发生氧化还原反应产生法拉第准电容；而四元氮可有效的改善材料的导电性从而有利于电子的快速传输。
3.采用配位/热解碳化方法制备出氮掺杂多孔晶态纳米碳材料（NPGC），并研究了不同碳化温度和不同三聚氰胺加入量对NPGC材料微观结构和电容特性的影响。测试结果表明NPGC材料具有大的比表面积、优良的导电性、以及高的氮含量。并且NPGC材料展示了较好的电容特性。在电流密度为1A/g下，比电容值可达到293F/g。经循环5000次后，其比电容仍为初始比电容的99.5%。
4.采用水热配位-ZnCl2活化的路线以生物衍生物壳聚糖为含氮的碳源制备出硼氮分别掺杂的多孔石墨化纳米碳材料（BNGC）。在合成过程中，首先，壳聚糖与Fe3+离子（固氮剂/石墨化催化剂前驱体）进行配位得到壳聚糖-Fe前驱体，随后将硼源加入到壳聚糖-Fe溶液中在180℃进行水热反应，在此过程中，H3BO3转化为B2O3气体，它们与壳聚糖-Fe上剩余的含氧基团进行反应得到分开掺杂的硼、氮碳材料。在经过氯化锌活化和酸处理后，具有大的比表面积、优良的导电性、硼氮的分别掺杂的BNGC样品被合成出来。BNGC样品独特的微观结构和硼氮的分别掺杂使得其具有高的比电容（313F/g，1A/g）、优异的倍率特性、较好的电化学循环稳定性、库伦效率、高的能量密度和功率密度。
5.采用同步ZnCl2活化和石墨化的方法以椰壳为碳源合成了多孔层状晶态纳米碳材料（PNGS）。在合成过程中，首先将石墨催化剂前驱体（FeCl3）和活化剂（ZnCl2）同时引入到椰壳的骨架中形成椰壳-Fe3+复合体。将此复合体经过碳化和去催化剂后，得到PGNS材料。所合成的PGNS样品具有高的比表面积和较好的导电性。当其做为超级电容器电极材料时，展示了优异的电容特性。在水系电解液中，PGNS样品具有高的比电容和优异的电化学循环稳定性。而在有机系电解液中，PGNS样品同样也展示了好的电化学性能：在功率密度为10kW/kg时，PGNS样品能量密度可高达54.7Wh/kg。
With the depletion of the conventional energy sources and the severity of theenvironmental pollution in the twenty-first century, the researches of the new energymaterials and devices have been attracted considerable attentions in whole society. As akind of energy storage and conversion device, supercapacitors, which bridge the gapbetween the traditional capacitors and batteries, have received currently much interestbecause their wide range of applications in as portable electronics, hybrid electricvehicles, and pulsing techniques based on their virtues of the high specific capacitance,reliable cycle life, wide operating voltage, high energy and power density. Electrodematerial is the key that affected the electrochemical performance of supercapacitors.Among various electrode materials, carbon materials are the main electrode materialsfor commercial supercapacitors due to their high cycle stability. However, the lowcapacitance of traditional carbon-based electrode materials (activated carbons andcarbon nanotubes) still limited the improvement of their energy density. According tothe group interaction, we have designed and prepared a series of advanced carbonelectrode materials with special microstructures from different carbon resources forsupercpacitors. The main contents in this paper have been shown as follows:
1. Porous crystalline carbons (PGC) were synthesized via a simple “Solution-Solid”route and their application as advanced electrode materials for supercapacitor were alsodemonstrated. The electrochemical tests prove that the PGC sample shows capacitivebehavior. The outstanding performance of the PGC sample is attributed to its specialmicrostructure. That is, the porous structure and high conductivity are favor forion-charge transport during the high galvanostatic charge-discharge process.
2. An easy and effective one-step hydrothermal process was developed to preparenitrogen-doped grapheme (NGS) by a hydrothermal reaction of GO with urea. A seriesof experiments indicate that the surface area, nitrogen content and type of NGS materials could be controlled by adjusting the experiment conditions. The as-made NGSsample (mass ratio of urea/GO is300:1, hydrothermal temperature:180oC,hydrothermal time:12h) exhibits the best capacitive performance: high capacitance (326F/g,0.2A/g), superior cycling stability (maintaining initial capacity) after2000cycles.Most importantly, in a two-electrode symmetric capacitor, the energy density of25.02Wh/kg should be achieved at power density of7980W/kg. The experimental resultsfurther demonstrated that the types of nitrogen play an important role in the capacitivebehaviors. In detail, the pyridinic-N and pyrrolic-N could provide pseudo-capacitanceby the redox reaction, while quaternary-N could improve the conductivity of the NGSthat is favorable to the electrons transport.
3. Nitrogen-doped porous crystalline carbon (NPGC) was prepared by means of asimple coordination-pyrolysis combination route, the effect of different carbonizedtemperature and different melamine content on the microstructure was also studied. Thetests indicated that the NPGC material has large surface area, well conductivity and highnitrogen content. The unusual structure of NPGC sample endows its superior capacitiveproperty. NPGC-2-900sample has high specific capacitance of293F/g at1A/g. Afterconsecutive5000cycles, the specific capacitance of NPGC-2-900still maintains theinitial capacity.
4. The separated boron and nitrogen co-doping porous graphitic carbon (BNGC) wasfabricated though a hydrothermal coordination-ZnCl2activation process from nitrogen-containing chitosan. In this synthesis, chitosan was first coordinated with Fe3+ions toobtain the chitosan-Fe precursor. Followed by the hydrothermal reaction, H3BO3wasconverted into B2O3steam, which reacts with residual oxygen groups of chitosan-Fe.After that, the boron atoms doped into the skeleton of to get the separated B and Nco-doping polymerized carbon. After ZnCl2activation and removal of Fe catalyst withhydrochloric acid, the BNGC with high surface area was synthesized. Benefiting fromthe structure of BNGC samples and isolated boron and nitrogen co-doping, the BNGC sample exhibits high specific capacitance (313F/g,1A/g), well electrochemicalstability, high coulombic efficiency, high energy and power densities.
5. The porous layered crystalline nanocarbon (PGNS) has been synthesized throughan effective simultaneous activation-graphitization route by using a renewable andinexpensive coconut shell. In the preparation, the graphitization catalyst precursor(FeCl3) and activating agent (ZnCl2) are simultaneously introduced into the frameworkof the coconut shell to get the coconut shell-Fe precursor. Following pyrolysis andremoval of the catalyst, the PGNS material obtained. The as-prepared PNGS sample hashigh surface area and well conductivity. The PNGS exhibits excellent capacitivebehavior. In aqueous electrolyte, PNGS sample has high specific capacitance, superiorcycle durability and Coulombic efficiency. Remarkably, in an organic electrolyte, PGNSalso shows outstanding electrochemical performance: an energy density of up to54.7Wh/kg can be achieved at a high power density of10kW/kg.
引文
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