过渡金属氧化物微纳结构的构筑及电化学性能研究
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摘要
随着日益加深的能源危机和环境问题以及风能、太阳能产生的电能需高效储存的要求,发展高效、廉价和环境友好的储能装置是各国科学家面对的重要的挑战和机遇。锂离子电池和超级电容器在我们日常生活所用的电子设备以及电动工具中都发挥着重要的作用,是目前的热点研究领域。过渡金属氧化物材料由于具有比传统碳／石墨基材料高2-3倍的比容量／电容,是锂离子电池和超级电容器中很有前途的电极材料。但是,目前两种储能器件的循环性能和倍率性能依然无法满足实际需要。因此,提高它们的性能,尤其是发展更好的电极材料是非常紧迫的任务。金属氧化物材料由于具有较好的电化学性能、容易合成等优点一直以来被看做是超级电容器和锂离子电池潜在的电极材料。但是,氧化物电极材料有电子电导率较差、循环过程中容易团聚和电解液副反应多等缺点,限制其应用。研究发现纳米化技术对金属氧化物电极材料性能提升很有帮助,因此发展和设计具有更高性能的纳米电极材料并将其应用到电化学储能设备中是非常有必要的。
在本论文中,我们旨在利用简单的方法构筑高性能的锂离子电池和超级电容器纳米电极材料。本论文的主要内容如下：
(1)利用尿素和镍盐为原料通过简单的水热法合成了α-Ni(OH)2材料,其中尿素可以提供氢氧根离子并且有利于超细纳米线／纳米片自组装为网状结构。通过检测不同反应时间段的中间产物来详细研究了形貌演变的过程。改变反应参数,如投料比等,可以实现对α-Ni(OH)2的形貌很好的调控。经过在空气氛围中煅烧后,α-Ni(OH)2经过拓扑转变得到了不同形貌的由超细纳米线或纳米片自组装而成的多孔NiO微米球。对比多种形貌的NiO的电化学性能研究表明,调控其表面结构和孔径分布对超级电容器的性能有很明显的影响。其中,由超细纳米线自组装的多孔网状NiO微球具有最好的电化学性能,在10A/g电流密度下循环2000圈容量保持率高达97%。
(2)采用一种简单、温和的反应路线成功地合成了花状α-Ni(OH)2前驱体材料,通过后续热处理前驱体制备了具有规则形貌和较高比表面积的由超薄纳米片组成的花状NiO多孔材料。详细研究发现溶剂乙二醇与水的体积比对前驱体的形貌有重要影响。将得到的多孔NiO纳米花应用到超级电容器材料中,该样品的比容量为335F/g,在电流密度10A/g下循环1500圈后容量保持率为91%。
(3)首次通过简单、新颖的设计路线合成了具有骨节状特征的多晶MnO@碳同轴纳米线。该核壳结构由方向高度一致的MnO纳米短棒相连接而成,石墨化的碳层均匀的包覆在MnO的外面。通过对比分析前驱体MnOOH, Mn2O3以及最终产物MnO@C的晶体结构,我们提出了从前驱体到最终产物的连续拓扑转变机理。锂离子电池测试表明MnO@碳同轴纳米线具有较高的比容量、优异的循环稳定性和倍率性能。具体来说,该电极材料在500mA/g电流密度下经过200次循环可逆比容量达到801mAh/g。该材料具有优异电化学性能的原因可以归结为：MnO纳米线外面高度均匀的碳包覆层不但可以有效地缓解不断充放电过程中的体积变化产生的应力,还可以显著地提高电极材料的电子导电率。
(4)利用简单的微乳液的方法合成了锌钴化合物前驱体,经过煅烧得到了形貌可保持的由纳米片堆积而成的ZnCo2O4多级结构。纳米片的厚度在10-20nm之间,并互相交错构成三维结构。ZnCo2O4多级结构用作锂离子电池负极材料时显示了非常高的可逆容量和好的循环性能。在100mA/g电流密度下,经过100次循环可逆比容量为930mAh/g。其良好的电化学性能是由于ZnCo2O4纳米片组装成的多级结构可以为锂离子的传输提供较短的路径,具有充足的空间来缓解材料在充放电过程中巨大的体积膨胀。
(5)利用简单的水热反应在无任何模板加入的条件下合成了海胆状的NiCo2O4纳米结构。合成的NiCo2O4直径约5gm,由无数短棒沿径向从中心生长而成,纳米棒的直径在100-200nm之间。把得到的NiCo2O4第一次应用到无酶葡萄糖检测中,结果显示该材料具有较低的检测限、小于1秒的响应时间和较宽的检测范围。NiCo2O4材料被证明具有应用到检测实际样品的前景。
One of the major challenges researchers are facing today is to provide highly efficient, low cost, and environmentally benign electrical energy storage devices to address the problems of climate, the impending exhaustion of fossil fuels and the need for efficient storage of energy produced by solar and wind power. Lithium ion batteries (LIBs) and supercapacitors are at the frontier of this research effort, as they play important roles in our daily life by powering portable consumer electronic devices and even electric vehicles. Transition metal oxide materials are promising electrode materials for lithium ion batteries and supercapacitors because of their high specific capacity/capacitance, typically2-3times higher than that of the carbon/graphite based materials. However, their cycling stability and rate performance still can not meet the requirements of practical applications. It is therefore urgent to improve their overall performance, which depends on the development of the advanced electrode architectures. Metal oxide materials have long been studied as potential electrode materials for LIBs and psedocapacitors due to the ease of large-scale fabrication and high electrochemical activity. However, metal oxide electrodes also have some drawbacks, such as poor electronic conductivity, easy aggregation during cycling, side reaction with the electrolyte, etc. It is reported that nanoscale materials can greatly increase the performance of the metal oxide electrodes. Therefore, numerous efforts are urgently required to design advanced electrode nanostructures with high performance in the application of electrochemical energy storage devices.
In this paper, we aim at utlizing simple methods to design nanostructured electrode materials with high performance for the LIBs and psedocapacitors. The main results are as follows:
(1) We use a novel hydrothermal route to synthesize α-Ni(OH)2, in which urea has been utilized not only to produce hydroxyl anions, but also to organize ultrathin nanowires/nanosheets into network-like hierarchical assemblage. The morphological evolution process of this organized product has been investigated by examining different reaction intermediates during the synthesis. The growth and thus final assemblage of a-Ni(OH)2can be finely tuned by selecting preparative parameters, such as the molar ratio of starting chemicals. Based on the toptactic transformation from α-Ni(OH)2, various mesoporous NiO hierarchical microspheres by ultrathin nanowires/nanosheets self-assembly have been prepared via thermal decomposition in air atmosphere. The electrochemical performances of the typical nickel oxide products are evaluated. It is demonstrated that tuning of the surface texture and the pore size of the NiO products is very significant in electrochemical capacitor. Mesoporous NiO network-like hierarchical microspheres exhibit excellent cyclic performance with a97%capacity retention at current density of10A/g in a testing range of2000cycles.
(2) Porous NiO nanoflowers with uniform morphology and high surface area have been obtained by annealing precursor synthesized by a facile solvothermal method. The results show that the ratio of ethylene glycol and water has an important impact on the morphology of the precursor. After heat treatment, the as-prepared NiO nanoflowers are applied as the electrode material for supercapaciors, and the sample exhibits superior performance with a high specific capacitance of335F/g and91%capacity retention at current density of10A/g after1500cycles.
(3) A facile method is designed for large-scale preparation of joint-like mesocrystalline MnO@carbon core-shell nanowires for the first time based on rational constructed functional systems. The nanostructures present the unique feature of the highly oriented-interconnected of MnO nanorods encapsulated inside and graphitized carbon layers coating outside. Through comparing and analyzing the MnOOH, Mn2O3and MnO@C crystal structures, the sequential topotactic transformation of the corresponding precursors to targets is proposed here. Li-ion battery testing is given to demonstrate that MnO@carbon core-shell nanowires show excellent capacity retention, superior cycling performance and high rate capability. Specifically, the MnO@carbon core-shell nanostructure could deliver reversible capacity as high as801mAh g-1at a high current density of500mA g-1with excellent electrochemical stability after200cycles testing. The remarkable electrochemical performance is mainly attributed to the highly uniform carbon layer around the MnO nanowires which can not only effectively buffer the structural strain and volume variations of anodes during the repeated electrochemical reactions, but also greatly enhance the conductivity of electrode materials.
(4) A simple microemulsion based method has been developed to synthesize ZnCo2O4hierarchical superstructure stacked by nanoplates, which was transformed from corresponding precursor by annealing process. The nanoplates shown a thickness of10-20nm were connected together to form well assembled three-dimension structure. When applied as anode material of lithium ion battery, ZnCo2O4hierarchical superstructure demonstrated high reversible capacity and good rcyclability. The ZnCo2O4hierarchical superstructure could deliver reversible capacity as high as930mAh g-1at a current density of100mA g-1with excellent electrochemical stability after100cycles testing. The improved electrochemical performance of the as-synthesized ZnCo2O4nanoplates might benefit from its unique hierarchical superstructure, which provides a short path for Li+ion diffusion, and enough free space to buffer the large volume changed during cycling.
(5) Urchin-like hierarchical NiCo2O4nanostructure has been synthesized by a simple hydrothermal method free of any template. As-synthesized NiCo2O4has a uniform diameter of5μm with numerous small nanorods radially grown from the center. Typical nanorods have a diameter of100-200nm. The NiCo2O4+was first investigated on the application of nonenzymatic glucose detection, demostrating a rather low detection limit, a fast responsible time less than1second and a wide detection range for the electrochemical detection of glucose. It is expected to have potential application in real sample analysis.
在本论文中,我们旨在利用简单的方法构筑高性能的锂离子电池和超级电容器纳米电极材料。本论文的主要内容如下：
(1)利用尿素和镍盐为原料通过简单的水热法合成了α-Ni(OH)2材料,其中尿素可以提供氢氧根离子并且有利于超细纳米线／纳米片自组装为网状结构。通过检测不同反应时间段的中间产物来详细研究了形貌演变的过程。改变反应参数,如投料比等,可以实现对α-Ni(OH)2的形貌很好的调控。经过在空气氛围中煅烧后,α-Ni(OH)2经过拓扑转变得到了不同形貌的由超细纳米线或纳米片自组装而成的多孔NiO微米球。对比多种形貌的NiO的电化学性能研究表明,调控其表面结构和孔径分布对超级电容器的性能有很明显的影响。其中,由超细纳米线自组装的多孔网状NiO微球具有最好的电化学性能,在10A/g电流密度下循环2000圈容量保持率高达97%。
(2)采用一种简单、温和的反应路线成功地合成了花状α-Ni(OH)2前驱体材料,通过后续热处理前驱体制备了具有规则形貌和较高比表面积的由超薄纳米片组成的花状NiO多孔材料。详细研究发现溶剂乙二醇与水的体积比对前驱体的形貌有重要影响。将得到的多孔NiO纳米花应用到超级电容器材料中,该样品的比容量为335F/g,在电流密度10A/g下循环1500圈后容量保持率为91%。
(3)首次通过简单、新颖的设计路线合成了具有骨节状特征的多晶MnO@碳同轴纳米线。该核壳结构由方向高度一致的MnO纳米短棒相连接而成,石墨化的碳层均匀的包覆在MnO的外面。通过对比分析前驱体MnOOH, Mn2O3以及最终产物MnO@C的晶体结构,我们提出了从前驱体到最终产物的连续拓扑转变机理。锂离子电池测试表明MnO@碳同轴纳米线具有较高的比容量、优异的循环稳定性和倍率性能。具体来说,该电极材料在500mA/g电流密度下经过200次循环可逆比容量达到801mAh/g。该材料具有优异电化学性能的原因可以归结为：MnO纳米线外面高度均匀的碳包覆层不但可以有效地缓解不断充放电过程中的体积变化产生的应力,还可以显著地提高电极材料的电子导电率。
(4)利用简单的微乳液的方法合成了锌钴化合物前驱体,经过煅烧得到了形貌可保持的由纳米片堆积而成的ZnCo2O4多级结构。纳米片的厚度在10-20nm之间,并互相交错构成三维结构。ZnCo2O4多级结构用作锂离子电池负极材料时显示了非常高的可逆容量和好的循环性能。在100mA/g电流密度下,经过100次循环可逆比容量为930mAh/g。其良好的电化学性能是由于ZnCo2O4纳米片组装成的多级结构可以为锂离子的传输提供较短的路径,具有充足的空间来缓解材料在充放电过程中巨大的体积膨胀。
(5)利用简单的水热反应在无任何模板加入的条件下合成了海胆状的NiCo2O4纳米结构。合成的NiCo2O4直径约5gm,由无数短棒沿径向从中心生长而成,纳米棒的直径在100-200nm之间。把得到的NiCo2O4第一次应用到无酶葡萄糖检测中,结果显示该材料具有较低的检测限、小于1秒的响应时间和较宽的检测范围。NiCo2O4材料被证明具有应用到检测实际样品的前景。
One of the major challenges researchers are facing today is to provide highly efficient, low cost, and environmentally benign electrical energy storage devices to address the problems of climate, the impending exhaustion of fossil fuels and the need for efficient storage of energy produced by solar and wind power. Lithium ion batteries (LIBs) and supercapacitors are at the frontier of this research effort, as they play important roles in our daily life by powering portable consumer electronic devices and even electric vehicles. Transition metal oxide materials are promising electrode materials for lithium ion batteries and supercapacitors because of their high specific capacity/capacitance, typically2-3times higher than that of the carbon/graphite based materials. However, their cycling stability and rate performance still can not meet the requirements of practical applications. It is therefore urgent to improve their overall performance, which depends on the development of the advanced electrode architectures. Metal oxide materials have long been studied as potential electrode materials for LIBs and psedocapacitors due to the ease of large-scale fabrication and high electrochemical activity. However, metal oxide electrodes also have some drawbacks, such as poor electronic conductivity, easy aggregation during cycling, side reaction with the electrolyte, etc. It is reported that nanoscale materials can greatly increase the performance of the metal oxide electrodes. Therefore, numerous efforts are urgently required to design advanced electrode nanostructures with high performance in the application of electrochemical energy storage devices.
In this paper, we aim at utlizing simple methods to design nanostructured electrode materials with high performance for the LIBs and psedocapacitors. The main results are as follows:
(1) We use a novel hydrothermal route to synthesize α-Ni(OH)2, in which urea has been utilized not only to produce hydroxyl anions, but also to organize ultrathin nanowires/nanosheets into network-like hierarchical assemblage. The morphological evolution process of this organized product has been investigated by examining different reaction intermediates during the synthesis. The growth and thus final assemblage of a-Ni(OH)2can be finely tuned by selecting preparative parameters, such as the molar ratio of starting chemicals. Based on the toptactic transformation from α-Ni(OH)2, various mesoporous NiO hierarchical microspheres by ultrathin nanowires/nanosheets self-assembly have been prepared via thermal decomposition in air atmosphere. The electrochemical performances of the typical nickel oxide products are evaluated. It is demonstrated that tuning of the surface texture and the pore size of the NiO products is very significant in electrochemical capacitor. Mesoporous NiO network-like hierarchical microspheres exhibit excellent cyclic performance with a97%capacity retention at current density of10A/g in a testing range of2000cycles.
(2) Porous NiO nanoflowers with uniform morphology and high surface area have been obtained by annealing precursor synthesized by a facile solvothermal method. The results show that the ratio of ethylene glycol and water has an important impact on the morphology of the precursor. After heat treatment, the as-prepared NiO nanoflowers are applied as the electrode material for supercapaciors, and the sample exhibits superior performance with a high specific capacitance of335F/g and91%capacity retention at current density of10A/g after1500cycles.
(3) A facile method is designed for large-scale preparation of joint-like mesocrystalline MnO@carbon core-shell nanowires for the first time based on rational constructed functional systems. The nanostructures present the unique feature of the highly oriented-interconnected of MnO nanorods encapsulated inside and graphitized carbon layers coating outside. Through comparing and analyzing the MnOOH, Mn2O3and MnO@C crystal structures, the sequential topotactic transformation of the corresponding precursors to targets is proposed here. Li-ion battery testing is given to demonstrate that MnO@carbon core-shell nanowires show excellent capacity retention, superior cycling performance and high rate capability. Specifically, the MnO@carbon core-shell nanostructure could deliver reversible capacity as high as801mAh g-1at a high current density of500mA g-1with excellent electrochemical stability after200cycles testing. The remarkable electrochemical performance is mainly attributed to the highly uniform carbon layer around the MnO nanowires which can not only effectively buffer the structural strain and volume variations of anodes during the repeated electrochemical reactions, but also greatly enhance the conductivity of electrode materials.
(4) A simple microemulsion based method has been developed to synthesize ZnCo2O4hierarchical superstructure stacked by nanoplates, which was transformed from corresponding precursor by annealing process. The nanoplates shown a thickness of10-20nm were connected together to form well assembled three-dimension structure. When applied as anode material of lithium ion battery, ZnCo2O4hierarchical superstructure demonstrated high reversible capacity and good rcyclability. The ZnCo2O4hierarchical superstructure could deliver reversible capacity as high as930mAh g-1at a current density of100mA g-1with excellent electrochemical stability after100cycles testing. The improved electrochemical performance of the as-synthesized ZnCo2O4nanoplates might benefit from its unique hierarchical superstructure, which provides a short path for Li+ion diffusion, and enough free space to buffer the large volume changed during cycling.
(5) Urchin-like hierarchical NiCo2O4nanostructure has been synthesized by a simple hydrothermal method free of any template. As-synthesized NiCo2O4has a uniform diameter of5μm with numerous small nanorods radially grown from the center. Typical nanorods have a diameter of100-200nm. The NiCo2O4+was first investigated on the application of nonenzymatic glucose detection, demostrating a rather low detection limit, a fast responsible time less than1second and a wide detection range for the electrochemical detection of glucose. It is expected to have potential application in real sample analysis.
引文
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[I]Poizot, P.; Laruelle, S.; Grugeon, S.; Dupont, L.; Tarascon, J. M., Nano-sized transition-metaloxides as negative-electrode materials for lithium-ion batteries. Nature 2000,407 (6803),496-9.
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[1]Pradhan, D.; Niroui, E.; Leung, K. T., High-Performance, Flexible Enzymatic Glucose Biosensor Based on ZnO Nanowires Supported on a Gold-Coated Polyester Substrate. Acs Applied Materials & Interfaces 2010,2 (8),2409-12.
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