硫化铜及钒基化合物的溶剂热合成及锂离子电池性能研究
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摘要
二十一世纪日益严重的能源、环境危机使人们对于能源的生产和转换提出了更高的需求。纳米材料由于其高选择性和高效性,成为能源生产和转换材料的首选.如选择纳米材料作为锂离子电池的电极材料,已然成为一个极受关注的研究课题。本文旨在利用溶剂热合成的纳米材料具有结晶性好、纯度高、颗粒团聚少等优点,控制合成不同形貌的过渡金属氧化物、硫化物,如三维的纳米/微米复合结构,二维类似与石墨烯结构的超薄纳米片；讨论了温度、时间等对产物形貌、组成的影响；根据材料本身的特征,研究其在锂离子电池中的电化学行为：并初步讨论不同的形貌结构对材料性能的影响。本论文的主要内容可归纳如下：
1.利用简单的乙醇-水体系,未添加任何表面活性剂,混合溶剂热条件下得到了由厚10nm的片交叉生长成的直径约为200-300nm的CuS纳米微球。通过发光性能的研究,发现量子效应作用导致光致发光及紫外可见吸收光谱的峰位置普遍发生蓝移。同时对硫化铜CuS纳米微球进行了锂电性能的测试,发现其存在两个稳定的放电平台。首次对其进行了水相锂电性能的测试,发现它存在一个放电平台处于水溶液的电化学稳定窗口内,是一种潜在的水溶液锂离子电池的负极材料。
2.用简单的低温溶剂热法合成了由大小400nm的纳米立方块组成的乙二醇钒微米球。在乙二醇溶液中,研究了温度对于其价态和形貌的影响,发现随着温度的升高,经历了由四价的球状乙二醇钒向五价片花状(NH4)2V6O16的转变。首次研究了乙二醇钒的电化学性能,发现在60mA/g电流密度下,其首次放电容量可达1826mAh/g,即使在200次循环之后,容量仍可以保持在477mAh/g,表现出较高的放电容量和优良的循环性能,使之有望应用于锂离子电池。并通过“自上而下”热转化法得到不同形貌的V2O3微纳结构也是一种潜在的锂离子电极材料。
3.以乙醇作为溶剂,不需要任何模板和表面活性剂,利用前驱物热分解的方法控制合成得类似石墨烯厚度的超薄V2O3纳米片。通过测试其电阻和温度的相互关系,发现原本在0-300K存在一级相变的V2O3并没有出现,这种V203极薄的纳米片具有良好的导电性,可能是一种很好的柔性电极材料。通过调节反应的温度、时间,控制合成由厚度不同的纳米片组成的大小和致密程度皆不同的三维片花球状的前驱物。分别在氩气和含10%乙炔气的氩气中退火,可得到主体形貌维持不变的V2O3及V2O3/C微纳结构。通过对比V2O3超薄片、三维片花及其各自的碳包覆材料在锂离子电池中的电化学性质,发现三维花球的V2O3/C微纳结构在0-3V的电压范围内,200mA/g的电流密度下,80次循环过后,仍可保持360mAh/g的放电容量,显示了优异的放电容量和稳定的循环性能。
4.利用简单的溶剂热,在300℃使用六氯-1.3-丁二烯和金属钠为原料,在聚乙二醇600辅助作用下,一步合成得到1-3层的石墨烯片。
The increasingly serious crises of the energy and environment in the21st century make people have a higher demand on the production and conversion of energy. Due to its high selectivity and high efficiency, nanomaterial is one of the most optimal choices. For example, choosing nanomaterial as the electrode material in the lithium ion battery has become a very popular research subject in the whole world. As we all know, the products of solvothermal synthesis method have a lot of unique merits such as high crystallinity, high purity, less aggregation and so on. The goal of this dissertation is to synthesis transition metal oxides and sulfides with different morphologies controllably, such as3D micro-nanostructures and2D graphene-like structures. According to the characteristics of material itself, we discuss the influences of temperature and time on the morphologies and compositions of these micro-nanostructures, study their electrochemical behaviors in the lithium ion battery, in the further, contrast the properties of materials having different morphologies. The main points are summarized briefly as follows:
1. We successfully synthesized monodispersed CuS nanospheres with a diameter of about200nm consisted of nanoplates with the thickness of10nm by a hydro/solovthermal strategy without any surfactant. The PL and UV-Vis absorption spectrums both exhibit some degree blue shift attributed to the quantum confinement of the CuS nanoplates. The electrochemical performances of CuS nanospheres were studied both in organic and aqueous lithium-ion batteries. There have two discharging platforms, one of which is in the window of aqueous solution on the electrochemical reaction. It may be a promising candidate of cathode material in aqueous lithium-ion batteries.
2. Vanadyl ethylene glycolate (VEG) spherical microstructures composed of nanocube-based with an average diameter of-400nm were solvothermally prepared at180℃. The influence of temperature in solvothermal process was investigated. When the temperature rised to250℃, the products transformed from VEG (IV) spheres to (NH4)2V6O16(V) flakes.The electrochemical properties of vanadyl ethylene glycolate in rechargeable lithium batteries were firstly investigated. At a current density of60mA/g the initial specific discharge capacity is1826mA/g and even after200cycles the discharge capacity is still maintained at477mA/g,which exbits high discharge capacity and good cycling stability. V2O3with different morphologies were also prepared by a simple top-down precursor-pyrolyzation strategy, which is also a promising electrode material in lithium-ion batteries.
3. Without any surfactant, V2O3graphene-like structures by the top-down precursor-pyrolyzation strategy had been synthesized controllably. Interestingly enough, these ultrathin V2O3nanosheets which should exist temperature-induced reversible metal insulator transition represents a brand new two-dimensional material having metallic behavior. Meanwhile, we successfully realized controllable synthesis of3D flower-like structure precursor composed of nanaosheets having different diameter, packing density, and thickness of nanosheets by adjusting temperature and time. Using different gases, the V2O3and V2O3/C with the perfect inheritance of the morphology of their precursors were prepared by top-down precursor-pyrolyzation strategy. Compared with the V2O32D ultrathin sheets,3D flower-like structures and their composites with carbon coating, at the current density of200mA/g, the discharge capacity of V2O3/C3D flower-like micro-nanostructures is still maintained at360mAh/g after80cycles, which exbits excellent discharge capacity and superior cycling stability.
4. Graphene nanosheets (1-3graphite layers)had been solvothermally synthesized through reducing hexachloro-1,3-butadiene (C4Cl6) by Metallic sodium in polyethylene glycol (PEG-600) at300℃
1.利用简单的乙醇-水体系,未添加任何表面活性剂,混合溶剂热条件下得到了由厚10nm的片交叉生长成的直径约为200-300nm的CuS纳米微球。通过发光性能的研究,发现量子效应作用导致光致发光及紫外可见吸收光谱的峰位置普遍发生蓝移。同时对硫化铜CuS纳米微球进行了锂电性能的测试,发现其存在两个稳定的放电平台。首次对其进行了水相锂电性能的测试,发现它存在一个放电平台处于水溶液的电化学稳定窗口内,是一种潜在的水溶液锂离子电池的负极材料。
2.用简单的低温溶剂热法合成了由大小400nm的纳米立方块组成的乙二醇钒微米球。在乙二醇溶液中,研究了温度对于其价态和形貌的影响,发现随着温度的升高,经历了由四价的球状乙二醇钒向五价片花状(NH4)2V6O16的转变。首次研究了乙二醇钒的电化学性能,发现在60mA/g电流密度下,其首次放电容量可达1826mAh/g,即使在200次循环之后,容量仍可以保持在477mAh/g,表现出较高的放电容量和优良的循环性能,使之有望应用于锂离子电池。并通过“自上而下”热转化法得到不同形貌的V2O3微纳结构也是一种潜在的锂离子电极材料。
3.以乙醇作为溶剂,不需要任何模板和表面活性剂,利用前驱物热分解的方法控制合成得类似石墨烯厚度的超薄V2O3纳米片。通过测试其电阻和温度的相互关系,发现原本在0-300K存在一级相变的V2O3并没有出现,这种V203极薄的纳米片具有良好的导电性,可能是一种很好的柔性电极材料。通过调节反应的温度、时间,控制合成由厚度不同的纳米片组成的大小和致密程度皆不同的三维片花球状的前驱物。分别在氩气和含10%乙炔气的氩气中退火,可得到主体形貌维持不变的V2O3及V2O3/C微纳结构。通过对比V2O3超薄片、三维片花及其各自的碳包覆材料在锂离子电池中的电化学性质,发现三维花球的V2O3/C微纳结构在0-3V的电压范围内,200mA/g的电流密度下,80次循环过后,仍可保持360mAh/g的放电容量,显示了优异的放电容量和稳定的循环性能。
4.利用简单的溶剂热,在300℃使用六氯-1.3-丁二烯和金属钠为原料,在聚乙二醇600辅助作用下,一步合成得到1-3层的石墨烯片。
The increasingly serious crises of the energy and environment in the21st century make people have a higher demand on the production and conversion of energy. Due to its high selectivity and high efficiency, nanomaterial is one of the most optimal choices. For example, choosing nanomaterial as the electrode material in the lithium ion battery has become a very popular research subject in the whole world. As we all know, the products of solvothermal synthesis method have a lot of unique merits such as high crystallinity, high purity, less aggregation and so on. The goal of this dissertation is to synthesis transition metal oxides and sulfides with different morphologies controllably, such as3D micro-nanostructures and2D graphene-like structures. According to the characteristics of material itself, we discuss the influences of temperature and time on the morphologies and compositions of these micro-nanostructures, study their electrochemical behaviors in the lithium ion battery, in the further, contrast the properties of materials having different morphologies. The main points are summarized briefly as follows:
1. We successfully synthesized monodispersed CuS nanospheres with a diameter of about200nm consisted of nanoplates with the thickness of10nm by a hydro/solovthermal strategy without any surfactant. The PL and UV-Vis absorption spectrums both exhibit some degree blue shift attributed to the quantum confinement of the CuS nanoplates. The electrochemical performances of CuS nanospheres were studied both in organic and aqueous lithium-ion batteries. There have two discharging platforms, one of which is in the window of aqueous solution on the electrochemical reaction. It may be a promising candidate of cathode material in aqueous lithium-ion batteries.
2. Vanadyl ethylene glycolate (VEG) spherical microstructures composed of nanocube-based with an average diameter of-400nm were solvothermally prepared at180℃. The influence of temperature in solvothermal process was investigated. When the temperature rised to250℃, the products transformed from VEG (IV) spheres to (NH4)2V6O16(V) flakes.The electrochemical properties of vanadyl ethylene glycolate in rechargeable lithium batteries were firstly investigated. At a current density of60mA/g the initial specific discharge capacity is1826mA/g and even after200cycles the discharge capacity is still maintained at477mA/g,which exbits high discharge capacity and good cycling stability. V2O3with different morphologies were also prepared by a simple top-down precursor-pyrolyzation strategy, which is also a promising electrode material in lithium-ion batteries.
3. Without any surfactant, V2O3graphene-like structures by the top-down precursor-pyrolyzation strategy had been synthesized controllably. Interestingly enough, these ultrathin V2O3nanosheets which should exist temperature-induced reversible metal insulator transition represents a brand new two-dimensional material having metallic behavior. Meanwhile, we successfully realized controllable synthesis of3D flower-like structure precursor composed of nanaosheets having different diameter, packing density, and thickness of nanosheets by adjusting temperature and time. Using different gases, the V2O3and V2O3/C with the perfect inheritance of the morphology of their precursors were prepared by top-down precursor-pyrolyzation strategy. Compared with the V2O32D ultrathin sheets,3D flower-like structures and their composites with carbon coating, at the current density of200mA/g, the discharge capacity of V2O3/C3D flower-like micro-nanostructures is still maintained at360mAh/g after80cycles, which exbits excellent discharge capacity and superior cycling stability.
4. Graphene nanosheets (1-3graphite layers)had been solvothermally synthesized through reducing hexachloro-1,3-butadiene (C4Cl6) by Metallic sodium in polyethylene glycol (PEG-600) at300℃
引文
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