高性能钛氧化物负极材料制备及其电化学性能研究
摘要
钛氧化物由于较高的充放电平台、高化学稳定性、充放电过程体积“零”应变，且具备开放的嵌脱锂通道等优势，成为潜在应用于新兴动力锂离子电池的负极材料之一。但其固有电导率低限制了快速充放电能力发挥。本文针对几种钛氧化物存在的上述突出问题，采用基于溶胶凝胶及水解合成策略构筑不同结构特点的纳米结构电极材料，借助于TG(热重分析法)、XRD(X射线衍射分析)、SEM(扫描电子显微镜)、TEM(透射电子显微镜)、CV (循环伏安)、充放电测试、EIS (电化学阻抗谱)等测试手段，深入研究了纳米结构的形成机制、制备材料的物理化学特征和电化学脱嵌锂行为。
采用溶胶凝胶路线，以嵌段共聚物F127作为配位体制备了纳米晶钛酸锂，在强酸环境下，F127的环氧乙烯（EO）链段和Ti~(4+)、Li~+通过氢键作用形成冠醚状配位体，形成有效络合，使参与反应的原料物质以分子级别混合，在较低的温度下（700℃）获得单相尖晶石钛酸锂纳米晶。SEM和TEM测试表明，钛酸锂的晶粒为规整多面体结构，结晶度好，分布均匀，晶粒尺寸约为100nm。作为锂离子电池负极材料展现了较好的电化学性能，在5C、10C、20C和40C测试倍率下容量分别为165mAhg~(-1)、150mAhg~(-1)、131mAhg~(-1)和108mAhg~(-1)。
在采用嵌段共聚物F127作为配位体的基础上，将前驱体在氩气气氛下煅烧，F127在煅烧过程中碳化形成的碳原位锚定在颗粒表面，有效的抑制了晶粒生长。最终在750℃下合成了颗粒尺寸在20nm左右的高结晶度钛酸锂。同时，表面形成的均匀碳网络大幅度改善了钛酸锂的电导率，为8.2103S m1。作为锂离子电池负极材料，钛酸锂/碳复合材料展现了优越的倍率性能和循环性能，在5C、10C、20C和40C的放电容量分别为160mAhg~(-1)，155mAhg~(-1)，139mAhg~(-1)和123mAhg~(-1)。
采用基于离子液体辅助的溶胶-凝胶路线合成了具有孔径分布均匀、高热稳定性的锐钛矿TiO_2纳米晶。考察了煅烧温度和咪唑离子液体阳离子碳链长度等因素对合成TiO_2的影响，发现长碳链离子液体表现出了更显著的模板剂和稳定剂的作用，并且离子液体在合成过程具有稳定TiO_2晶体结构的作用，所获得介孔纳米晶TiO_2具有较大的比表面积（112m2g1）。作为锂离子电池负极材料表现出优越的倍率性能和循环性能，介孔TiO_2纳米晶在5C、10C倍率下的容量为140mAhg~(-1)和118mAhg~(-1)，同时在不同倍率下均表现出较好的容量保持率和接近于100%的库伦效率。
采用TiCl4做为钛源，离子液体C_(16)mimBr作为结构导向剂，经一步水解获得了纳米花状金红石二氧化钛微结构。纳米花的平均颗粒尺寸为400nm，是由6nm的TiO_2纳米晶颗粒沿着[001]方向定向生长的纳米线呈放射状构成。花状结构外表面暴露的都是垂直于C轴利于锂离子高速输运的端面，同时纳米线能够提供锂离子和电子的连续扩散通道。制备的金红石型TiO_2表现出了突出的放电容量、良好的倍率性能和循环稳定性。充放电测试表明约有0.72mol的锂离子能够可逆的脱嵌入TiO_2晶格中，可逆容量达到242mAhg~(-1)，在5C，10C和20C的容量分别为170mAhg~(-1)、144mAhg~(-1)和116mAhg~(-1)。进一步采用原位复合技术，成功获得了金红石TiO_2/Graphene复合材料。复合电极体系表现出了优良的倍率性能和循环稳定性，TiO_2/Graphene复合材料在5C、10C和20C的容量分别为186mAhg~(-1)、171mAhg~(-1)和140mAhg~(-1)，充放电效率接近100%。
Titanium oxides have been regarded as potential candidates for anode materialsof lithium ion batteries, owing to their advantages including high charge-dischargevoltage, good chemical stability, zero volume strain during the charge and dischargeprocess, and open channel for lithium-ion insertion and extraction. However, the lowelectron conductivity of lithium titanium oxide adversely has restricted its ability offast charge and discharge. With regards to the disadvantages of several titaniumoxides, we prepared nanostructure electrode materials with different structure byemploying strategies of sol-gel and hydrolysis methods. In this thesis, TG(Thermogravimetry analysis), XRD (X-ray diffraction), SEM (Scanning ElectronMicroscopy), TEM (Transmission Electron Microscopy), CV (Cyclic Voltammetry)、DC（Discharge and Charge test）、EIS (Electrochemical impedance spectroscopy)measurements are performed to characterize the morphologies, structures andelectrochemical performance of the as-derived samples.
Firstly, we report a facile approach for synthesizing nanocrystalline Li_4Ti_5O_(12)via sol-gel process by employing a nonionic surfactant tri-block copolymer (pluronicF127) as the chelating agent. In the strong acid condition of our experiment, thealkylene oxide segments of F127could form crown-ether-type complexes with Ti~(4+)and Li+through coordination bonds, bringing the reaction partners sufficiently closetogether. Therefore, a pure-phase Li_4Ti_5O_(12)could be obtained at a relative lowtemperature of700oC. SEM and TEM measurements indicate that the as-derivedLi_4Ti_5O_(12)has a cubic morphology, high crystallinity and a uniform particle sizedistribution of around100nm. Nanocrystal Li_4Ti_5O_(12)is tested as an anode materialfor lithium ion batteries, exhibiting excellent electrochemical performance. Thespecific charge capacities of the cell are165mAhg~(-1)、150mAhg~(-1)、131mAhg~(-1)and108mAhg~(-1)at5C,10C,20C and40C, respectively.
The titanium gel precursor is further calcined under Ar atmosphere on the basisof employing a nonionic surfactant tri-block copolymer (pluronic F127) as thechelating agent. The grain growth of Li_4Ti_5O_(12)is effectively restrained by the carbongenerated from the carbonization of F127in the caclination process, and a smallparticle size of Li_4Ti_5O_(12)(~20nm) is successfully obtained at the calcinationtemperature of750oC. The electrical conductivity is further enhanced to be8.2103S m1due to the formed carbon-network on the surface of the sample. The as-derivednanocrystalline Li_4Ti_5O_(12)is tested as anode material for lithium ion battery, exhibiting excellent rate capability and cycle performance. The specific chargecapacities of the cell are160mAhg~(-1)、155mAhg~(-1)、139mAhg~(-1)and123mAhg~(-1)at5C,10C,20C and40C, respectively.
Moreover, mesoporous anatase TiO_2nanocrystalline with uniform pore sizedistribution, large surface area and high thermal stability was prepared via sol-gelapproach by employing room temperature ionic liquids (RTILs). We studied theinfluence of the calcination temperature and the carbon-chain length of RTILs on theperformance of the as-derived TiO_2. The result indicates that the long carbon-chainionic liquids showed superior function of template and stabilizing agent. Meanwhile,RTILs play a critical role in stabilizing the crystal structure of anatase TiO_2in oursynthesis. The mesoporous anatase TiO_2shows a large surface area of112m2g1.The as-derived mesoporous anatase TiO_2nanocrystalline is tested as an anodematerial for lithium ion batteries, exhibiting excellent rate capability and cycleperformance. The cell exhibits a reversible capacity of140mAhg~(-1)and118mAhg1at the current density of5C and10C. Meanwhile, the cell demonstrates goodcapacity retentions and high coulombic efficiencies (~100%) at all current rates.
Finally, we report the synthesis of “flower” rutile TiO_2through a facile one-pothydrolysis route by employing titanium tetrachloride as the titanium source and1-hexadecyl-3-methyl imidazolium bromine (C_(16)mimBr) as the structure-directingagent. The rutile TiO_2particle features flower-like nanostructure with the averagesize of400nm comprised with numerous well-defined and straight nanorods. Thenanorods with a diameter of around6nm are oriented radially from the central regiontoward edges of the particle. The dandelions-like nanostructure exposes plenty ofvertical cross-section of c-axis, which could enlarge the effective contact area for thetransport of Li+. Meanwhile, the well-connected nanorod-crystals provide acontinuous pathway for the diffusion of lithium ions and electrons in the titaniascaffold. The as-derived “flower” rutile TiO_2is tested as anode material for lithiumion batteries, exhibiting excellent rate capability and cycle performance. The chargeand discharge measurement indicates that about0.72Li+could be reversibly insertedand extracted into the TiO_2structure, corresponding to the capacity of242mAhg~(-1).Meanwhile, the cell exhibits a reversible capacity of170mAhg~(-1)、144mAhg~(-1)and116mAhg~(-1)at the current density of5C,10C and20C respectively. Furthermore,we successfully obtain rutile TiO_2/graphene composite by in-situ synthesis route. Theas-derived composite is tested as an anode material for lithium ion batteries,exhibiting excellent rate capability and cycle stability. The cell exhibits a reversiblecapacity of186mAhg~(-1)、171mAhg~(-1)and140mAhg~(-1)at the current density of5C, 10C and20C respectively. Meanwhile, the cell demonstrates high coulombicefficiency of~100%at all current rates.
采用溶胶凝胶路线，以嵌段共聚物F127作为配位体制备了纳米晶钛酸锂，在强酸环境下，F127的环氧乙烯（EO）链段和Ti~(4+)、Li~+通过氢键作用形成冠醚状配位体，形成有效络合，使参与反应的原料物质以分子级别混合，在较低的温度下（700℃）获得单相尖晶石钛酸锂纳米晶。SEM和TEM测试表明，钛酸锂的晶粒为规整多面体结构，结晶度好，分布均匀，晶粒尺寸约为100nm。作为锂离子电池负极材料展现了较好的电化学性能，在5C、10C、20C和40C测试倍率下容量分别为165mAhg~(-1)、150mAhg~(-1)、131mAhg~(-1)和108mAhg~(-1)。
在采用嵌段共聚物F127作为配位体的基础上，将前驱体在氩气气氛下煅烧，F127在煅烧过程中碳化形成的碳原位锚定在颗粒表面，有效的抑制了晶粒生长。最终在750℃下合成了颗粒尺寸在20nm左右的高结晶度钛酸锂。同时，表面形成的均匀碳网络大幅度改善了钛酸锂的电导率，为8.2103S m1。作为锂离子电池负极材料，钛酸锂/碳复合材料展现了优越的倍率性能和循环性能，在5C、10C、20C和40C的放电容量分别为160mAhg~(-1)，155mAhg~(-1)，139mAhg~(-1)和123mAhg~(-1)。
采用基于离子液体辅助的溶胶-凝胶路线合成了具有孔径分布均匀、高热稳定性的锐钛矿TiO_2纳米晶。考察了煅烧温度和咪唑离子液体阳离子碳链长度等因素对合成TiO_2的影响，发现长碳链离子液体表现出了更显著的模板剂和稳定剂的作用，并且离子液体在合成过程具有稳定TiO_2晶体结构的作用，所获得介孔纳米晶TiO_2具有较大的比表面积（112m2g1）。作为锂离子电池负极材料表现出优越的倍率性能和循环性能，介孔TiO_2纳米晶在5C、10C倍率下的容量为140mAhg~(-1)和118mAhg~(-1)，同时在不同倍率下均表现出较好的容量保持率和接近于100%的库伦效率。
采用TiCl4做为钛源，离子液体C_(16)mimBr作为结构导向剂，经一步水解获得了纳米花状金红石二氧化钛微结构。纳米花的平均颗粒尺寸为400nm，是由6nm的TiO_2纳米晶颗粒沿着[001]方向定向生长的纳米线呈放射状构成。花状结构外表面暴露的都是垂直于C轴利于锂离子高速输运的端面，同时纳米线能够提供锂离子和电子的连续扩散通道。制备的金红石型TiO_2表现出了突出的放电容量、良好的倍率性能和循环稳定性。充放电测试表明约有0.72mol的锂离子能够可逆的脱嵌入TiO_2晶格中，可逆容量达到242mAhg~(-1)，在5C，10C和20C的容量分别为170mAhg~(-1)、144mAhg~(-1)和116mAhg~(-1)。进一步采用原位复合技术，成功获得了金红石TiO_2/Graphene复合材料。复合电极体系表现出了优良的倍率性能和循环稳定性，TiO_2/Graphene复合材料在5C、10C和20C的容量分别为186mAhg~(-1)、171mAhg~(-1)和140mAhg~(-1)，充放电效率接近100%。
Titanium oxides have been regarded as potential candidates for anode materialsof lithium ion batteries, owing to their advantages including high charge-dischargevoltage, good chemical stability, zero volume strain during the charge and dischargeprocess, and open channel for lithium-ion insertion and extraction. However, the lowelectron conductivity of lithium titanium oxide adversely has restricted its ability offast charge and discharge. With regards to the disadvantages of several titaniumoxides, we prepared nanostructure electrode materials with different structure byemploying strategies of sol-gel and hydrolysis methods. In this thesis, TG(Thermogravimetry analysis), XRD (X-ray diffraction), SEM (Scanning ElectronMicroscopy), TEM (Transmission Electron Microscopy), CV (Cyclic Voltammetry)、DC（Discharge and Charge test）、EIS (Electrochemical impedance spectroscopy)measurements are performed to characterize the morphologies, structures andelectrochemical performance of the as-derived samples.
Firstly, we report a facile approach for synthesizing nanocrystalline Li_4Ti_5O_(12)via sol-gel process by employing a nonionic surfactant tri-block copolymer (pluronicF127) as the chelating agent. In the strong acid condition of our experiment, thealkylene oxide segments of F127could form crown-ether-type complexes with Ti~(4+)and Li+through coordination bonds, bringing the reaction partners sufficiently closetogether. Therefore, a pure-phase Li_4Ti_5O_(12)could be obtained at a relative lowtemperature of700oC. SEM and TEM measurements indicate that the as-derivedLi_4Ti_5O_(12)has a cubic morphology, high crystallinity and a uniform particle sizedistribution of around100nm. Nanocrystal Li_4Ti_5O_(12)is tested as an anode materialfor lithium ion batteries, exhibiting excellent electrochemical performance. Thespecific charge capacities of the cell are165mAhg~(-1)、150mAhg~(-1)、131mAhg~(-1)and108mAhg~(-1)at5C,10C,20C and40C, respectively.
The titanium gel precursor is further calcined under Ar atmosphere on the basisof employing a nonionic surfactant tri-block copolymer (pluronic F127) as thechelating agent. The grain growth of Li_4Ti_5O_(12)is effectively restrained by the carbongenerated from the carbonization of F127in the caclination process, and a smallparticle size of Li_4Ti_5O_(12)(~20nm) is successfully obtained at the calcinationtemperature of750oC. The electrical conductivity is further enhanced to be8.2103S m1due to the formed carbon-network on the surface of the sample. The as-derivednanocrystalline Li_4Ti_5O_(12)is tested as anode material for lithium ion battery, exhibiting excellent rate capability and cycle performance. The specific chargecapacities of the cell are160mAhg~(-1)、155mAhg~(-1)、139mAhg~(-1)and123mAhg~(-1)at5C,10C,20C and40C, respectively.
Moreover, mesoporous anatase TiO_2nanocrystalline with uniform pore sizedistribution, large surface area and high thermal stability was prepared via sol-gelapproach by employing room temperature ionic liquids (RTILs). We studied theinfluence of the calcination temperature and the carbon-chain length of RTILs on theperformance of the as-derived TiO_2. The result indicates that the long carbon-chainionic liquids showed superior function of template and stabilizing agent. Meanwhile,RTILs play a critical role in stabilizing the crystal structure of anatase TiO_2in oursynthesis. The mesoporous anatase TiO_2shows a large surface area of112m2g1.The as-derived mesoporous anatase TiO_2nanocrystalline is tested as an anodematerial for lithium ion batteries, exhibiting excellent rate capability and cycleperformance. The cell exhibits a reversible capacity of140mAhg~(-1)and118mAhg1at the current density of5C and10C. Meanwhile, the cell demonstrates goodcapacity retentions and high coulombic efficiencies (~100%) at all current rates.
Finally, we report the synthesis of “flower” rutile TiO_2through a facile one-pothydrolysis route by employing titanium tetrachloride as the titanium source and1-hexadecyl-3-methyl imidazolium bromine (C_(16)mimBr) as the structure-directingagent. The rutile TiO_2particle features flower-like nanostructure with the averagesize of400nm comprised with numerous well-defined and straight nanorods. Thenanorods with a diameter of around6nm are oriented radially from the central regiontoward edges of the particle. The dandelions-like nanostructure exposes plenty ofvertical cross-section of c-axis, which could enlarge the effective contact area for thetransport of Li+. Meanwhile, the well-connected nanorod-crystals provide acontinuous pathway for the diffusion of lithium ions and electrons in the titaniascaffold. The as-derived “flower” rutile TiO_2is tested as anode material for lithiumion batteries, exhibiting excellent rate capability and cycle performance. The chargeand discharge measurement indicates that about0.72Li+could be reversibly insertedand extracted into the TiO_2structure, corresponding to the capacity of242mAhg~(-1).Meanwhile, the cell exhibits a reversible capacity of170mAhg~(-1)、144mAhg~(-1)and116mAhg~(-1)at the current density of5C,10C and20C respectively. Furthermore,we successfully obtain rutile TiO_2/graphene composite by in-situ synthesis route. Theas-derived composite is tested as an anode material for lithium ion batteries,exhibiting excellent rate capability and cycle stability. The cell exhibits a reversiblecapacity of186mAhg~(-1)、171mAhg~(-1)and140mAhg~(-1)at the current density of5C, 10C and20C respectively. Meanwhile, the cell demonstrates high coulombicefficiency of~100%at all current rates.
引文
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