锂离子电池锡基负极材料的制备及其电化学性能研究
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摘要
作为锂离子电池新型负极材料,锡基负极材料近年来成为研究的热点之一。与现有的锂离子电池负极碳材料相比,锡基材料具有较高的比容量。然而锡基材料较差的循环性能,成为制约其实际应用的关键因素。本文针对这一关键问题开展了较系统的研究,取得了以下的主要结果:
(1)运用红外灯照射的方法制备了粒径为5nm的SnO_2粒子,样品分别经400℃、600℃、800℃热处理后,其粒径分别为10.8nm、24.2nm、39.1nm。XRD实验表明,所制备的纳米SnO_2粒子属于金红石型结构。不同粒径的纳米SnO_2粒子的红外光谱实验结果表明:在红外灯照射下先有有机锡化合物生成,随热处理温度的升高,有机基团被脱去,从而形成不同粒径的纳米SnO_2粒子。SnO_2纳米粒子电极的充放电实验表明:粒径为10.8nm的SnO_2粒子电极的充放电性能最好。因此,SnO_2纳米粒子的储锂性能,其粒径的大小是有一临界值。
(2)在含有十二烷基硫酸钠(SDS)和SnCl_2·2H_2O的乙二醇溶液中加入纯化的碳纳米管,加热于160℃下,制备SnO_2/CNTs复合材料,并以XRD、HRTEM、SEM等方法表征该材料的物相结构和表面形貌。结果表明:SnO_2纳米粒子均匀地覆盖在碳纳米管上,粒径小于10nm。以该纳米结构SnO_2/CNTs复合材料作为电极材料与锂片组装成扣式电池,恒流充放电测试显示该材料作为锂离子电池负极材料具有较高的比容量和良好的循环性能。
(3)运用电沉积技术在铜片集流体上沉积了一层锡和一层镍,分别得到Cu/Sn/Ni和Cu/Ni/Sn两种结构的镀层。XRD结果表明:热处理使镀层与基底之间相互扩散形成了Cu_6Sn_5和Ni_3Sn_4合金相。四种电极的充放电实验表明:热处理可以提高电极的循环性能。对循环后的热处理电极的表面形貌观察表明:在锡镀层表面修饰0.5μm金属镍,可以有效地抑制充放电过程中的体积膨胀。
(4)在铜片和泡沫铜上应用电沉积技术制备了锡-镍合金材料,并对材料进行热处理。样品的XRD实验表明,电沉积所得到的Sn-Ni合金镀层属于Ni_3Sn_4结构的合金。热处理使样品平面样品表面变得粗糙,而对三维多孔电极的表面形貌没有太大的影响。电极的充放电实验结果表明:三维多孔Sn-Ni合金电极的循环性能比平面结构电极的好;对电极进行热处理也可以提高电极的循环性能。
As a new anode material for lithium ion battery, Tin-based material has attracted much attention. Compared to graphite, which is used mainly in present commercialized production of Li-ion batteries, tin-based material exhibited higher theoretical capacity. But, its poor cyclability restricted it application for commercial anode material of lithium ion battery. In order to improve the performance of Sn-based active materials, the nanosized SnO_2 particles、sandwich structural Cu/Sn/Ni and Cu/Ni/Sn eledtrodes, and three-dimensional reticular Sn-Ni alloy electrode were prepared by sol-gel and electrodepositon. The phase structure and surface morphology of the said materials were determined by XRD、TEM and SEM. The electrochemical performance of the electrodes was measured by constant current charge-discharge test.
(1) SnO_2 nanoparticles with four different sizes of ~ 5, 10.8, 24.2, and 39.1 nm were synthesized using infrared irradiation and thermal treatment. X-ray diffraction (XRD) results indicated that the particles had tetragonal rutile structure (cassiterite SnO_2). TEM and FT-IR spectra revealed that at 673K, the disperse SnO_2 nanospheres began to aggregate to form bigger size clusters; the oblate spheroids must appear. Electrochemical tests showed that particle size had a significant influence on the lithium ion insertion/desertion properties, and the 10.8 nm-sized SnO_2 nanoparticles electrodes had a superior capacity and cycling stability as compared to the ~ 5, 24.2, and 39.1 nm-sized ones.
(2) The nano-structural SnO_2/carbon nanotubes composites were prepared in a solution of SnCl_2 ,ethylene glycol (EG),purified MWCNTs and sodium dodecyl sulfate (SDS) at 160℃. The phase structure and surface morphology of the composites were measured by XRD、HRTEM and SEM. The results indicate that there are high dispersions and high loadings of SnO_2 nanoparticles on MWCNTs. Electrochemical lithium storage performance was studied preliminarily on the obtained samples. MWCNTs modified with SnO_2 nanoparicles were shown to have a higher electrochemical reversible capacity than that of MWCNTs during the charge and discharge process. MWCNTs can accommodate the larger structure strain of the active materials produced during Li-ion insertion and extraction, which may improve the cycle performance of the electrode.
(3) The sandwich structural Cu/Sn/Ni and Cu/Ni/Sn deposits, which contained one layers Sn deposits and one-layer Ni deposits, were prepared by electroplating on Cu foil. The results of XRD indicated that after annealing Cu_6Sn_5 and Ni_3Sn_4 were formed on copper current collector with the diffusion between plating material and copper substrate. Charge-discharge test revealed that heat-treatment of the electrodes could improve the cycle performance of electrode. SEM observations showed that sandwich structure of electrode coated with 0.5μm nickel could restrain the volume expansion of active materials.
(4) The planar and three-dimensional reticular Sn-Ni alloy deposits were prepared by electrodepositing on Cu foil and foamed Cu, respectively. The X-ray diffraction patterns of the thermally treated Sn-Ni alloy deposit showed that the Sn-Ni alloy had a Ni3Sn4 phase. The surface of planar electrode became rough after annealing, but the surface of three-dimensional reticular electrode didn’t change. Charge-discharge test indicated heat-treatment of the electrodes could improve the cycle performance of electrode, and the cycle performance of three-dimensional reticular Sn-Ni alloy was better than that of the planar electrode. SEM result of the Sn-Ni alloy electrode showed that the three-dimensioned reticular structure in Sn-Ni alloy electrode could relax the volume expansion during cycling; three-dimensional reticular structure of Sn-Ni alloy electrodes was also beneficial to diffusion of lithium ion into/out of porous materials.
(1)运用红外灯照射的方法制备了粒径为5nm的SnO_2粒子,样品分别经400℃、600℃、800℃热处理后,其粒径分别为10.8nm、24.2nm、39.1nm。XRD实验表明,所制备的纳米SnO_2粒子属于金红石型结构。不同粒径的纳米SnO_2粒子的红外光谱实验结果表明:在红外灯照射下先有有机锡化合物生成,随热处理温度的升高,有机基团被脱去,从而形成不同粒径的纳米SnO_2粒子。SnO_2纳米粒子电极的充放电实验表明:粒径为10.8nm的SnO_2粒子电极的充放电性能最好。因此,SnO_2纳米粒子的储锂性能,其粒径的大小是有一临界值。
(2)在含有十二烷基硫酸钠(SDS)和SnCl_2·2H_2O的乙二醇溶液中加入纯化的碳纳米管,加热于160℃下,制备SnO_2/CNTs复合材料,并以XRD、HRTEM、SEM等方法表征该材料的物相结构和表面形貌。结果表明:SnO_2纳米粒子均匀地覆盖在碳纳米管上,粒径小于10nm。以该纳米结构SnO_2/CNTs复合材料作为电极材料与锂片组装成扣式电池,恒流充放电测试显示该材料作为锂离子电池负极材料具有较高的比容量和良好的循环性能。
(3)运用电沉积技术在铜片集流体上沉积了一层锡和一层镍,分别得到Cu/Sn/Ni和Cu/Ni/Sn两种结构的镀层。XRD结果表明:热处理使镀层与基底之间相互扩散形成了Cu_6Sn_5和Ni_3Sn_4合金相。四种电极的充放电实验表明:热处理可以提高电极的循环性能。对循环后的热处理电极的表面形貌观察表明:在锡镀层表面修饰0.5μm金属镍,可以有效地抑制充放电过程中的体积膨胀。
(4)在铜片和泡沫铜上应用电沉积技术制备了锡-镍合金材料,并对材料进行热处理。样品的XRD实验表明,电沉积所得到的Sn-Ni合金镀层属于Ni_3Sn_4结构的合金。热处理使样品平面样品表面变得粗糙,而对三维多孔电极的表面形貌没有太大的影响。电极的充放电实验结果表明:三维多孔Sn-Ni合金电极的循环性能比平面结构电极的好;对电极进行热处理也可以提高电极的循环性能。
As a new anode material for lithium ion battery, Tin-based material has attracted much attention. Compared to graphite, which is used mainly in present commercialized production of Li-ion batteries, tin-based material exhibited higher theoretical capacity. But, its poor cyclability restricted it application for commercial anode material of lithium ion battery. In order to improve the performance of Sn-based active materials, the nanosized SnO_2 particles、sandwich structural Cu/Sn/Ni and Cu/Ni/Sn eledtrodes, and three-dimensional reticular Sn-Ni alloy electrode were prepared by sol-gel and electrodepositon. The phase structure and surface morphology of the said materials were determined by XRD、TEM and SEM. The electrochemical performance of the electrodes was measured by constant current charge-discharge test.
(1) SnO_2 nanoparticles with four different sizes of ~ 5, 10.8, 24.2, and 39.1 nm were synthesized using infrared irradiation and thermal treatment. X-ray diffraction (XRD) results indicated that the particles had tetragonal rutile structure (cassiterite SnO_2). TEM and FT-IR spectra revealed that at 673K, the disperse SnO_2 nanospheres began to aggregate to form bigger size clusters; the oblate spheroids must appear. Electrochemical tests showed that particle size had a significant influence on the lithium ion insertion/desertion properties, and the 10.8 nm-sized SnO_2 nanoparticles electrodes had a superior capacity and cycling stability as compared to the ~ 5, 24.2, and 39.1 nm-sized ones.
(2) The nano-structural SnO_2/carbon nanotubes composites were prepared in a solution of SnCl_2 ,ethylene glycol (EG),purified MWCNTs and sodium dodecyl sulfate (SDS) at 160℃. The phase structure and surface morphology of the composites were measured by XRD、HRTEM and SEM. The results indicate that there are high dispersions and high loadings of SnO_2 nanoparticles on MWCNTs. Electrochemical lithium storage performance was studied preliminarily on the obtained samples. MWCNTs modified with SnO_2 nanoparicles were shown to have a higher electrochemical reversible capacity than that of MWCNTs during the charge and discharge process. MWCNTs can accommodate the larger structure strain of the active materials produced during Li-ion insertion and extraction, which may improve the cycle performance of the electrode.
(3) The sandwich structural Cu/Sn/Ni and Cu/Ni/Sn deposits, which contained one layers Sn deposits and one-layer Ni deposits, were prepared by electroplating on Cu foil. The results of XRD indicated that after annealing Cu_6Sn_5 and Ni_3Sn_4 were formed on copper current collector with the diffusion between plating material and copper substrate. Charge-discharge test revealed that heat-treatment of the electrodes could improve the cycle performance of electrode. SEM observations showed that sandwich structure of electrode coated with 0.5μm nickel could restrain the volume expansion of active materials.
(4) The planar and three-dimensional reticular Sn-Ni alloy deposits were prepared by electrodepositing on Cu foil and foamed Cu, respectively. The X-ray diffraction patterns of the thermally treated Sn-Ni alloy deposit showed that the Sn-Ni alloy had a Ni3Sn4 phase. The surface of planar electrode became rough after annealing, but the surface of three-dimensional reticular electrode didn’t change. Charge-discharge test indicated heat-treatment of the electrodes could improve the cycle performance of electrode, and the cycle performance of three-dimensional reticular Sn-Ni alloy was better than that of the planar electrode. SEM result of the Sn-Ni alloy electrode showed that the three-dimensioned reticular structure in Sn-Ni alloy electrode could relax the volume expansion during cycling; three-dimensional reticular structure of Sn-Ni alloy electrodes was also beneficial to diffusion of lithium ion into/out of porous materials.
引文
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