锂离子电池正极材料Li_2MnSiO_4的合成和电化学性能研究
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摘要
Li2MnSiO4作为一种新型锂离子电池正极材料,尽管2006年才被Dominko研究小组首次报道,但由于其具有333 mAh/g的高理论容量、成本低廉、环境友好等突出的优点,被认为是一种极具潜力的锂离子电池正极材料。然而,Li2MnSiO4材料的电子电导率低,循环性能差,循环过程中结构易坍塌,急需系统深入研究。本文以Li2MnSiO4为研究对象,对其合成工艺、改性技术、电化学性能等方面进行了系统的研究。
采用最易产业化的高温固相法和新颖的多元醇法合成Li2MnSiO4系列锂离子电池正极材料；利用XRD、FESEM、HRTEM、ICP-AES、元素分析和粒度分析等手段对合成材料进行表征；利用电池测试仪测试合成材料的电化学性能。
利用TG-DSC初步确定固相反应的基础温度为800℃。利用正交试验法进行工艺优化。研究了合成温度和保温时间对Li2MnSiO4材料组织及电化学性能的影响。结果表明,随着合成温度的升高和保温时间的延长,Li2MnSiO4样品电化学性能提高。在900℃保温20 h合成的Li2MnSiO4样品具有较好的首次放电比容量117.9 mAh/g。探讨了样品的纯度、组织结构与电化学性能的关系。
利用交流阻抗法研究Li2-xMnSiO4材料的脱嵌锂动力学,测得了不同充放电状态下Li2-xMnSiO4材料的交流阻抗谱,并计算相应的锂离子扩散系数,结果表明,充电时,随着脱锂量的增加,Li2-xMnSiO4材料的锂离子扩散系数增大；放电时,随着嵌锂量的增加,Li2-xMnSiO4材料的锂离子扩散系数减小。
采用固相法,以导电碳黑、石墨、蔗糖和柠檬酸为碳源合成了一系列Li2MnSiO4/C复合材料。探索了碳源及碳含量对Li2MnSiO4/C材料组织及电化学性能的影响。成功筛选出最佳的蔗糖碳源,其对应样品的首次可逆容量达到88mAh/g,10次循环后容量保持在62.1 mAh/g。在本实验范围内,不管采用何种碳源,随着碳含量的升高,样品的杂质含量增多,晶粒度和粒度减小,当碳含量为9%-10%的范围时,合成的Li2MnSiO4/C样品总能得到最好的电化学性能。分析了碳源及碳含量对Li2MnSiO4／C性能的影响机理。
采用固相法成功合成了Fe2+、A13+、Mg2+、Ti4+掺杂的Li2Mn1-xMxSiO4(M=Fe,Al, Mg, Ti)固溶体材料,有效地解决了Li2MnSiO4在充放电过程中结构坍塌的问题。Fe2+掺杂样品的电化学性能随掺Fe2+量的提高而提高,当x=0.9时得到最高的首次放电比容量72.3 mAh/g。A13+、Mg2+、Ti4+等离子掺杂可有效提高Li2MnSiO4材料的电化学性能；其机理在于离子掺杂可以稳定Li2MnSiO4的晶体结构。进一步阐明了离子掺杂稳定Li2MnSiO4结构的机理,掺杂半径较小的阳离子可以减小Li2MnSiO4的晶胞体积,从而稳定其结构。晶体场理论分析表明Fe2+掺杂可以提高Li2MnSiO4的晶体场稳定化能,从而稳定其结构。
采用多元醇法,以蔗糖为碳源成功合成出Li2MnSiO4/C材料,并考察合成温度对其组织和电化学性能的影响。结果表明,合成的材料具有纳米级颗粒尺寸；在Li2MnSiO4颗粒周围包覆有一层无定型的碳膜；600℃合成的样品具有较优的电化学性能,在C/30倍率下首次可逆容量达到132 mAh/g。Al3+掺杂可以有效体高Li2MnSiO4样品的充放电性能,在0.1C倍率下充放电时,掺杂10%Al3+的样品比未掺Al3+样品的首次放电比容量提高1.4倍。
Li2MnSiO4 was firstly reported by Dominko's group as a new cathode material for lithium ion batteries in 2006. Because of its high theoretical capacity (333 mAh/g), low cost and environmental compatible, Li2MnSiO4 was considered as a potential cathode material for lithium ion batteries. However, the electron conductivity of Li2MnSiO4 is low and the cycle ability is poor, so Li2MnSiO4 is in dire need of system and deep researching. This thesis focused on Li2MnSiO4 and studied its synthesis process, modified technic and electrochemical performance.
Solid state method and polyol process were used to synthesize the Li2MnSiO4 cathode material; XRD, FESEM, HRTEM, ICP-AES, elemental analysis and granularity analysis were employed to character the physical and chemical properties; Battery testing system was used to test the electrochemical properties.
The basic process parameter reaction temperature of 800℃was chose via TG-DSC, and then optimized by orthogonal experiments. Effect of sythesis temperature and holding time on microstructure and electrochemical performance of Li2MnSiO4 material were studied. The results showed that along with the raise of sythesis temperature and prolong of holding time, the electrochemical performance of Li2MnSiO4 was improved. The sample synthesized at 900℃for 20 h has the better initial discharge capacity of 117.9 mAh/g. The relationship of phase purity, microstructure and electrochemical properties was discussed.
EIS was employed to study the extraction insertion kinetics of Li2MnSiO4 material. The EIS of Li2-xMnSi04 at different charge-discharge state was tested, and the corresponding lithium ion diffusion coefficient was calculated. In charge cycle, the lithium ion diffusion coefficient of Li2-xMnSi04 increased with the increase of x. In discharge cycle, the lithium ion diffusion coefficient of Li2-xMnSi04 decreased with the decrease of x.
Li2MnSiO4/C composites were synthesized by solid state method with carbon black, graphite, sucrose and citric acid as carbon source. Effect of carbon source and carbon content on microstructure and electrochemical performance of Li2MnSiO4/C was studied. The Li2MnSiO4 sample corresponding to the best sucrose carbon source has the best initial reversible capacity of 88 mAh/g, and a discharge capacity of 62.1 mAh/g was obtained after 10 cycles. In the scope of this study, whichever carbon source was chose, along with the increase of carbon content, the grain size and particle size reduced and the amount of impurity increased. When carbon content was 9%-10%, the Li2MnSiO4/C samples can always achieve the best electrochemical performance. The effect mechanism of carbon source and carbon content on the electrochemical performance of Li2MnSiO4/C was analysed.
Li2Mni-xMxSi04 (M=Fe, Al, Mg, Ti) cathode material was synthesize by solid state reaction; the problem that the structure of Li2MnSiO4 is collapsed during the charge-discharge cycle has been effectively solved. The electrochemical performance of the Fe2＋doping samples was increased with the raise of the Fe2＋doping amount. The best initial discharge capacity of 72.3 mAh/g was achived when x= 0.9. Al3＋, Mg2＋and Ti4＋doing can improve the electrochemical performance of Li2MnSiO4 effectively, since ion doping can stabilize the crystal structure of Li2MnSiO4. The mechanism of that ion doping stabilize the structure of Li2MnSiO4 was illustrated. The crystal volume of Li2MnSiO4 was shrinked by doped positive ion which has small ion radius, thus the structure was stabilized. The crystal field theory in coordination chemistry was used to reveal that Fe2＋doping can improve the crystal field stabilization energies and thus the structure was stabilized.
Li2MnSiO4/C material was synthesized by polyol method with sucrose as carbon source, and the effect of synthesis temperature on microstructure and electrochemical performance of Li2MnSi04/C was explored. The results shown, the obtained samples have pure Li2MnSiO4 phase and nanoparticles, which coated by a very thin amorphous carbon film. The sample obtained at 600℃has a best initial reversible capacity of 132 mAh/g. Al3＋doping can remarkably improve the charge-discharge property of Li2MnSiO4. When cycled at 0.1C rate, the initial discharge capacity of the sample doped 10% Al3＋was 2.4 times as that of the pristine sample.
采用最易产业化的高温固相法和新颖的多元醇法合成Li2MnSiO4系列锂离子电池正极材料；利用XRD、FESEM、HRTEM、ICP-AES、元素分析和粒度分析等手段对合成材料进行表征；利用电池测试仪测试合成材料的电化学性能。
利用TG-DSC初步确定固相反应的基础温度为800℃。利用正交试验法进行工艺优化。研究了合成温度和保温时间对Li2MnSiO4材料组织及电化学性能的影响。结果表明,随着合成温度的升高和保温时间的延长,Li2MnSiO4样品电化学性能提高。在900℃保温20 h合成的Li2MnSiO4样品具有较好的首次放电比容量117.9 mAh/g。探讨了样品的纯度、组织结构与电化学性能的关系。
利用交流阻抗法研究Li2-xMnSiO4材料的脱嵌锂动力学,测得了不同充放电状态下Li2-xMnSiO4材料的交流阻抗谱,并计算相应的锂离子扩散系数,结果表明,充电时,随着脱锂量的增加,Li2-xMnSiO4材料的锂离子扩散系数增大；放电时,随着嵌锂量的增加,Li2-xMnSiO4材料的锂离子扩散系数减小。
采用固相法,以导电碳黑、石墨、蔗糖和柠檬酸为碳源合成了一系列Li2MnSiO4/C复合材料。探索了碳源及碳含量对Li2MnSiO4/C材料组织及电化学性能的影响。成功筛选出最佳的蔗糖碳源,其对应样品的首次可逆容量达到88mAh/g,10次循环后容量保持在62.1 mAh/g。在本实验范围内,不管采用何种碳源,随着碳含量的升高,样品的杂质含量增多,晶粒度和粒度减小,当碳含量为9%-10%的范围时,合成的Li2MnSiO4/C样品总能得到最好的电化学性能。分析了碳源及碳含量对Li2MnSiO4／C性能的影响机理。
采用固相法成功合成了Fe2+、A13+、Mg2+、Ti4+掺杂的Li2Mn1-xMxSiO4(M=Fe,Al, Mg, Ti)固溶体材料,有效地解决了Li2MnSiO4在充放电过程中结构坍塌的问题。Fe2+掺杂样品的电化学性能随掺Fe2+量的提高而提高,当x=0.9时得到最高的首次放电比容量72.3 mAh/g。A13+、Mg2+、Ti4+等离子掺杂可有效提高Li2MnSiO4材料的电化学性能；其机理在于离子掺杂可以稳定Li2MnSiO4的晶体结构。进一步阐明了离子掺杂稳定Li2MnSiO4结构的机理,掺杂半径较小的阳离子可以减小Li2MnSiO4的晶胞体积,从而稳定其结构。晶体场理论分析表明Fe2+掺杂可以提高Li2MnSiO4的晶体场稳定化能,从而稳定其结构。
采用多元醇法,以蔗糖为碳源成功合成出Li2MnSiO4/C材料,并考察合成温度对其组织和电化学性能的影响。结果表明,合成的材料具有纳米级颗粒尺寸；在Li2MnSiO4颗粒周围包覆有一层无定型的碳膜；600℃合成的样品具有较优的电化学性能,在C/30倍率下首次可逆容量达到132 mAh/g。Al3+掺杂可以有效体高Li2MnSiO4样品的充放电性能,在0.1C倍率下充放电时,掺杂10%Al3+的样品比未掺Al3+样品的首次放电比容量提高1.4倍。
Li2MnSiO4 was firstly reported by Dominko's group as a new cathode material for lithium ion batteries in 2006. Because of its high theoretical capacity (333 mAh/g), low cost and environmental compatible, Li2MnSiO4 was considered as a potential cathode material for lithium ion batteries. However, the electron conductivity of Li2MnSiO4 is low and the cycle ability is poor, so Li2MnSiO4 is in dire need of system and deep researching. This thesis focused on Li2MnSiO4 and studied its synthesis process, modified technic and electrochemical performance.
Solid state method and polyol process were used to synthesize the Li2MnSiO4 cathode material; XRD, FESEM, HRTEM, ICP-AES, elemental analysis and granularity analysis were employed to character the physical and chemical properties; Battery testing system was used to test the electrochemical properties.
The basic process parameter reaction temperature of 800℃was chose via TG-DSC, and then optimized by orthogonal experiments. Effect of sythesis temperature and holding time on microstructure and electrochemical performance of Li2MnSiO4 material were studied. The results showed that along with the raise of sythesis temperature and prolong of holding time, the electrochemical performance of Li2MnSiO4 was improved. The sample synthesized at 900℃for 20 h has the better initial discharge capacity of 117.9 mAh/g. The relationship of phase purity, microstructure and electrochemical properties was discussed.
EIS was employed to study the extraction insertion kinetics of Li2MnSiO4 material. The EIS of Li2-xMnSi04 at different charge-discharge state was tested, and the corresponding lithium ion diffusion coefficient was calculated. In charge cycle, the lithium ion diffusion coefficient of Li2-xMnSi04 increased with the increase of x. In discharge cycle, the lithium ion diffusion coefficient of Li2-xMnSi04 decreased with the decrease of x.
Li2MnSiO4/C composites were synthesized by solid state method with carbon black, graphite, sucrose and citric acid as carbon source. Effect of carbon source and carbon content on microstructure and electrochemical performance of Li2MnSiO4/C was studied. The Li2MnSiO4 sample corresponding to the best sucrose carbon source has the best initial reversible capacity of 88 mAh/g, and a discharge capacity of 62.1 mAh/g was obtained after 10 cycles. In the scope of this study, whichever carbon source was chose, along with the increase of carbon content, the grain size and particle size reduced and the amount of impurity increased. When carbon content was 9%-10%, the Li2MnSiO4/C samples can always achieve the best electrochemical performance. The effect mechanism of carbon source and carbon content on the electrochemical performance of Li2MnSiO4/C was analysed.
Li2Mni-xMxSi04 (M=Fe, Al, Mg, Ti) cathode material was synthesize by solid state reaction; the problem that the structure of Li2MnSiO4 is collapsed during the charge-discharge cycle has been effectively solved. The electrochemical performance of the Fe2＋doping samples was increased with the raise of the Fe2＋doping amount. The best initial discharge capacity of 72.3 mAh/g was achived when x= 0.9. Al3＋, Mg2＋and Ti4＋doing can improve the electrochemical performance of Li2MnSiO4 effectively, since ion doping can stabilize the crystal structure of Li2MnSiO4. The mechanism of that ion doping stabilize the structure of Li2MnSiO4 was illustrated. The crystal volume of Li2MnSiO4 was shrinked by doped positive ion which has small ion radius, thus the structure was stabilized. The crystal field theory in coordination chemistry was used to reveal that Fe2＋doping can improve the crystal field stabilization energies and thus the structure was stabilized.
Li2MnSiO4/C material was synthesized by polyol method with sucrose as carbon source, and the effect of synthesis temperature on microstructure and electrochemical performance of Li2MnSi04/C was explored. The results shown, the obtained samples have pure Li2MnSiO4 phase and nanoparticles, which coated by a very thin amorphous carbon film. The sample obtained at 600℃has a best initial reversible capacity of 132 mAh/g. Al3＋doping can remarkably improve the charge-discharge property of Li2MnSiO4. When cycled at 0.1C rate, the initial discharge capacity of the sample doped 10% Al3＋was 2.4 times as that of the pristine sample.
引文
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