锰基化合物的形貌调控及其电化学性能研究
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摘要
在众多的锂离子电池正极材料中,锰系化合物特别是LiMn2O4具有资源丰富、价格低廉、环境友好等优点,因而在锂离子电池,尤其是在电动汽车(EV)及混合动力汽车(HEV)电源应用方面极具竞争潜力。然而,由于自身结构的原因,容量衰减问题一直制约了LiMn2O4的大规模应用。因此,开发和设计高效、稳定的微结构来提高LiMn2O4的电化学性能已经成了该领域的关键性课题。为此,本论文开展了LiMn2O4和β-MnO2的形貌调控及其电化学性能研究,获得的主要研究内容和结论归纳如下：
1.以水热合成的β-MnO2单晶纳米棒为前驱物,利用自模板反应法制备了LiMn2O4单晶纳米棒。发现在由四方相β-MnO2向立方相LiMn2O4转变过程中,前驱物β-MnO2的棒状形貌、单晶特性甚至生长取向均能在终产物中被保留下来。与以商品β-MnO2为前驱物合成的不规则的大尺寸LiMn2O4相比,LiMn2O4单晶纳米棒表现出更优异的电化学性能。即在室温下,0.5C的首次放电比容量为125mAhg-17C倍率下具有约95mAh g-1的放电容量,且以3C的倍率循环500周后仍能保持约75%的容量。其优异的性能应归因于材料的单晶特性和棒状形貌。即单晶内部结构的高度有序性使离子的扩散障碍较小,并具有良好的电子传导能力；而其纳米棒形貌为离子提供了较短的扩散路径便于Li+的嵌入和脱出,且其较高的比表面积便于电解液充分渗透提高了材料的利用效率。上述研究结果为一维结构的电极材料在锂离子电池中的应用提供了一些新的思路。
2.在成功合成上述LiMn2O4单晶纳米棒的基础上,制备了掺杂Al的单晶LiMn2O4纳米棒。发现其尺寸大小与未掺杂的单晶LiMn2O4纳米棒基本类似,且随着Al掺杂量的增加,虽然其放电容量逐渐减小,但循环性能逐渐提高。当Al的掺杂量x=0.1时的产物LiAlxMn2-xO4的材料容量保持率较好,并表现出较好的高温大倍率循环性能。即在50℃高温下,以3C倍率循环500周后仍能保持70%的容量,而未进行掺杂的LiMn2O4纳米棒在同等条件下仅能保持33%。上述掺杂Al的LiMn2O4具备较好的高温循环性能,有望成为一种极有前景的动力型锂离子电池正极材料,推动锂离子电池的发展。
3.以混合溶剂热法制备的γ-MnO(OH)纳米棒为前驱物合成了LiMn2O4纳米棒,对比研究了不同煅烧温度所得产物的电化学性能。结果表明,600℃煅烧时合成所得产物不仅保持了γ-MnO(OH)的棒状形貌,而且表现出最佳的电化学性能。即在室温下,0.5C的条件下首次放电比容量达125.6mAh g-1,以3C倍率循环100周后容量保持率达95.6%。上述以γ-MnO(OH)纳米棒为模板合成的LiMn2O4纳米棒正极材料具有合成方法简便易行、原料价廉易得、无毒无害以及优良的电化学活性,对高性能锂离子电池的研发具有重要的借鉴意义。
4.通过调整反应原料中浓盐酸的用量,采用水热法合成了中空双锥状β-MnO2单晶。研究表明,中空双锥状β-MnO2单晶的形成经历了自组装、溶解-重结晶、亚稳面的腐蚀三个主要过程。与商品β-MnO2相比,合成的中空双锥状β-MnO2单晶表现出了更优异的电化学活性。即在1.5～3.8V,10mAg-1的条件下,首次放电比容量达269mAh g-1,相当于每单元β-MnO2可嵌入0.87个Li+,而商品β-MnO2仅能嵌入0.2个Li+。该中空双锥状β-MnO2单晶具有合成方法简便易行、原料价廉易得、无毒无害以及优良的电化学活性,预计将在锂电池领域的应用中发挥重要的作用。
Among various cathode materials for lithium ion battery, Mn-based compounds (especially for spinel LiMn2O4) are considered as one of the most promising candidates due to its advantages such as low-cost, environmental friendliness and high abundance. However, the application of LiMn2O4is confined by the capacity decay and cycling instability caused by manganese dissolution, oxygen vacancy and Jahn-Teller effect. Therefore, it's necessary to explore an efficient system with stable structure to improve the electrochemical property. In present work, the morphology-controlled synthesis and electrochemical performance of LiMn2O4and β-MnO2were studied. The main contents and conclusions are as follows:
1. Single-crystalline LiMn2O4nanorods with a diameter of-100nm were synthesized via a template-engaged reaction using tetragonal β-MnO2nanorods as starting material. The investigations on the structures and morphologies of both the precursor and the final product reveal that a minimal structure reconstruction can be responsible for the chemical transformation from tetragonal β-MnO2nanorods to cubic LiMn2O4nanorods. The obtained LiMn2O4nanorods as cathode material for Li-ion battery exhibits superior high-rate capability and good cycling stability in a potential range of3.5-4.3V vs. Li+/Li, which can deliver an initial discharge capacity of125mAh g-1(>84%of the theoretical capacity of LiMn2O4) at a current rate of0.5C, and about75%of its initial capacity can be remained after500charge-discharge cycles at a current rate of3C. Importantly, the rod-like nanostructure and single-crystalline nature are also well preserved after prolonged the charge/discharge cycling time at a relatively high current rate, indicating good structural stability of the single-crystalline nanorods during the lithium intercalation/deintercalation processes, and such high-rate capacity and cycling performance can be ascribed to the favorable morphology and the high crystallinity of the obtained LiMn2O4nanorods.
2. Al-doped LiMn2O4nanorods were synthesized base on the above route, which almost have the same size with the above LiMn2O4nanorods. With the increasing doped amount of Al, the initial discharge capacity of the products decrease, but the cycling performance is gradually improved. It is found that the LiAl0.1Mn1.9O4nanorods has the best capacity retention through the comparison of the rate capability at0.5～5C rate for10cycles successively. The LiAl0.1Mn1.9O4nanorods also have excellent cycling performance at an elevated temperature, which still retain70%of the initial capacity at3C after500cycle at50℃, while the LiMn2O4nanorods has only33%of the initial capacity at the same condition. The Al-doped LiMn2O4nanorods with excellent cycle performance at high temperature will be promising cathode materials for high-power lithium ion batteries to promote the development of lithium ion battery.
3. LiMn2O4nanorods were synthesized using y-MnO(OH) nanorods as self-template, which was prepared via solvothermal reaction. The electrochemical performance of the products obtained at different calcination temperature was studied. It is found that the LiMn2O4nanorods obtained at600℃has the best electrochemical performance, which delivers the initial capacity of125.6mAh g-1and the capacity retention of95.6%after100cycles at3C. Considering that the low cost of raw materials, simple operation and the low calcination temperature, it is a promising route to synthesize one-dimensional LiMn2O4nanorods with good electrochemical performance using γ-MnO(OH) as precursor.
4. Single-crystal β-MnO2hollow bipyramids (HB-β-MnO2) were synthesized via a template-free hydrothermal method. The as-synthesized hollow bipyramids with100-300nm pores along the axis direction of β-MnO2bipyramids are formed through self-assembly and phase transformation processes from α-MnO2nanowires to β-MnO2bipyramids followed by chemical etching of its metastable crystal faces. Compared to the commercial bulk β-MnO2(c-β-MnO2), the as-synthesized HB-β-MnO2exhibits more excellent electrochemical performance with an initial discharge capacity of269mAh g-1, which means up to0.87Li+intercalation per β-MnO2unit, while only0.2Li+intercalation per β-MnO2unit for the commercial c-β-MnO2, The excellent electrochemical activity of the as-synthesized HB-β-MnO2can be attributed to its hollow structure and single crystal nature. The former can provide higher contact area with the electrolyte and buffer ability against volume change during the charge/discharge processes, while the latter contributes to good electronic conductivity and structural integrity stability. Considering the low cost, simple synthesis and the excellent electrochemical activity of the HB-β-MnO2, it will play an important role in the field of lithium battery.
1.以水热合成的β-MnO2单晶纳米棒为前驱物,利用自模板反应法制备了LiMn2O4单晶纳米棒。发现在由四方相β-MnO2向立方相LiMn2O4转变过程中,前驱物β-MnO2的棒状形貌、单晶特性甚至生长取向均能在终产物中被保留下来。与以商品β-MnO2为前驱物合成的不规则的大尺寸LiMn2O4相比,LiMn2O4单晶纳米棒表现出更优异的电化学性能。即在室温下,0.5C的首次放电比容量为125mAhg-17C倍率下具有约95mAh g-1的放电容量,且以3C的倍率循环500周后仍能保持约75%的容量。其优异的性能应归因于材料的单晶特性和棒状形貌。即单晶内部结构的高度有序性使离子的扩散障碍较小,并具有良好的电子传导能力；而其纳米棒形貌为离子提供了较短的扩散路径便于Li+的嵌入和脱出,且其较高的比表面积便于电解液充分渗透提高了材料的利用效率。上述研究结果为一维结构的电极材料在锂离子电池中的应用提供了一些新的思路。
2.在成功合成上述LiMn2O4单晶纳米棒的基础上,制备了掺杂Al的单晶LiMn2O4纳米棒。发现其尺寸大小与未掺杂的单晶LiMn2O4纳米棒基本类似,且随着Al掺杂量的增加,虽然其放电容量逐渐减小,但循环性能逐渐提高。当Al的掺杂量x=0.1时的产物LiAlxMn2-xO4的材料容量保持率较好,并表现出较好的高温大倍率循环性能。即在50℃高温下,以3C倍率循环500周后仍能保持70%的容量,而未进行掺杂的LiMn2O4纳米棒在同等条件下仅能保持33%。上述掺杂Al的LiMn2O4具备较好的高温循环性能,有望成为一种极有前景的动力型锂离子电池正极材料,推动锂离子电池的发展。
3.以混合溶剂热法制备的γ-MnO(OH)纳米棒为前驱物合成了LiMn2O4纳米棒,对比研究了不同煅烧温度所得产物的电化学性能。结果表明,600℃煅烧时合成所得产物不仅保持了γ-MnO(OH)的棒状形貌,而且表现出最佳的电化学性能。即在室温下,0.5C的条件下首次放电比容量达125.6mAh g-1,以3C倍率循环100周后容量保持率达95.6%。上述以γ-MnO(OH)纳米棒为模板合成的LiMn2O4纳米棒正极材料具有合成方法简便易行、原料价廉易得、无毒无害以及优良的电化学活性,对高性能锂离子电池的研发具有重要的借鉴意义。
4.通过调整反应原料中浓盐酸的用量,采用水热法合成了中空双锥状β-MnO2单晶。研究表明,中空双锥状β-MnO2单晶的形成经历了自组装、溶解-重结晶、亚稳面的腐蚀三个主要过程。与商品β-MnO2相比,合成的中空双锥状β-MnO2单晶表现出了更优异的电化学活性。即在1.5～3.8V,10mAg-1的条件下,首次放电比容量达269mAh g-1,相当于每单元β-MnO2可嵌入0.87个Li+,而商品β-MnO2仅能嵌入0.2个Li+。该中空双锥状β-MnO2单晶具有合成方法简便易行、原料价廉易得、无毒无害以及优良的电化学活性,预计将在锂电池领域的应用中发挥重要的作用。
Among various cathode materials for lithium ion battery, Mn-based compounds (especially for spinel LiMn2O4) are considered as one of the most promising candidates due to its advantages such as low-cost, environmental friendliness and high abundance. However, the application of LiMn2O4is confined by the capacity decay and cycling instability caused by manganese dissolution, oxygen vacancy and Jahn-Teller effect. Therefore, it's necessary to explore an efficient system with stable structure to improve the electrochemical property. In present work, the morphology-controlled synthesis and electrochemical performance of LiMn2O4and β-MnO2were studied. The main contents and conclusions are as follows:
1. Single-crystalline LiMn2O4nanorods with a diameter of-100nm were synthesized via a template-engaged reaction using tetragonal β-MnO2nanorods as starting material. The investigations on the structures and morphologies of both the precursor and the final product reveal that a minimal structure reconstruction can be responsible for the chemical transformation from tetragonal β-MnO2nanorods to cubic LiMn2O4nanorods. The obtained LiMn2O4nanorods as cathode material for Li-ion battery exhibits superior high-rate capability and good cycling stability in a potential range of3.5-4.3V vs. Li+/Li, which can deliver an initial discharge capacity of125mAh g-1(>84%of the theoretical capacity of LiMn2O4) at a current rate of0.5C, and about75%of its initial capacity can be remained after500charge-discharge cycles at a current rate of3C. Importantly, the rod-like nanostructure and single-crystalline nature are also well preserved after prolonged the charge/discharge cycling time at a relatively high current rate, indicating good structural stability of the single-crystalline nanorods during the lithium intercalation/deintercalation processes, and such high-rate capacity and cycling performance can be ascribed to the favorable morphology and the high crystallinity of the obtained LiMn2O4nanorods.
2. Al-doped LiMn2O4nanorods were synthesized base on the above route, which almost have the same size with the above LiMn2O4nanorods. With the increasing doped amount of Al, the initial discharge capacity of the products decrease, but the cycling performance is gradually improved. It is found that the LiAl0.1Mn1.9O4nanorods has the best capacity retention through the comparison of the rate capability at0.5～5C rate for10cycles successively. The LiAl0.1Mn1.9O4nanorods also have excellent cycling performance at an elevated temperature, which still retain70%of the initial capacity at3C after500cycle at50℃, while the LiMn2O4nanorods has only33%of the initial capacity at the same condition. The Al-doped LiMn2O4nanorods with excellent cycle performance at high temperature will be promising cathode materials for high-power lithium ion batteries to promote the development of lithium ion battery.
3. LiMn2O4nanorods were synthesized using y-MnO(OH) nanorods as self-template, which was prepared via solvothermal reaction. The electrochemical performance of the products obtained at different calcination temperature was studied. It is found that the LiMn2O4nanorods obtained at600℃has the best electrochemical performance, which delivers the initial capacity of125.6mAh g-1and the capacity retention of95.6%after100cycles at3C. Considering that the low cost of raw materials, simple operation and the low calcination temperature, it is a promising route to synthesize one-dimensional LiMn2O4nanorods with good electrochemical performance using γ-MnO(OH) as precursor.
4. Single-crystal β-MnO2hollow bipyramids (HB-β-MnO2) were synthesized via a template-free hydrothermal method. The as-synthesized hollow bipyramids with100-300nm pores along the axis direction of β-MnO2bipyramids are formed through self-assembly and phase transformation processes from α-MnO2nanowires to β-MnO2bipyramids followed by chemical etching of its metastable crystal faces. Compared to the commercial bulk β-MnO2(c-β-MnO2), the as-synthesized HB-β-MnO2exhibits more excellent electrochemical performance with an initial discharge capacity of269mAh g-1, which means up to0.87Li+intercalation per β-MnO2unit, while only0.2Li+intercalation per β-MnO2unit for the commercial c-β-MnO2, The excellent electrochemical activity of the as-synthesized HB-β-MnO2can be attributed to its hollow structure and single crystal nature. The former can provide higher contact area with the electrolyte and buffer ability against volume change during the charge/discharge processes, while the latter contributes to good electronic conductivity and structural integrity stability. Considering the low cost, simple synthesis and the excellent electrochemical activity of the HB-β-MnO2, it will play an important role in the field of lithium battery.
引文
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