锂离子电池纳米电极材料的研究
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摘要
化石燃料的大量应用导致了温室效应,随着全球变暖问题日益紧迫,节能减排成为当今世界最为关注的焦点和主题。为了降低对石油能源的依靠和二氧化碳的排放,许多国家加大了对混合电动汽车及电动汽车的研究和投入,对其主要电源设备锂离子电池的能量密度,特别是功率密度提出了更高的要求。电极材料是影响锂离子性能的关键。由于纳米材料具有尺寸小,锂离子嵌/脱行程短,动力学性能优秀；比表面积大,嵌锂活性位点多；大电流下充放电时电极极化程度小、可逆容量高等特点,锂离子电池纳米电极材料得到广泛关注和研究。
本论文从纳米材料出发,以MoOx、Ge、C为研究客体,探索了多种形貌纳米材料的合成条件及规律,进一步扩充了纳米材料库；测试了它们在大电流密度下的充放电性能,并着重考察了MoO2纳米材料电化学性能与其结构形貌的关系。主要内容包括：
1.a-MoO3纳米带的制备和电化学性能研究
通过水热法制备了单晶α-MoO3纳米带。该纳米带材料长5-10μm,宽200-500 nm,厚约50 nm,沿着[001]方向生长。作为锂离子电池正极材料,α-MOO3纳米带在30 mA/g电流密度下表现出264mAh/g的容量;当电流密度上升到5000mA/g时,容量达176mAh/gi(能量密度300Wh/kg,功率密度9000 W/kg),50次循环后容量还能保持到114mAh/g。相比微米级MoO3纳米材料在5000mA/g电流密度下容量不到70mAh/g,MoO3纳米带表现出更优越的倍率性能。
2.系列MoO2纳米材料的制备和电化学性能研究
首先,利用乙醇蒸汽还原法制得MOO2纳米颗粒。相比传统制备MOo2采用H2还原MoO3的方法,采用乙醇蒸汽替代H2,更加便宜、安全,而且还原温度降低,节约了能源。乙醇蒸汽在400℃6下还原MoO3,得到表面有半石墨化碳包覆的粒径约为100nm的单斜MoO2颗粒。该产物在500 mA/g的电流密度下首次充放电表现出约320mAh/g的可逆容量,20次循环几乎没有衰减。而H2还原MoO3所得MoO2微米颗粒在500 mA/g电流密度下可逆容量不到175mAh/g。可见乙醇蒸汽还原所得的MoO2表现出良好的大电流放电性能。
同时,本文还关注MoO2一维纳米结构的合成。文献报道的一维MoO2纳米线和纳米棒主要是通过电化学沉积或气相沉积来制备,这些方法比较复杂,产物较难控制,产量低。用α-MoO3纳米带作为前驱体分散在水中,加入葡萄糖和乙醇后180℃反应一段时间,可得到碳包覆的单斜MoO2纳米带。通过对合成条件的探索,可以发现葡萄糖在α-MoO3纳米带表面的缩聚和焦化形成保护层的作用,有效防止了其在被乙醇还原过程中坍塌。所得MoO2@C纳米带含碳量23.81%,比表面积46.85 m2/g。500 mA/g电流密度下恒流充放电,该材料首次可逆容量达600 mAh/g,30次循环后仍能保持在550mAh/g。电流密度上升到1 000mA/g,首次可逆容量接近500mAh/g,30次循环后仍可保持在300mAh/g。
此外,还以微米级MoO3为前驱体,乙二胺为还原剂,Fe2O3为辅助剂,通过水热法合成了银耳状六方MoO2。该材料具有多级结构,它由超薄MoO2纳米片(厚约10 nm)组成外观形貌,内部包裹辅助剂Fe2O3。在70 mA/g电流密度下,银耳状MoO2可逆容量可达650mAh/g;当电流密度提高到10倍700 mA/g,其可逆容量仍然可以保持在300mAh/g左右。
从所合成的MoO2纳米材料的电化学性能可以看出,它们都表现出比微米级MoO2材料更加良好的大电流充放电性能,这与它们尺寸小,比表面积大的形貌结构特征是分不开的。对比三种材料,MoO2@C纳米带表现出最好的性能,这可能是由于它具有适中的尺寸、一维形貌和完好的碳包覆层,这三个因素使其在大电流下既具有高的比容量,又保持了良好的循环性能。
3.无序介孔Ge的制备和电化学性能
以GeO2为前驱体、Mg为还原剂,通过机械球磨方法使其发生氧化还原反应,得到Ge、MgO和GeMg：的混合物,然后在盐酸溶液的刻蚀作用下除去MgO和GeMg2,成功制备了无序介孔的Ge单质。通过TEM观察,可以清楚看到无序介孔的存在,氮气等温吸附结果测得其比表面积为49.98 m2/g,主要孔径分布在10nm左右,进一步证明了产物的无序介孔结构。作为锂离子电池负极材料,无序介孔Ge在150 mA/g电流密度下首次可逆容量为944.2mAh/g,20次循环后可逆容量还能保持在789.3mAh/g,表现出比无孔Ge更好的循环性能(无孔Ge首次可逆容量为970.2 mAh/g,20次后衰减至16.1mAh/g)和较好的大倍率性能。
4.碳纳米球的制备和电化学性能
以乳液聚合所得聚丙烯腈(PAN)纳米粒子为前驱体,通过在其表面包覆一层磷酸钛以隔离粒子间相互接触,有效防止了PAN在碳化过程中发生交联和团聚。碳化之后酸洗除去包覆层,得到了平均粒径约为50 nm的纯净碳纳米球。将碳纳米球作为锂离子电池负极材料测试了其电化学性能。循环伏安法测得其表观扩散系数为1.59×10-cm2/s,在5 mA/cm2(约720.0 mA/g)电流密度下首次可逆容量为131.3mAh/g,表现出比石墨微球更好的倍率性能。
5.氧化物包覆石墨材料在丙烯碳酸酯(PC)基电解液中的电化学性能
用MoO3作为包覆材料,在石墨化材料CMS表面进行了改性。研究发现,MoO3包覆层减少了石墨端面在电解液中的暴露。恒流充放电结果显示,MoO3包覆后的CMS有效防止了PC电解液的持续分解和溶剂化Li+在石墨片层中的嵌入,使CMS在PC基电解液中能够可逆储锂。其首次可逆容量达到380mAh/g,
18次循环后可逆容量仍能够保持在300mAh/g(60 mA/g电流密度下恒流充放电),与石墨材料在乙烯碳酸酯(EC)中的容量相当,性能比较令人满意。
The lithium ion battery is now prevailing in many portable electronic devices such as cell phones, digital cameras/videos and laptops due to its longer cycling life and higher energy density than other rechargeable batteries. However, its relatively low charge/discharge rate and safety concerns have limited its use in new applications such as regenerative braking in hybrid electric vehicles (HEVs), power backups, power sources for EVs, and portable power tools, which require both high energy and high power densities. The rate limitations result from a number of factors including low ionic (Li+) and electronic conductivities of electrode materials, and slow insertion/extraction rate of Li+ into the active materials.Recent studies show that decreasing the particle size and enlarging the surface area of electrode materials are effective ways to improve the electrochemical performance, especially the rate capability of electrode materials. So, in my dissertation, the work is focused on the nanostructured materials:the preparation, characterization and electrochemical performace of varies nanostructured electrode materials are discussed.
1.Single crystallineα-MoO3 nanobelts are synthesized with a facile hydrothermal method.Theα-MoO3 nanobelts grow along the direction of [001],with the length of 5-10μm,width of 200～500 nm and thickness of about 50 nm.When used as cathode materials for rechargeable lithium battery,they exhibit good rate performance.At a low current density,30 mA/g, they deliver a discharge capacity of 264 mAh/g in the voltage of 1.5-3.5 V vs. Li+/Li.At a current density of 5000 mA/g (9000 W/kg), they deliver a capacity of 176 mAh/g, and preserve 114 mAh/g after 50 cycles.
2.A series of MoO2 nanomaterials have been synthesized.
Firstly, monoclinic MoO2 nanoparticles are synthesized through reduction of MoO3 with ethanol vapor at 400℃During the reduction process, the starting material (MoO3) collapsed into nanoparticles(～100 nm), and on the nanoparticles remains a semi-graphite carbon layer from ethanol decomposition.As anode materials for lithiumn ion battery, the carbon coated MoO2 nanoparticles displays a reversible capacity of about 318 mAh/g in the initial cycle, with capacity retention of 100% after 20 cycles in the range of 0.01～3.00 V vs. lithium metal at a current density of around 500 mA/g. However, at the same discharge/charge condition, the MoO2 microparticles obtained from reduction of MoO3 with H2 only deliver a reversible capacity less than 175 mAh/g.
Secondly, carbon coated monoclinic MoO2 nanobelts (MoO2@C nanobelts) are synthesized withα-MoO3 nanobelts as precursor, ethanol as reducer and glucose as protector. In the reduction procedure, glucose decomposes on the surface ofα-MoO3 nanobelts, forming an caramel layer which protects the nanobelts from collapse. The MoO2@C nanobelts delivers a reversible capacity of around 600 mAh/g in the initial cycle, and preserve 550 mAh/g after 30 cylces, at a current density of 500 mAh/g in the range of 0.01-3.00 V vs. lithium metal.When the current density increases to 1000 mA/g, the reversible capacity is close to 550 mAh/g, and retains around 300 mAh/g after 30 cycles.
Moreover, tremella-like hexagonal MoO2 was obtained via a Fe2O3-assisted hydrothermal reduction of MoO3 in ethylenediamine aqueous solution.The "tremella" consists of ultrathin MoO2 nanosheets (about 10 nm in thickness),with residual Fe2O3 resting in its body. This structured MoO2 shows a reversible capacity up to 650 mAh/g at a current density of 70 mAh/g in the range of 0.01-3.00 V, and preseves around 300 mAh/g when the current density increase to 70 mAh/g.
The above synthesized nanostructured MoO2 show much better rate capability compared with their micro-sized counterpart, which is highly related with their decreased size, and increased surface areas. And among them, MoO2@C nanobelts present the best electrochemical performance, which may because they have optimum size, one-dimensional morphology and perfect carbon coating.
3.Disordered mesoporous Ge was prepared by mechanochemical reaction of GeO2 and Mg powders followed by an etching process with HC1 solution.With a pore-distribution concentrated around 10 nm, the product presents a BET surface area of 49.98 m2/g. When using as an anode material for lithium ion battery, the mesoporous Ge exhibits a reversible capacity of 950 mAh/g and retains a capacity of 789 mAh/g after 20 cycles at a current density of 150 mA/g. The cycleability is significantly improved compared with nonporous Ge.
4.A low-cost and practical route to prepare carbon nanospheres (CNSs) from pyrolysis of polyacrylonitrile (PAN) nanospheres is introduced.A layer of titanium phosphate is coated on the surface of PAN nanospheres before the carbonization process, which effectively prevents the crosslinking and aggregation of PAN nanoparticles under high temperature. After removal of the coating following the carbonization, CNSs with average size of 50 nm are obtained.The CNSs, with the Li+ diffusion coefficient of 1.59×10-9 cm2/s, present better rate capability compared with carbonaceous mesophase spheres (CMS) as anode material for lithium ion battery.
5.Besides the synthesis of nanostructured electrode materials, CMS@MoO3 composite was prepared by coating MoO3 on CMS in order to improve the performance of graphite as an anode for lithium ion battery in propylene carbonate (PC)-based electrolyte. The coated MoO3 layer acts as a protective layer which separates graphite from PC-based electrolyte solution.Cyclic voltammograms and discharge/charge measurement suggest that the cointercalation of PC is suppressed and lithium ions can reversibly intercalate into and deintercalate from the CMS@MoO3.CMS with the optimum amount of MoO3(14.4 wt.% of the composite) presents the best electrochemical performance:it delivers a reversible capacity of 380 mAh/g in 1 M LiClO4 solution of PC/DMC (1:1,v/v), and preserves above 300 mAh/g after 18 cycles.
本论文从纳米材料出发,以MoOx、Ge、C为研究客体,探索了多种形貌纳米材料的合成条件及规律,进一步扩充了纳米材料库；测试了它们在大电流密度下的充放电性能,并着重考察了MoO2纳米材料电化学性能与其结构形貌的关系。主要内容包括：
1.a-MoO3纳米带的制备和电化学性能研究
通过水热法制备了单晶α-MoO3纳米带。该纳米带材料长5-10μm,宽200-500 nm,厚约50 nm,沿着[001]方向生长。作为锂离子电池正极材料,α-MOO3纳米带在30 mA/g电流密度下表现出264mAh/g的容量;当电流密度上升到5000mA/g时,容量达176mAh/gi(能量密度300Wh/kg,功率密度9000 W/kg),50次循环后容量还能保持到114mAh/g。相比微米级MoO3纳米材料在5000mA/g电流密度下容量不到70mAh/g,MoO3纳米带表现出更优越的倍率性能。
2.系列MoO2纳米材料的制备和电化学性能研究
首先,利用乙醇蒸汽还原法制得MOO2纳米颗粒。相比传统制备MOo2采用H2还原MoO3的方法,采用乙醇蒸汽替代H2,更加便宜、安全,而且还原温度降低,节约了能源。乙醇蒸汽在400℃6下还原MoO3,得到表面有半石墨化碳包覆的粒径约为100nm的单斜MoO2颗粒。该产物在500 mA/g的电流密度下首次充放电表现出约320mAh/g的可逆容量,20次循环几乎没有衰减。而H2还原MoO3所得MoO2微米颗粒在500 mA/g电流密度下可逆容量不到175mAh/g。可见乙醇蒸汽还原所得的MoO2表现出良好的大电流放电性能。
同时,本文还关注MoO2一维纳米结构的合成。文献报道的一维MoO2纳米线和纳米棒主要是通过电化学沉积或气相沉积来制备,这些方法比较复杂,产物较难控制,产量低。用α-MoO3纳米带作为前驱体分散在水中,加入葡萄糖和乙醇后180℃反应一段时间,可得到碳包覆的单斜MoO2纳米带。通过对合成条件的探索,可以发现葡萄糖在α-MoO3纳米带表面的缩聚和焦化形成保护层的作用,有效防止了其在被乙醇还原过程中坍塌。所得MoO2@C纳米带含碳量23.81%,比表面积46.85 m2/g。500 mA/g电流密度下恒流充放电,该材料首次可逆容量达600 mAh/g,30次循环后仍能保持在550mAh/g。电流密度上升到1 000mA/g,首次可逆容量接近500mAh/g,30次循环后仍可保持在300mAh/g。
此外,还以微米级MoO3为前驱体,乙二胺为还原剂,Fe2O3为辅助剂,通过水热法合成了银耳状六方MoO2。该材料具有多级结构,它由超薄MoO2纳米片(厚约10 nm)组成外观形貌,内部包裹辅助剂Fe2O3。在70 mA/g电流密度下,银耳状MoO2可逆容量可达650mAh/g;当电流密度提高到10倍700 mA/g,其可逆容量仍然可以保持在300mAh/g左右。
从所合成的MoO2纳米材料的电化学性能可以看出,它们都表现出比微米级MoO2材料更加良好的大电流充放电性能,这与它们尺寸小,比表面积大的形貌结构特征是分不开的。对比三种材料,MoO2@C纳米带表现出最好的性能,这可能是由于它具有适中的尺寸、一维形貌和完好的碳包覆层,这三个因素使其在大电流下既具有高的比容量,又保持了良好的循环性能。
3.无序介孔Ge的制备和电化学性能
以GeO2为前驱体、Mg为还原剂,通过机械球磨方法使其发生氧化还原反应,得到Ge、MgO和GeMg：的混合物,然后在盐酸溶液的刻蚀作用下除去MgO和GeMg2,成功制备了无序介孔的Ge单质。通过TEM观察,可以清楚看到无序介孔的存在,氮气等温吸附结果测得其比表面积为49.98 m2/g,主要孔径分布在10nm左右,进一步证明了产物的无序介孔结构。作为锂离子电池负极材料,无序介孔Ge在150 mA/g电流密度下首次可逆容量为944.2mAh/g,20次循环后可逆容量还能保持在789.3mAh/g,表现出比无孔Ge更好的循环性能(无孔Ge首次可逆容量为970.2 mAh/g,20次后衰减至16.1mAh/g)和较好的大倍率性能。
4.碳纳米球的制备和电化学性能
以乳液聚合所得聚丙烯腈(PAN)纳米粒子为前驱体,通过在其表面包覆一层磷酸钛以隔离粒子间相互接触,有效防止了PAN在碳化过程中发生交联和团聚。碳化之后酸洗除去包覆层,得到了平均粒径约为50 nm的纯净碳纳米球。将碳纳米球作为锂离子电池负极材料测试了其电化学性能。循环伏安法测得其表观扩散系数为1.59×10-cm2/s,在5 mA/cm2(约720.0 mA/g)电流密度下首次可逆容量为131.3mAh/g,表现出比石墨微球更好的倍率性能。
5.氧化物包覆石墨材料在丙烯碳酸酯(PC)基电解液中的电化学性能
用MoO3作为包覆材料,在石墨化材料CMS表面进行了改性。研究发现,MoO3包覆层减少了石墨端面在电解液中的暴露。恒流充放电结果显示,MoO3包覆后的CMS有效防止了PC电解液的持续分解和溶剂化Li+在石墨片层中的嵌入,使CMS在PC基电解液中能够可逆储锂。其首次可逆容量达到380mAh/g,
18次循环后可逆容量仍能够保持在300mAh/g(60 mA/g电流密度下恒流充放电),与石墨材料在乙烯碳酸酯(EC)中的容量相当,性能比较令人满意。
The lithium ion battery is now prevailing in many portable electronic devices such as cell phones, digital cameras/videos and laptops due to its longer cycling life and higher energy density than other rechargeable batteries. However, its relatively low charge/discharge rate and safety concerns have limited its use in new applications such as regenerative braking in hybrid electric vehicles (HEVs), power backups, power sources for EVs, and portable power tools, which require both high energy and high power densities. The rate limitations result from a number of factors including low ionic (Li+) and electronic conductivities of electrode materials, and slow insertion/extraction rate of Li+ into the active materials.Recent studies show that decreasing the particle size and enlarging the surface area of electrode materials are effective ways to improve the electrochemical performance, especially the rate capability of electrode materials. So, in my dissertation, the work is focused on the nanostructured materials:the preparation, characterization and electrochemical performace of varies nanostructured electrode materials are discussed.
1.Single crystallineα-MoO3 nanobelts are synthesized with a facile hydrothermal method.Theα-MoO3 nanobelts grow along the direction of [001],with the length of 5-10μm,width of 200～500 nm and thickness of about 50 nm.When used as cathode materials for rechargeable lithium battery,they exhibit good rate performance.At a low current density,30 mA/g, they deliver a discharge capacity of 264 mAh/g in the voltage of 1.5-3.5 V vs. Li+/Li.At a current density of 5000 mA/g (9000 W/kg), they deliver a capacity of 176 mAh/g, and preserve 114 mAh/g after 50 cycles.
2.A series of MoO2 nanomaterials have been synthesized.
Firstly, monoclinic MoO2 nanoparticles are synthesized through reduction of MoO3 with ethanol vapor at 400℃During the reduction process, the starting material (MoO3) collapsed into nanoparticles(～100 nm), and on the nanoparticles remains a semi-graphite carbon layer from ethanol decomposition.As anode materials for lithiumn ion battery, the carbon coated MoO2 nanoparticles displays a reversible capacity of about 318 mAh/g in the initial cycle, with capacity retention of 100% after 20 cycles in the range of 0.01～3.00 V vs. lithium metal at a current density of around 500 mA/g. However, at the same discharge/charge condition, the MoO2 microparticles obtained from reduction of MoO3 with H2 only deliver a reversible capacity less than 175 mAh/g.
Secondly, carbon coated monoclinic MoO2 nanobelts (MoO2@C nanobelts) are synthesized withα-MoO3 nanobelts as precursor, ethanol as reducer and glucose as protector. In the reduction procedure, glucose decomposes on the surface ofα-MoO3 nanobelts, forming an caramel layer which protects the nanobelts from collapse. The MoO2@C nanobelts delivers a reversible capacity of around 600 mAh/g in the initial cycle, and preserve 550 mAh/g after 30 cylces, at a current density of 500 mAh/g in the range of 0.01-3.00 V vs. lithium metal.When the current density increases to 1000 mA/g, the reversible capacity is close to 550 mAh/g, and retains around 300 mAh/g after 30 cycles.
Moreover, tremella-like hexagonal MoO2 was obtained via a Fe2O3-assisted hydrothermal reduction of MoO3 in ethylenediamine aqueous solution.The "tremella" consists of ultrathin MoO2 nanosheets (about 10 nm in thickness),with residual Fe2O3 resting in its body. This structured MoO2 shows a reversible capacity up to 650 mAh/g at a current density of 70 mAh/g in the range of 0.01-3.00 V, and preseves around 300 mAh/g when the current density increase to 70 mAh/g.
The above synthesized nanostructured MoO2 show much better rate capability compared with their micro-sized counterpart, which is highly related with their decreased size, and increased surface areas. And among them, MoO2@C nanobelts present the best electrochemical performance, which may because they have optimum size, one-dimensional morphology and perfect carbon coating.
3.Disordered mesoporous Ge was prepared by mechanochemical reaction of GeO2 and Mg powders followed by an etching process with HC1 solution.With a pore-distribution concentrated around 10 nm, the product presents a BET surface area of 49.98 m2/g. When using as an anode material for lithium ion battery, the mesoporous Ge exhibits a reversible capacity of 950 mAh/g and retains a capacity of 789 mAh/g after 20 cycles at a current density of 150 mA/g. The cycleability is significantly improved compared with nonporous Ge.
4.A low-cost and practical route to prepare carbon nanospheres (CNSs) from pyrolysis of polyacrylonitrile (PAN) nanospheres is introduced.A layer of titanium phosphate is coated on the surface of PAN nanospheres before the carbonization process, which effectively prevents the crosslinking and aggregation of PAN nanoparticles under high temperature. After removal of the coating following the carbonization, CNSs with average size of 50 nm are obtained.The CNSs, with the Li+ diffusion coefficient of 1.59×10-9 cm2/s, present better rate capability compared with carbonaceous mesophase spheres (CMS) as anode material for lithium ion battery.
5.Besides the synthesis of nanostructured electrode materials, CMS@MoO3 composite was prepared by coating MoO3 on CMS in order to improve the performance of graphite as an anode for lithium ion battery in propylene carbonate (PC)-based electrolyte. The coated MoO3 layer acts as a protective layer which separates graphite from PC-based electrolyte solution.Cyclic voltammograms and discharge/charge measurement suggest that the cointercalation of PC is suppressed and lithium ions can reversibly intercalate into and deintercalate from the CMS@MoO3.CMS with the optimum amount of MoO3(14.4 wt.% of the composite) presents the best electrochemical performance:it delivers a reversible capacity of 380 mAh/g in 1 M LiClO4 solution of PC/DMC (1:1,v/v), and preserves above 300 mAh/g after 18 cycles.
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