CN102265434B - 用于锂二次电池的正极活性材料 - Google Patents
用于锂二次电池的正极活性材料 Download PDFInfo
- Publication number
- CN102265434B CN102265434B CN201080003774.XA CN201080003774A CN102265434B CN 102265434 B CN102265434 B CN 102265434B CN 201080003774 A CN201080003774 A CN 201080003774A CN 102265434 B CN102265434 B CN 102265434B
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- Prior art keywords
- fluoropolymer resin
- positive electrode
- lithium
- metal oxide
- carbon particle
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- 239000007774 positive electrode material Substances 0.000 title claims abstract description 36
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 34
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 33
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 48
- 239000002245 particle Substances 0.000 claims abstract description 37
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 claims abstract description 27
- 239000003792 electrolyte Substances 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 229920002313 fluoropolymer Polymers 0.000 claims description 42
- 239000004811 fluoropolymer Substances 0.000 claims description 42
- 229920005989 resin Polymers 0.000 claims description 42
- 239000011347 resin Substances 0.000 claims description 42
- -1 polyethylene Polymers 0.000 claims description 21
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 239000004020 conductor Substances 0.000 claims description 9
- 239000000853 adhesive Substances 0.000 claims description 8
- 230000001070 adhesive effect Effects 0.000 claims description 8
- 239000004698 Polyethylene Substances 0.000 claims description 6
- 230000009849 deactivation Effects 0.000 claims description 6
- 229920000573 polyethylene Polymers 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 4
- 229910012427 LiNi0.53Mn0.27Co0.20O2 Inorganic materials 0.000 claims description 3
- 229910012748 LiNi0.5Mn0.3Co0.2O2 Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002952 polymeric resin Substances 0.000 abstract description 4
- 229920003002 synthetic resin Polymers 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 239000011149 active material Substances 0.000 description 25
- 230000000052 comparative effect Effects 0.000 description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 13
- 239000000126 substance Substances 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 12
- 239000000203 mixture Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 9
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- 229910052759 nickel Inorganic materials 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
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- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 238000011160 research Methods 0.000 description 5
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- 239000010936 titanium Substances 0.000 description 5
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
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- 125000000524 functional group Chemical group 0.000 description 4
- 229910003002 lithium salt Inorganic materials 0.000 description 4
- 159000000002 lithium salts Chemical class 0.000 description 4
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 229910014689 LiMnO Inorganic materials 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
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- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
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- HCLJOFJIQIJXHS-UHFFFAOYSA-N 2-[2-[2-(2-prop-2-enoyloxyethoxy)ethoxy]ethoxy]ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOCCOCCOC(=O)C=C HCLJOFJIQIJXHS-UHFFFAOYSA-N 0.000 description 2
- SZNYYWIUQFZLLT-UHFFFAOYSA-N 2-methyl-1-(2-methylpropoxy)propane Chemical compound CC(C)COCC(C)C SZNYYWIUQFZLLT-UHFFFAOYSA-N 0.000 description 2
- PFCHFHIRKBAQGU-UHFFFAOYSA-N 3-hexanone Chemical compound CCCC(=O)CC PFCHFHIRKBAQGU-UHFFFAOYSA-N 0.000 description 2
- YYPNJNDODFVZLE-UHFFFAOYSA-N 3-methylbut-2-enoic acid Chemical compound CC(C)=CC(O)=O YYPNJNDODFVZLE-UHFFFAOYSA-N 0.000 description 2
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 2
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- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
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- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
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- KLARSDUHONHPRF-UHFFFAOYSA-N [Li].[Mn] Chemical compound [Li].[Mn] KLARSDUHONHPRF-UHFFFAOYSA-N 0.000 description 2
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- 229910052733 gallium Inorganic materials 0.000 description 1
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- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
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- H01M4/00—Electrodes
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60L—PROPULSION OF ELECTRICALLY-PROPELLED VEHICLES; SUPPLYING ELECTRIC POWER FOR AUXILIARY EQUIPMENT OF ELECTRICALLY-PROPELLED VEHICLES; ELECTRODYNAMIC BRAKE SYSTEMS FOR VEHICLES IN GENERAL; MAGNETIC SUSPENSION OR LEVITATION FOR VEHICLES; MONITORING OPERATING VARIABLES OF ELECTRICALLY-PROPELLED VEHICLES; ELECTRIC SAFETY DEVICES FOR ELECTRICALLY-PROPELLED VEHICLES
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- B60L50/50—Electric propulsion with power supplied within the vehicle using propulsion power supplied by batteries or fuel cells
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
本发明公开了一种锂二次电池用正极活性材料,其包含锂过渡金属氧化物,其中利用碳粒子和聚合物树脂在所述锂过渡金属氧化物的表面对其进行涂覆,所述聚合物树脂是因锂二次电池用电解质和有机溶剂而被惰性化的物质且所述聚合物树脂具有至少80℃的熔点。具有所公开的正极活性材料的锂二次电池具有提高的倍率性能和高温稳定性的优势,从而提供了优异的单电池特性。
Description
技术领域
本发明涉及一种正极活性材料,更特别地,涉及包含锂过渡金属氧化物的正极活性材料,其中所述锂过渡金属氧化物在表面涂覆有碳粒子和聚合物树脂,所述聚合物树脂因锂二次电池用电解质和有机溶剂而被惰性化且所述聚合物树脂具有至少80℃的熔点。
背景技术
随着移动设备的技术进步和需求,对作为能源的二次电池的需求急剧增加。
特别地,随着人们对环境问题关注的增加,已经针对电动车辆和混合电动车辆进行了大量研究,从而取代使用化石燃料的常规汽车如汽油车辆、柴油车辆等,所述常规汽车已成空气污染的主因。这种电动车辆或混合电动车辆通常使用镍金属氢化物电池型电源来驱动,然而,具有高能量密度和放电电压的锂二次电池目前正在积极研究当中且在相关领域中已部分实现了商业化。
尽管通常使用碳物质制备锂二次电池用负极活性材料,但是也已经提出使用锂金属或硫化合物。至于锂二次电池用正极活性材料,广泛使用含锂的钴氧化物(LiCoO2)。另外,还可使用其他锂过渡金属氧化物如含锂的锰氧化物如具有层状晶体结构的LiMnO2、具有尖晶石晶体结构的LiMn2O4等以及含锂的镍氧化物(LiNiO2)。
然而,用于正极活性材料的这种锂过渡金属氧化物因非水电解质的离子传导率低而具有电导率低且充放电倍率(rate)性能不足的劣势。
为了解决这种问题,已经提出了一些常规技术如对正极活性材料的表面进行涂覆或对所述正极活性材料进行表面处理。例如,为了降低正极活性材料与电解质之间的界面的接触电阻或者为了减少在高温下产生的副产物,已经公开了一种利用导电聚合物的正极活性材料的涂覆方法,所述方法包括将导电材料涂布到正极活性材料上。然而,仍需要开发具有充分单电池特性的改进的正极活性材料。
此外,高能量密度意味着可能遭受危险且诸如燃烧、爆炸等的危险会随着能量密度的提高而变得更加严重。
因此,尽管对不同的方法进行了广泛的调查和研究,但是尚未获得令人满意的结果。
因为能量密度的增大与移动设备的复杂性和多功能性的增加成比例,所以所述移动设备的安全性更为重要且应进一步提高用于EV、HEV、电动工具等的锂二次电池的倍率性能。
然而,由于安全性与倍率性能具有基本上矛盾的趋势,所以同时提高上述两种特性非常困难且目前对所述问题的研究和/或讨论非常少。
发明内容
技术问题
因此,本发明旨在解决上述现有技术中的问题并克服相关领域中的技术限制。
作为本发明人进行的广泛研究和大量实验的结果,发现,通过将碳粒子和聚合物树脂涂布到锂过渡金属氧化物的表面上而制备的正极活性材料可获得提高的电导率和离子传导率,由此提供了优异的倍率性能并提高了高温稳定性。从而成功地完成了本发明。
技术方案
因此,本发明提供了一种包含锂过渡金属氧化物的正极活性材料,其中所述锂过渡金属氧化物在表面涂覆有碳粒子和聚合物树脂,所述聚合物树脂因锂二次电池用电解质和有机溶剂而被惰性化且所述聚合物树脂具有至少80℃的熔点。
通过将碳粒子和聚合物树脂涂布至锂过渡金属氧化物的表面而制备的本发明正极活性材料可具有高电导率和离子传导率,从而显示出优异的倍率性能,同时保持高温稳定性。
另外,本发明人发现,向作为正极活性材料的锂过渡金属氧化物的表面涂布碳粒子和聚合物树脂提供了基于上述物质相互作用的协同效应。因此,与单独添加碳粒子或聚合物树脂相比,可明显提高单电池性能和高温稳定性。这一事实的原因在于,碳粒子增大了电导率和离子传导率,从而提高了倍率性能。此外,在80℃以上熔化的聚合物树脂可在电池的反常高温状态下增大内阻,从而防止离子和电子的迁移,由此抑制电池的燃烧和/或爆炸并提高高温稳定性。
涂布至正极活性材料表面的碳粒子没有特别限制,只要其能够增加电导率和离子传导率,由此提高倍率性能即可。所述碳粒子的非限制性实例可包括:石墨材料如天然石墨、人造石墨等;碳黑如碳黑、乙炔黑、科琴(ketchen)黑、槽法碳黑、炉黑、灯黑、夏黑等;或碳纤维等。这些材料可单独使用或以其两种以上组合的方式使用。
如果所述碳粒子的尺寸太小,则因粒子聚集而造成分散性下降且可能难以进行均匀涂覆。另一方面,如果碳粒子的尺寸太大,则难以利用碳粒子对锂过渡金属氧化物的表面进行界面涂覆,从而使得传导率不足。考虑到这些状况,碳基粒子可具有0.01~1μm的粒径。
碳粒子的涂布可提高倍率性能,然而,可任选地使高温稳定性劣化。因此,本发明采用对正极活性材料的表面同时涂布聚合物树脂和碳粒子。
所述聚合物树脂因锂二次电池用电解质和有机溶剂而被惰性化且所述聚合物树脂具有至少80℃的熔点。
由于所述聚合物树脂因电解质和/或有机溶剂而被惰性化,所以在电极的制造期间所述聚合物树脂不被除去,和/或当在电池中含有所述聚合物树脂时,所述聚合物树脂不被溶出至电解质中或不发生降解,从而有利地防止单电池性能的下降。此外,在电池的内部温度超过80℃之后,所述聚合物树脂熔化,然后烧焦并粘着至正极活性材料的表面上或流入正极活性材料的间隙中,由此降低离子和电子的迁移率。因此,通过提高电池的内阻,可防止电化学反应的进行,从而抑制电池的燃烧。
这种聚合物树脂没有特别限制,条件是可实现上述特性,然而其非限制性实例可以为选自如下的至少一种:聚乙烯、聚丙烯、聚丁烯和聚苯乙烯、包含其两种以上的共聚物或共混物。
所述聚合物树脂可具有80~200℃的熔点。如果熔点小于80℃,则即使在正常工作条件下也可使内阻增大,由此降低了单电池的特性。当熔点大于200℃时,难以获得期望的高温稳定性。
如果聚合物树脂的含量太大,则内阻增大且可能难以获得因添加碳粒子而带来的电导率和离子传导率的提高。另一方面,当聚合物树脂含量太小时,可能不能获得充分的高温稳定性。或者,随着碳粒子的含量增大,电导率提高,然而,聚合物树脂的涂覆面积相对变小且可能很少获得高温稳定性的提高。此外,涂布到锂过渡金属氧化物上的碳粒子对聚合物树脂的相对含量比可为90∶10~10∶90(重量%)。
所述碳粒子和所述聚合物树脂可各自为涂布至锂过渡金属氧化物表面的独立相、或者为碳粒子被捕集入聚合物树脂内部的复合形式。
可通过化学键合将所述碳粒子和聚合物树脂与锂过渡金属氧化物的表面结合在一起,但考虑到处理简易性和锂过渡金属氧化物的稳定性,优选通过物理接触如范德华力或静电力等来进行结合。
通过使用例如用于融合的机械融合装置或Nobilta设备的简单方法,可实现这种物理接触。所述机械融合装置在干燥状态下利用物理旋转来制备混合物,从而形成构成成分的静电耦合。
要实现本发明的功能效果,不必利用上述碳粒子和聚合物树脂完全涂覆锂过渡金属氧化物。如果碳粒子和聚合物树脂两者的涂覆面积过大,则锂离子的迁移率下降且倍率性能可能劣化。当涂覆面积太小时,可能不能获得期望的效果。因此,优选利用上述碳粒子和聚合物树脂涂覆锂过渡金属氧化物总表面的约20~80%。
如果涂覆量太小,则可能难以获得涂覆效果。相反,当涂覆量太大时,单电池性能可能劣化。因此,相对于活性材料的总重量,涂覆量可以为0.5~10重量%。
电解质包含锂盐和非水溶剂,且所述锂盐为溶于非水溶剂中以充当电池中的锂离子源的材料,从而使得典型的锂二次电池能够运行,并促进了锂离子在正极和负极之间的移动。这种锂盐可包括例如LiCl、LiBr、LiI、LiClO4、LiBF4、LiB10Cl10、LiPF6、LiCF3SO3、LiCF3CO2、LiAsF6、LiSbF6、LiAlCl4、CH3SO3Li、CF3SO3Li、(CF3SO2)2NLi、氯硼烷锂、低级脂族羧酸锂、四苯基硼酸锂、酰亚胺等。
非水有机溶剂充当用于传输电化学反应性离子的介质。这种非水溶剂可以为非质子溶剂,包括例如:N-甲基-2-吡咯烷酮、碳酸亚丙酯、碳酸亚乙酯、碳酸亚丁酯、碳酸二甲酯、碳酸二乙酯、γ-丁内酯、1,2-二甲氧基乙烷、四羟基呋喃、2-甲基四氢呋喃、二甲亚砜、1,3-二氧戊环、甲酰胺、二甲基甲酰胺、二氧戊环、乙腈、硝基甲烷、甲酸甲酯、乙酸甲酯、磷酸三酯、三甲氧基甲烷、二氧戊环衍生物、环丁砜、甲基环丁砜、1,3-二甲基-2-咪唑烷酮、碳酸亚丙酯衍生物、四氢呋喃衍生物、醚、丙酸甲酯、丙酸乙酯等。当使用上述有机溶剂的两种以上的混合物时,本领域技术人员应理解到,可考虑单电池性能而适当调节其混合比。
所述有机溶剂还可以为用于制备正极制造用浆体的分散溶剂,例如:水;醇类如甲醇、乙醇、丙醇、异丙醇、丁醇、异丁醇、仲丁醇、叔丁醇、戊醇、异戊醇、己醇等;酮类如丙酮、甲基乙基酮、甲基丙基酮、乙基丙基酮、环戊酮、环己酮、环庚酮等;醚类如甲基乙基醚、二乙醚、二丙醚、二异丙醚、二丁醚、二异丁醚、二正戊醚、二异戊醚、甲基丙基醚、甲基异丙基醚、甲基丁基醚、乙基丙基醚、乙基异丁基醚、乙基正戊基醚、乙基异戊基醚、四氢呋喃等;内酯类如γ-丁内酯、δ-丁内酯等;内酰胺类如β-内酰胺;脂环族化合物如环戊烷、环己烷、环庚烷等;芳族烃如苯、甲苯、邻二甲苯、间二甲苯、对二甲苯、乙苯、丙苯、异丙苯、丁苯、异丁苯、正戊苯等;脂族烃如庚烷、辛烷、壬烷、癸烷等;链或环状酰胺如N-甲基吡咯烷酮;酯类如乳酸甲酯、乳酸乙酯、乳酸丙酯、乳酸丁酯、苯甲酸甲酯等;用于形成电解质溶剂的液体物质,但是当然不限于此。可以以其两种至五种的组合的方式使用上述分散溶剂。
优选地,所述有机溶剂可以为NMP、氯仿、DMSO、碳酸烷基酯等。
因此,本发明的聚合物树脂可以为因上述电解质和有机溶剂而被惰性化的物质,其具有在上文限定的范围内的熔点。
所述正极活性材料没有特别限制,只要其包含能够吸收和释放锂离子的锂过渡金属氧化物即可,且可包括例如:层状化合物如锂钴氧化物(LiCoO2)、锂镍氧化物(LiNiO2)等、或由一种以上过渡金属取代的化合物;由Li1+yMn2-yO4(其中y为0~0.33)表示的锂锰化合物、LiMnO3、LiMn2O3、LiMnO2等;锂铜氧化物(Li2CuO2);钒氧化物如LiV3O8、LiFe3O4、V2O5、Cu2V2O7等;由LiNi1-yMyO2(其中M=Co、Mn、Al、Cu、Fe、Mg、B或Ga且y为0.01~0.3)表示的Ni位点型锂镍氧化物;由LiMn2-yMyO2(其中M=Co、Ni、Fe、Cr、Zn或Ta,且y为0.01~0.1)或Li2Mn3MO8(其中M=Fe、Co、Ni、Cu或Zn)表示的复合锂锰化合物;Li被碱土金属部分取代的LiMn2O4;二硫化物;FeX(MoO4)3等,但不特别限制于此。
根据本发明的优选实施方式,所述锂过渡金属氧化物可以为LizNi1-x-yCoxMnyO2(0≤x≤1,0≤y≤1,0≤x+y≤1,0.95≤z≤1.15)。
上述锂镍-钴-锰氧化物具有优异的循环性能和容量,但高温稳定性下降。因此,如果根据本发明利用碳粒子和聚合物树脂对这种氧化物进行涂覆,则可获得改进的倍率性能和高温稳定性、以及高容量,由此显示非常优异的单电池特性。
本发明还提供一种含有上述正极活性材料的锂二次电池。所述锂二次电池可包含例如正极、负极、隔板和含锂盐的非水电解质。
通过例如向正极集电体涂布正极活性材料、导电材料和粘合剂的混合物并对涂覆的集电体进行干燥来制造正极。任选地,可向所述混合物中添加填料。通过向负极集电体涂布负极活性材料并对涂覆的集电体进行干燥来制造负极,如果需要,所述负极可还包含上述成分。
所述负极活性材料可包括例如:碳和石墨材料如天然石墨、人造石墨、可膨胀石墨、碳纤维、硬碳、碳黑、碳纳米管、富勒烯、活性碳等;可与锂形成合金的金属如Al、Si、Sn、Ag、Bi、Mg、Zn、In、Ge、Pb、Pd、Pt、Ti等以及含所述金属的化合物;金属及其与碳和石墨材料的化合物的复合材料;含锂的氮化物等。
其中,更优选碳基活性材料、硅基活性材料、锡基活性材料和/或硅-碳基活性材料,其可单独或以其两种以上组合的方式使用。
所述隔板设置在所述正极与所述负极之间,且所述隔板由具有高离子渗透率和优异机械强度的薄绝缘膜构成。隔板中各个孔的直径通常为0.01~10μm且其厚度通常为5~300μm。可使用片或无纺布来制造这种隔板,所述片或无纺布由例如烯烃聚合物如具有耐化学性和疏水性的聚丙烯、玻璃纤维或聚乙烯制成。当使用固体电解质如聚合物电解质时,这种电解质也可充当隔板。
所述隔板的另一个实例可以为具有活性膜的有机/无机复合多孔隔板,其特征在于,选自活性膜中的一部分多孔区域、聚烯烃基隔板基材、和基材表面中的至少一个区域涂覆有无机粒子与粘合剂聚合物的混合物。任选地,所述无机粒子可涂布至电极侧面。
这种无机粒子可包括例如具有5以上介电常数的无机粒子、显示压电性能的无机粒子、具有锂离子转运能力的无机粒子等。
所述粘合剂可包括例如:聚偏二氟乙烯、聚乙烯醇、羧甲基纤维素(CMC)、淀粉、羟丙基纤维素、再生纤维素、聚乙烯基吡咯烷酮、四氟乙烯、聚乙烯、聚丙烯、乙烯-丙烯-二烯三元共聚物(EPDM)、磺化的EPDM、苯乙烯-丁烯橡胶、氟橡胶、不同的共聚物、高度皂化的聚乙烯醇等。
使用导电材料来提高电极活性材料的电导率,且相对于电极混合物的总重量可以以1~20重量%的量添加所述导电材料。所述导电材料没有特别限制,只要其显示电导率而不会造成电池的化学变化即可。例如,所述导电材料可包括:石墨如天然石墨或人造石墨;碳黑如碳黑、乙炔黑、科琴黑、槽法碳黑、炉黑、灯黑、夏黑等;导电纤维如包括碳纳米管或富勒烯的碳衍生物、碳纤维、金属纤维等;金属粉末如碳氟化物、铝或镍粉;导电晶须如氧化锌、钛酸钾等;导电金属氧化物如二氧化钛;导电材料如聚亚苯基衍生物等。
粘度控制剂是指调节电极混合物的粘度以有助于更容易地将电极混合物共混并涂布到集电体上的过程的成分。相对于电极混合物的总重量,优选以最高达30重量%的量添加所述粘度控制剂。这种粘度控制剂的实例可包括羧甲基纤维素、聚偏二氟乙烯等,但是当然不限于此。任选地,上述溶剂也可充当粘度控制剂。
本文中所使用的填料是用于抑制电极膨胀的附加成分,所述填料没有特别限制,只要其包含纤维状材料而不会造成电池的化学变化即可。例如,可使用烯烃基聚合物如聚乙烯、聚丙烯等或纤维状材料如玻璃纤维、碳纤维等形成所述填料。
偶联剂是用于提高电极活性材料与粘合剂之间粘附性的另一种附加成分,其特征在于具有至少两个官能团,且相对于粘合剂的重量可以以最高达30重量%的量使用所述偶联剂。这种偶联剂的实例可以为具有至少两个官能团的材料,其中一个官能团与存在于硅、锡或石墨基活性材料表面上的羟基或羧基发生反应而形成化学键,同时另一个官能团与聚合物粘合剂发生反应而形成另一个化学键。偶联剂的优选实例可以为硅烷基偶联剂,其包括:三乙氧基甲硅烷基丙基四硫化物、巯丙基三乙氧基硅烷、氨丙基三乙氧基硅烷、氯丙基三乙氧基硅烷、乙烯基三乙氧基硅烷、甲基丙烯酰氧基丙基三乙氧基硅烷、环氧丙氧基丙基三乙氧基硅烷、异氰酸根合丙基三乙氧基硅烷、氰酸根合丙基三乙氧基硅烷等,但不特别限制于此。
本文中使用的粘附促进剂是用于提高活性材料对集电体粘附性的附加成分,且相对于粘合剂可以以不超过10重量%的量添加所述粘附促进剂。所述粘附促进剂的实例可包括草酸、己二酸、甲酸、丙烯酸衍生物、衣康酸衍生物等。
分子量控制剂可包括例如叔十二烷基硫醇、正十二烷基硫醇、正辛基硫醇等。交联剂可包括例如1,3-丁二醇二丙烯酸酯、1,3-丁二醇二甲基丙烯酸酯、1,4-丁二醇二丙烯酸酯、1,4-丁二醇二甲基丙烯酸酯、丙烯酸芳基酯、甲基丙烯酸芳基酯、三羟甲基丙烷三丙烯酸酯、四乙二醇二丙烯酸酯、四乙二醇二甲基丙烯酸酯、二乙烯基苯等。
所述电极的集电体是在活性材料的电化学反应期间电子发生移动的部分,基于电极的类型,可将所述集电体分为负极集电体和正极集电体。
通常以3~500μm的厚度制造负极集电体。负极集电体的材料没有特别限制,只要所述负极集电体显示电导率且不会造成电池的化学变化即可,所述负极集电体可包括例如铜、不锈钢、铝、镍、钛、煅烧碳,或者利用碳、镍、钛、银等表面处理过的铜或不锈钢,或者铝-镉合金等。
通常以3~500μm的厚度制造正极集电体。正极集电体的材料没有特别限制,只要所述正极集电体显示高电导率且不会造成电池的化学变化即可,所述正极集电体可包括例如不锈钢、铝、镍、钛、煅烧碳,或者利用碳、镍、钛、银等表面处理过的铝或不锈钢。
所述集电体可在其表面上形成微细的凹凸,从而增强电极活性材料的粘合,且可以以不同的形式如膜、片、箔、网、多孔体、泡沫、无纺布等来利用所述集电体。
可根据相关领域中已知的任何常规方法来制造本发明的锂二次电池。关于本发明的锂二次电池,正极、负极和隔板的构造没有特别限制,例如可以在圆形、角形或袋形箱中以卷绕或堆叠的形式放置各种片。
可将本发明的锂二次电池用于需要优异的倍率性能和高温稳定性的各种装置中,例如:由电动机驱动的电动工具;电动汽车如电动车辆(EV)、混合电动车辆(HEV)、插电式混合电动车辆(PHEV)等;电动双轮车辆如电动自行车、电动滑板车等;电动高尔夫球车等,而无特别限制。
有益效果
如上所述,当将本发明的正极活性材料引入到锂二次电池中时,可有利地提高倍率性能和高温稳定性而不会使电池性能劣化。
附图说明
根据结合附图进行的下列详细说明,将更清楚地理解本发明的上述和其他目的、特征和其他优势,其中:
图1是显示实施例1中制备的正极活性材料的SEM照片;
图2是显示比较例1中制备的正极活性材料的SEM照片;
图3说明了在0.1C下将使用比较例1中制备的正极活性材料形成的电池充电至4.3V之后,通过DSC测量加热位置与加热强度的图;
图4说明了在0.1C下将使用实施例1中制备的正极活性材料形成的电池充电至4.3V之后,通过DSC测量加热位置与加热强度的图;
图5说明了在0.1C下将使用实施例2中制备的正极活性材料形成的电池充电至4.3V之后,通过DSC测量加热位置与加热强度的图;
图6说明了使用比较例1中制备的正极活性材料形成的电池的SCC测量结果的图;
图7说明了使用实施例1中制备的正极活性材料形成的电池的SCC测量结果的图;且
图8说明了使用实施例2中制备的正极活性材料形成的电池的SCC测量结果的图。
具体实施方式
在下文中,参考下列实施例对本发明的例示性实施方式进行更详细的说明。然而,本领域的技术人员应理解,提出这些实施方式仅出于例示性目的,而不限制本发明的范围。
实施例1
在将相对重量比为100∶2∶2的活性材料∶碳∶聚乙烯放入干燥涂覆装置中之后,在2.5kW和3000rpm下将所述混合物处理5分钟。所述活性材料是LiNi0.53Mn0.27Co0.20O2。
实施例2
除了LiNi0.53Mn0.27Co0.20O2∶碳∶聚乙烯的相对重量比为100∶1∶1之外,重复与实施例1中相同的程序以对活性材料进行处理。
实施例3
除了LiNi0.5Mn0.3Co0.2O2∶碳∶聚乙烯的相对重量比为100∶2∶2之外,重复与实施例1中相同的程序以对活性材料进行处理。
比较例1
在不进行附加处理的条件下制备实施例1中使用的活性材料。
实验例1
关于实施例1和比较例1中得到的各种活性材料,通过SEM对活性材料的表面进行观察。将实施例1和比较例1的材料的观察结果分别示于图1和2中。
实验例2
通过以95∶2.5∶2.5的相对重量比将活性材料、导电材料和粘合剂共混,从而将实施例1~3和比较例1中得到的各种活性材料形成为浆体,随后将所述浆体涂布到Al箔上而形成电极。在对形成的电极进行冲孔以达到25%的孔隙率之后,使用冲孔的电极制造纽扣单电池。负极为Li且电解质为溶于碳酸酯溶剂中的1M LiPF6。在0.1C和3~4.25V下对制得的单电池进行充放电处理,在对容量和单电池效率进行监测之后,将实施例1和2与比较例1的材料所获得的结果示于表1中。
表1
首次充电(mAh/g) | 首次放电(mAh/g) | 首次效率(%) | |
比较例1 | 184.3 | 162.1 | 87.9 |
实施例1 | 184.9 | 162.5 | 87.9 |
实施例2 | 184.7 | 162.7 | 88.1 |
如表1中所示,发现所有的活性材料都显示有利的电化学性能且实施例3中得到的活性材料显示基本相同的结果。
实验例3
在0.1C下将实验例2的使用各种活性材料制造的单电池充电至4.3V之后,使用差示扫描量热仪(DSC)对加热位置和加热强度进行测量。将比较例1、实施例1和2的结果分别示于图3、4和5中。
与比较例1相比可发现,实施例1和2中获得的两种活性材料都具有急剧下降的加热强度。还观察到,加热强度最强的主峰的加热位置向更高温度迁移。另外观察到,当活性材料中碳和聚乙烯的含量增大时,加热强度进一步下降且同时主峰的位置向更高温度迁移。实施例3也显示了与实施例1基本相同的结果。因此我们确认,优选提高了活性材料的安全性。
实验例4
对于实验例2的使用各种活性材料制造的单电池,测量了短路电流(SCC)。图6、7和8分别显示了比较例1、实施例1和2的结果。
与比较例1相比可发现,实施例1和2中获得的两种活性材料都显示下降的电流峰值。另外观察到,当在活性材料中碳和聚乙烯的含量增大时,电流峰值的大小进一步下降。同样地,实施例3显示了与实施例1基本相同的结果。因此我们确认,优选提高了活性材料的安全性。
尽管出于例示性目的而公开了本发明的优选实施方式,但是本领域的技术人员应理解,在不背离所附权利要求书中公开的本发明的范围和主旨的情况下,在上述详细说明的基础上可以具有各种应用和变化。
Claims (7)
1.一种锂二次电池用正极,被构造成其中包含正极活性材料、导电材料和粘合剂的浆料被涂布至正极集电体的结构,其中所述正极活性材料是通过干燥涂覆装置而制得,且其中所述正极活性材料包含:
锂过渡金属氧化物,其中在所述锂过渡金属氧化物的表面涂覆有碳粒子和聚合物树脂,所述聚合物树脂因锂二次电池用电解质和有机溶剂而被惰性化且所述聚合物树脂具有至少80℃的熔点,
其中所述碳粒子具有0.01~1μm的平均粒径,
其中所述碳粒子和所述聚合物树脂各自为涂布至所述锂过渡金属氧化物表面的独立相,
其中所述锂过渡金属氧化物是LiNi0.53Mn0.27Co0.20O2或LiNi0.5Mn0.3Co0.2O2,
其中所述碳粒子是碳,
其中所述聚合物树脂是聚乙烯,且
其中所述锂过渡金属氧化物:碳粒子:聚合物树脂的混合比以重量比计为100:1:1或100:2:2。
2.如权利要求1所述的正极,其中所述聚合物树脂具有80~200℃的熔点。
3.如权利要求1所述的正极,其中所述碳粒子和所述聚合物树脂以所述碳粒子被捕集入所述聚合物树脂内部的复合形式涂布至所述锂过渡金属氧化物的表面。
4.如权利要求1所述的正极,其中所述碳粒子和所述聚合物树脂通过物理结合与所述锂过渡金属氧化物的表面结合在一起。
5.如权利要求1所述的正极,其中所述锂过渡金属氧化物总表面的20%~80%涂覆有所述碳粒子和所述聚合物树脂。
6.一种锂二次电池,其包含权利要求1~5中任一项所述的正极。
7.如权利要求6所述的锂二次电池,其中所述锂二次电池用作电动工具或电动车辆用的电源。
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