CN104364943B - 高电压正极活性材料及其制备方法 - Google Patents
高电压正极活性材料及其制备方法 Download PDFInfo
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- CN104364943B CN104364943B CN201380030573.2A CN201380030573A CN104364943B CN 104364943 B CN104364943 B CN 104364943B CN 201380030573 A CN201380030573 A CN 201380030573A CN 104364943 B CN104364943 B CN 104364943B
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- 150000001450 anions Chemical class 0.000 claims description 6
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- 238000007796 conventional method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- DMSZORWOGDLWGN-UHFFFAOYSA-N ctk1a3526 Chemical class NP(N)(N)=O DMSZORWOGDLWGN-UHFFFAOYSA-N 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
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- 238000013461 design Methods 0.000 description 1
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- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
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- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
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- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 230000010220 ion permeability Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 239000002655 kraft paper Substances 0.000 description 1
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- 239000006233 lamp black Substances 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- YADSGOSSYOOKMP-UHFFFAOYSA-N lead dioxide Inorganic materials O=[Pb]=O YADSGOSSYOOKMP-UHFFFAOYSA-N 0.000 description 1
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 229910001547 lithium hexafluoroantimonate(V) Inorganic materials 0.000 description 1
- 229910001540 lithium hexafluoroarsenate(V) Inorganic materials 0.000 description 1
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 229910001537 lithium tetrachloroaluminate Inorganic materials 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- HSFDLPWPRRSVSM-UHFFFAOYSA-M lithium;2,2,2-trifluoroacetate Chemical compound [Li+].[O-]C(=O)C(F)(F)F HSFDLPWPRRSVSM-UHFFFAOYSA-M 0.000 description 1
- VROAXDSNYPAOBJ-UHFFFAOYSA-N lithium;oxido(oxo)nickel Chemical compound [Li+].[O-][Ni]=O VROAXDSNYPAOBJ-UHFFFAOYSA-N 0.000 description 1
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 description 1
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- PQIOSYKVBBWRRI-UHFFFAOYSA-N methylphosphonyl difluoride Chemical group CP(F)(F)=O PQIOSYKVBBWRRI-UHFFFAOYSA-N 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920001197 polyacetylene Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
- 239000001008 quinone-imine dye Substances 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
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- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 229920005608 sulfonated EPDM Polymers 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- BHZCMUVGYXEBMY-UHFFFAOYSA-N trilithium;azanide Chemical compound [Li+].[Li+].[Li+].[NH2-] BHZCMUVGYXEBMY-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/54—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [Mn2O4]-, e.g. Li(NixMn2-x)O4, Li(MyNixMn2-x-y)O4
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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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- H01M4/525—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
本文中公开了一种高电压正极活性材料及其制备方法。所述正极活性材料包含具有由式(1)表示的组成的尖晶石型化合物的粒子和存在于所述尖晶石型化合物的粒子的表面上的碳基材料:Li1+a MxMn2‑xO4‑zAz (1)其中‑0.1≤a≤0.1,0.3≤x≤0.8且0≤z≤0.1。
Description
技术领域
本发明涉及一种高电压正极活性材料及其制备方法,并且更特别地,涉及一种正极活性材料及其制备方法,其中所述正极活性材料包含具有由式(1)表示的组成的尖晶石型化合物的粒子和存在于所述尖晶石型化合物的粒子的表面上的碳基材料:
Li1+a MxMn2-xO4-zAz (1)
其中a,x和z如详细说明书中所限定。
背景技术
伴随信息技术(IT)的重大进步,各种移动信息通信装置已经被广泛使用并且二十一世纪标志着其中在任何地方和任何时间都可以获得高品质信息服务的泛在社会的开端。
锂二次电池在这种泛在社会的演变中起着重要作用。
与其他二次电池相比,锂二次电池具有高工作电压和能量密度并且可以长时间使用,由此满足对于种类不断增加的复杂装置的需要的复杂需求。
近来,已经在全世界进行了许多尝试以发展现有的锂二次电池技术,从而不仅将它们的应用延伸至环境友好的运输系统如电动车辆,而且延伸至电力储存。
用于中型或大型电源如电动车辆或电力储存系统(或者能量储存系统(ESS))的二次电池需要高功率、高能量密度和高能量效率。尽管具有诸如低价格和高功率的优点,但是LiMn2O4具有如下缺点:其能量密度低于锂钴氧化物的能量密度。
发明内容
技术问题
尽管开发了其中锰(Mn)被金属如镍(Ni)部分置换而提高具有4V范围内工作电压(约3.7V至约4.5V)的LiMn2O4的低能量密度的LiMn2O4化合物,但是本发明人发现,由于锰被金属如镍部分置换的LiMn2O4化合物具有4.6V以上的高工作电压,所以即使当电池处于正常工作范围中时电解质也分解并且其性能因所述化合物与电解质的副反应而下降。本发明人还发现,Mn离子遭受溶出。具有4V范围内工作电压的LiMn2O4不遭受该问题。
因此,进行了本发明以解决上述问题,并且本发明的目的是提供一种用于5V范围内的高电压的正极活性材料及其制备方法。
技术方案
根据本发明,可以通过如下实现上述和其他目的:提供一种正极活性材料,其包含具有由式(1)表示的组成的尖晶石型化合物的粒子和存在于所述尖晶石型化合物的粒子的表面上的碳基材料:
Li1+a MxMn2-xO4-zAz (1)
其中M为选自如下的至少一种:Ni、Ti、Co、Al、Cu、Fe、Mg、B、Cr、Zr、Zn和第II周期过渡金属,
A为一价阴离子或二价阴离子,以及
-0.1≤a≤0.1,0.3≤x≤0.8且0≤z≤0.1。
式(1)的尖晶石型化合物与LiMn2O4的不同之处在于,式(1)的尖晶石型化合物具有等于或高于4.6V且等于或小于4.9V的工作电压,而LiMn2O4具有4V范围内的工作电压(约3.7V至约4.3V)。因为式(1)的尖晶石型化合物具有等于或高于4.6V且等于或小于4.9V的工作电压,所以与LiMn2O4相比,式(1)的尖晶石型化合物显示高能量密度特性。
碳基材料可以覆盖尖晶石型化合物的粒子的表面的全部或一部分。具体地,碳基材料可以覆盖尖晶石型化合物的粒子的整个表面的等于或大于20%且等于或小于100%。在非限制性实施方式中,碳基材料可以覆盖尖晶石型化合物的粒子的整个表面的等于或大于50%且等于或小于80%。由此,由于覆盖有碳基材料的尖晶石型化合物的粒子部分的表面能的变化而抑制了锰的溶出。
碳基材料可以充当保护层以抑制与电解质的反应。保护层可以在高电压下充放电时阻挡电解质和式(1)的化合物之间的直接接触,从而抑制电解质的副反应。结果,根据本发明的正极活性材料可显示稳定的充放电循环特性,从而提高可逆的充放电容量。
另外,由于碳基材料具有高电导率,所以碳基材料降低了由式(1)表示的尖晶石型化合物的界面电阻,从而提高输出(或功率)特性。
在本发明的非限制性实施方式中,式(1)的化合物可包含由式(2)表示的化合物:
Li1+a NibMcMn2-(b+c)O4-zAz (2)
其中M为选自如下的至少一种:Ti、Co、Al、Cu、Fe、Mg、B、Cr、Zr、Zn和第II周期过渡金属,
A为一价阴离子或二价阴离子且为选自如下的至少一种:S,N和卤素如F、Cl、Br和I。
-0.1≤a≤0.1,0.3≤b≤0.6,0≤c≤0.2且0≤z≤0.1。
碳基材料可以物理地、化学地或物理化学地结合至尖晶石型化合物的粒子的表面。
碳基材料的平均粒径(D50)可以等于或大于2nm且等于或小于500nm。平均粒径(D50)在上述范围之外是不优选的,因为当平均粒径(D50)小于2nm时,不可能有效地抑制锰的溶出和与电解质的副反应,并且当平均粒径(D50)大于500nm时,碳基材料可能阻挡锂离子的扩散通道,从而降低高倍率特性。
正极活性材料可以通过如下制备:其中制备液体涂布溶液并与正极材料混合的液体法,使用球磨的高机械能量的机械化学方法,流化床涂布方法,喷雾干燥法,其中在水溶液中将涂布材料沉淀到活性材料的表面上的沉淀方法,利用气相涂布材料和正极材料之间的反应的方法,溅射法和使用静电的机械融合(mechanofusion method)法。
在一个具体实例中,正极活性材料可以根据包括如下的方法制备:将具有由上式(1)表示的组成的尖晶石型化合物和碳前体混合,并在惰性气氛或氧浓度为35体积%以下的缺氧气氛下对混合物进行热处理。
在一个具体实例中,可以使用干混法将尖晶石型化合物和碳前体混合。
在一个具体实例中,可以在400~800℃的温度下进行热处理,碳前体可以包含选自如下的至少一种:石油基沥青、焦油、酚醛树脂、呋喃树脂和碳水化合物,并且惰性气氛可以为氮气(N2)或氩气(Ar)气氛。
根据本发明的正极活性材料可以与上述正极活性材料之外的其他含锂过渡金属氧化物混合。
所述其他含锂过渡金属氧化物的实例包括但不限于:层状化合物如锂钴氧化物(LiCoO2)和锂镍氧化物(LiNiO2)自身或者被一种或多种过渡金属置换的所述层状化合物;锂锰氧化物如Li1+yMn2-yO4(其中0≤y≤0.33)、LiMnO3、LiMn2O3和LiMnO2;锂铜氧化物(Li2CuO2);钒氧化物如LiV3O8、LiV3O4、V2O5和Cu2V2O7;由LiNi1-yMyO2(M=Co、Mn、Al、Cu、Fe、Mg、B或Ga且0.01≤y≤0.3)表示的Ni位点型锂镍氧化物;由LiMn2-yMyO2(M=Co、Ni、Fe、Cr、Zn或Ta且0.01≤y≤0.1)或Li2Mn3MO8(M=Fe、Co、Ni、Cu或Zn)表示的锂锰复合氧化物;其中Li被碱土金属离子部分置换的LiMn2O4;二硫化合物;和Fe2(MoO4)3。
正极可以通过如下形成:将包含正极活性材料的正极混合物添加到溶剂如NMP中以制备浆料,并将浆料涂布至正极集电器,随后进行干燥和轧制。
除了正极活性材料之外,正极混合物还可以任选地包含导电材料、粘合剂、填料等。
正极集电器通常制造成3~500μm的厚度。可以使用任意正极集电器而没有特别限制,只要提供高导电性而不在电池中引起化学变化即可。正极集电器的实例包括铜,不锈钢,铝,镍,钛,烧结碳,用碳、镍、钛或银表面处理过的铜或不锈钢,或铝-镉合金。正极集电器可以在其表面上包含微小的不规则以提高对正极活性材料的粘合力。另外,可以以各种形式如膜、片、箔、网、多孔结构、泡沫或无纺布提供正极集电器。
基于包含正极活性材料的混合物的总重量,通常以0.01~30重量%的量添加导电材料。可以使用任何导电材料而没有特别限制,只要提供适当的导电性而不在电池中引起化学变化即可。导电材料的实例包括石墨如天然或人造石墨;炭黑如乙炔黑、科琴黑、槽法炭黑、炉黑、灯黑和热裂法炭黑;导电纤维如碳纤维和金属纤维;金属粉末如氟化碳粉末、铝粉和镍粉;导电晶须如氧化锌晶须和钛酸钾晶须;导电金属氧化物如二氧化钛;以及聚苯撑衍生物。
粘合剂是帮助活性材料对导电材料和集电器的粘合的成分。基于包含正极活性材料的化合物的总重量,通常以1~50重量%的量添加粘合剂。粘合剂的实例包括聚偏二氟乙烯、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EPDM、丁苯橡胶、氟橡胶和各种共聚物。
填料为任选地使用以抑制正极膨胀的成分。可以使用任何填料而没有特别限制,只要填料为在电池中不引起化学变化的纤维材料即可。填料的实例包括烯烃基聚合物如聚乙烯和聚丙烯;以及纤维材料如玻璃纤维和碳纤维。
可以用于本发明的分散液的代表性实例可包括异丙醇、N-甲基吡咯烷酮(NMP)和丙酮。
通过考虑所用材料的特性而选择使用常规方法或适当的新型方法实施作为电极材料的糊膏向金属材料的均匀涂布。例如,可以将电极糊膏分布到集电器上,然后使用刮刀在其上均匀分散。在适当时,也可以通过单一步骤进行电极糊膏的分布和分散。此外,可以通过选自压铸、逗号涂布(comma coating)、丝网印刷等的方法进行电极糊膏的涂布。或者,可以通过将糊膏在单独基材上成型,然后通过压制或层压将其附着至集电器实现电极糊膏的涂布。
优选在50~200℃下的真空烘箱中实施多达一天的涂布至金属板的糊膏的干燥。
例如,负极可以通过将负极活性材料涂布至负极集电器,随后干燥和压制而制备。任选地,负极可还包含诸如上述导电材料、粘合剂或填料的成分。
负极集电器通常制造成3~500μm的厚度。可以使用任何负极集电器而没有特别限制,只要提供适当的导电性而不在电池中引起化学变化即可。负极集电器的实例包括铜,不锈钢,铝,镍,钛,烧结碳,用碳、镍、钛或银表面处理过的铜或不锈钢,或者铝-镉合金。与正极集电器类似,负极集电器也可以在其表面上具有微小的不规则以提高对负极活性材料的粘合力。另外,可以以各种形式如膜、片、箔、网、多孔结构、泡沫和无纺布提供负极集电器。
负极活性材料的实例可包括碳如非石墨化碳和石墨化碳;金属复合氧化物如LixFe2O3(0≤x≤1),LixWO2(0≤x≤1)和SnxMe1-xMe’yOz(Me:Mn,Fe,Pb或Ge;Me’:Al,B,P,Si,周期表I、II和III族元素,或者卤素;0<x≤1;1≤y≤3;且1≤z≤8);锂金属;锂合金;硅基合金;锡基合金;金属氧化物如SnO、SnO2、PbO、PbO2、Pb2O3、Pb3O4、Sb2O3、Sb2O4、Sb2O5、GeO、GeO2、Bi2O3、Bi2O4和Bi2O5;导电聚合物如聚乙炔;和Li-Co-Ni基材料。
隔膜设置在正极和负极之间。作为隔膜,使用具有高离子渗透性和高机械强度的绝缘薄膜。隔膜通常具有0.01~10μm的孔径和5~300μm的厚度。例如,使用具有耐化学性和疏水性的烯烃基聚合物如聚丙烯、由聚乙烯或玻璃纤维制成的片或无纺布、或者牛皮纸作为隔膜。隔膜的可商购获得的产品的代表性实例可包括Celgard系列如CelgardR2400和2300(可得自Hoechest Celanese Corp.)、聚丙烯隔膜(可得自Ube Industries Ltd.或Pall RAI Corp.)和聚乙烯系列(可得自Tonen或Entek)。
在适当时,可以将凝胶聚合物电解质涂布在隔膜上以提高电池稳定性。凝胶聚合物的代表性实例可包括聚环氧乙烷、聚偏二氟乙烯和聚丙烯腈。
当使用固体电解质如聚合物电解质时,所述固体电解质也可以充当隔膜。
含锂盐的非水电解质包含非水电解质和锂。可以使用非水电解液、有机固体电解质、无机固体电解质等作为非水电解质。
电解液的实例包括非质子有机溶剂如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、碳酸甲乙酯、γ-丁内酯、1,2-二甲氧基乙烷、1,2-二乙氧基乙烷、四氢呋喃、2-甲基四氢呋喃、二甲基亚砜、1,3-二氧戊环、4-甲基-1,3-二烯、乙醚、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、丙酸甲酯和丙酸乙酯。
有机固体电解质的实例包括有机固体电解质如聚乙烯衍生物、聚环氧乙烷衍生物、聚环氧丙烷衍生物、磷酸酯聚合物、聚搅拌赖氨酸(polyagitation lysine)、聚酯硫化物、聚乙烯醇、聚偏二氟乙烯和含有离子离解基团的聚合物。
无机固体电解质的实例包括无机固体电解质如锂的氮化物、卤化物和硫酸盐如Li3N、LiI、Li5NI2、Li3N-LiI-LiOH、LiSiO4、LiSiO4-LiI-LiOH、Li2SiS3、Li4SiO4、Li4SiO4-LiI-LiOH和Li3PO4-Li2S-SiS2。
锂盐是易溶于非水电解质中的材料且可包括例如LiCl、LiBr、LiI、LiClO4、LiBF4、LiB10Cl10、LiPF6、LiCF3SO3、LiCF3CO2、LiAsF6、LiSbF6、LiAlCl4、CH3SO3Li、CF3SO3Li、LiSCN、LiC(CF3SO2)3、(CF3SO2)2NLi、氯硼烷锂、低级脂族羧酸锂、四苯基硼酸锂和酰亚胺。
另外,为了提高充放电特性和阻燃性,例如,可以向非水电解质中添加吡啶、亚磷酸三乙酯、三乙醇胺、环醚、乙二胺、正甘醇二甲醚、六磷酸三酰胺(hexaphosphorictriamide)、硝基苯衍生物、硫、醌亚胺染料、N-取代的唑烷酮、N,N-取代的咪唑烷、乙二醇二烷基醚、铵盐、吡咯、2-甲氧基乙醇、三氯化铝等。如果必要,为了赋予不燃性,非水电解质可还包含含卤素的溶剂如四氯化碳或三氟乙烯。此外,为了提高高温储存特性,非水电解质可另外包含二氧化碳气体且可还包含碳酸氟代亚乙酯(FEC)、丙烯磺酸内酯(PRS)、碳酸氟代亚丙酯(FPC)等。
根据本发明的二次电池优选用于充当小型装置用电源的电池用单电池(batterycell)并还优选用作包含多个电池用单电池的中型或大型电池模块的单元单电池(unitcell)。
本发明还提供包含所述电池模块的作为中型或大型装置用电源的电池组。中型或大型装置的优选实例包括但不限于电动车辆(EV),包括混合动力车辆(HEV)和插电式混合动力车辆(PHEV);和电力储存装置。
具体实施方式
现在将通过实施例对本发明进行进一步说明。然而,应注意,给出下列实施例仅为了例示本发明且本发明的范围不限于此。
<实施例1>
以100:5的重量比将LiNi0.5Mn1.5O4和石油基沥青引入到锥形搅拌器中,然后在400rpm下混合1小时。之后,在500℃的温度下在氮气气氛下将混合物热处理20小时,从而制备经碳基材料表面改性的LiNi0.5Mn1.5O4。
将经碳基材料表面改性的LiNi0.5Mn1.5O4、导电材料和粘合剂以97:2.5:2.5的比率称重,然后添加到NMP中,随后通过混合形成正极混合物。将正极混合物涂布至厚度为20μm的铝箔,随后通过轧制并干燥形成锂二次电池用正极。
然后,使用形成的锂二次电池用正极、作为对电极(即负极)的锂金属膜、作为隔膜的聚乙烯膜(Celgard,厚度:20μm)和液体电解质制造2016硬币式电池,所述液体电解质包含溶解在其中碳酸亚乙酯、碳酸二甲酯和碳酸二乙酯以1:2:1的比率混合的溶剂中的1MLiPF6。
<比较例1>
以与实施例1中相同的方式制造硬币式电池,不同之处在于,将未用碳基材料表面改性的LiNi0.5Mn1.5O4用作正极活性材料。
<实验例1>
初始充放电特性
在0.1C的电流下在3.5至4.9V的电压范围内对实施例1和比较例1中制造的硬币式电池充放电一次,并对充放电特性进行评价。将结果示于下表1中。
表1
<实验例2>
快速充电特性
在0.1C的电流下对实施例1和比较例1中制造的硬币式电池进行充放电,然后在5.0C的电流下进行充电,并对快速充电特性进行评价。将评价结果示于下表2中。
表2
<实验例3>
使用寿命特性
在1.0C的电流下将实施例1和比较例1中制造的硬币式电池充放电100次,并对使用寿命特性进行评价。将评价结果示于下表3中。
表3
<实验例4>
溶出锰量测定
在0.1C的电流下在3.5至4.9V的电压范围内对实施例1和比较例1中制造的硬币式电池充放电一次,并在0.1C的电流下充电至4.9V。然后将电池拆开。将从各拆开电池获得的正极浸入包含15mL电解质的容器中,并在80℃恒温槽中储存2周。然后,使用ICP(PerkinElmer,Model 7100)对溶出到电解质中的锰的含量进行分析。
表4
<实验例5>
高温储存特性评价
在0.1C的电流下在3.5至4.9V的电压范围内对实施例1和比较例1中制造的硬币式电池充放电一次,并在0.1C的电流下充电至4.9V。然后将电池在60℃恒温槽中储存一周,并对各电池的自放电量和容量恢复率进行测定。当以充满电状态将电池储存在高温下时,加速了正极活性材料表面上的电解质的分解,从而提高自放电。这造成正极活性材料的结构的破坏。设计该实验以观察该现象。
表5
【工业实用性】
根据本发明,上式1的尖晶石型化合物的粒子的表面的全部或一部分涂布有碳基材料。这抑制了锰的溶出和高压下的电解质副反应,从而使得能够提供改善的高电压锂二次电池。
Claims (9)
1.一种正极活性材料,包含:
具有由式(1)表示的组成的尖晶石型化合物的粒子;和
存在于所述尖晶石型化合物的粒子的表面上的碳基材料,
其中所述碳基材料的平均粒径D50等于或大于2nm且等于或小于500nm:
Li1+aMxMn2-xO4-zAz (1)
其中M为选自如下的至少一种:Ni,Ti,Co,Al,Cu,Fe,Mg,B,Cr,Zr,Zn和第II周期过渡金属,
A为一价阴离子或二价阴离子,以及
-0.1≤a≤0.1,0.3≤x≤0.8且0≤z≤0.1,
其中所述碳基材料覆盖式(1)的尖晶石型化合物的全部表面的等于或大于50%且等于或小于80%。
2.根据权利要求1的正极活性材料,其中所述尖晶石型化合物包含由式(2)表示的化合物:
Li1+aNibMcMn2-(b+c)O4-zAz (2)
其中M为选自如下的至少一种:Ti,Co,Al,Cu,Fe,Mg,B,Cr,Zr,Zn和第II周期过渡金属,
A为一价阴离子或二价阴离子,以及
-0.1≤a≤0.1,0.3≤b≤0.6,0≤c≤0.2且0≤z≤0.1。
3.根据权利要求1的正极活性材料,其中所述碳基材料物理地和/或化学地结合至式(1)的尖晶石型化合物的粒子的表面。
4.一种制备正极活性材料的方法,所述方法包括:
将具有由式(1)表示的组成的尖晶石型化合物和碳前体混合;并且
在惰性气氛或氧浓度为35体积%以下的缺氧气氛下在400~800℃的温度下对所得混合物进行热处理,
其中所述惰性气氛为氮气(N2)或氩气(Ar)气氛,
其中使用干混法将所述碳前体和所述尖晶石型化合物混合:
Li1+aMxMn2-xO4-zAz (1)
其中M为选自如下的至少一种:Ni,Ti,Co,Al,Cu,Fe,Mg,B,Cr,Zr,Zn和第II周期过渡金属,
A为一价阴离子或二价阴离子,以及
-0.1≤a≤0.1,0.3≤x≤0.8且0≤z≤0.1。
5.根据权利要求4的方法,其中所述尖晶石型化合物包含由式(2)表示的化合物:
Li1+aNibMcMn2-(b+c)O4-zAz (2)
其中M为选自如下的至少一种:Ti,Co,Al,Cu,Fe,Mg,B,Cr,Zr,Zn和第II周期过渡金属,
A为一价阴离子或二价阴离子,以及
-0.1≤a≤0.1,0.3≤b≤0.6,0≤c≤0.2且0≤z≤0.1。
6.根据权利要求4的方法,其中所述碳前体包含选自如下的至少一种:石油基沥青、焦油、酚醛树脂、呋喃树脂和碳水化合物。
7.一种锂二次电池,包含根据权利要求1的正极活性材料。
8.一种电池组,包含根据权利要求7的锂二次电池。
9.一种电动车辆,包含根据权利要求8的电池组。
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