CN104769744A - 热稳定性优异的隔膜以及包含其的二次电池 - Google Patents
热稳定性优异的隔膜以及包含其的二次电池 Download PDFInfo
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- CN104769744A CN104769744A CN201480002843.3A CN201480002843A CN104769744A CN 104769744 A CN104769744 A CN 104769744A CN 201480002843 A CN201480002843 A CN 201480002843A CN 104769744 A CN104769744 A CN 104769744A
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- barrier film
- microcapsules
- heat stabilizer
- compound
- slurry
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Landscapes
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Abstract
本发明涉及一种隔膜,其为将包含由核心-壳层-间隔层组成并负载着热稳定剂的微胶囊施加于膜而形成,所述隔膜可在使用其的电池过热时释放所述热稳定剂,从而实现所述电池的热稳定性效果。
Description
技术领域
本申请要求于2013年9月17日在韩国提交的韩国专利申请No.10-2013-0112013以及于2014年9月17日在韩国提交的韩国专利申请No.10-2014-0123674的优先权,该申请的说明书及附图所公开的内容以引用的形式纳入本文。
本发明涉及热稳定性优异的隔膜以及包含所述隔膜的二次电池。
背景技术
随着移动设备的发展和使用的增加,二次电池作为主要能源的需求急剧增加。在所述二次电池中,特别是锂二次电池已经是可商购的,并且因其具有高能量密度和高电压而被广泛使用。
许多公司已生产这种电池,但其安全特性互相不同。评估和确保电池的安全性是非常重要的。对于安全性的最重要的考虑因素是电池在操作失误或故障时不应对使用者造成伤害。为此,安全规格严格地限制电池内发生起火和排烟。其中,最急待解决的问题是过度充电。
所有电池在被过度充电时都是危险的,锂离子二次电池也不例外。特别是,电池的“高温过度充电”是最危险的。通常,当所述锂离子二次电池被过度充电至4.2V或更高时,电解质溶液开始分解,并且所述锂离子二次电池达到闪点(flash point)的高温时极可能起火燃烧。
为了克服该问题,已提出各种尝试,但是仍然需要更有效的解决方案。
发明的内容
技术问题
本发明旨在解决上述问题,因此,本发明的一方面提供了包含只能在高于某一温度和/或某一压力的条件下释放热稳定剂的微胶囊的隔膜、制备所述隔膜的方法以及包含所述隔膜的二次电池。
因此,本发明的隔膜不具有这样的问题——负载着热稳定剂的微胶囊在电极的层压过程中过早地破裂,从而不能达到在二次电池过热时的所需效果。
另外,本发明的另一方面提供了一种隔膜,其配置有负载着热稳定剂的微胶囊以在二次电池过热时有效地发挥作用,从而所述二次电池的热稳定性得到改善;制备所述隔膜的方法;以及包含所述隔膜的二次电池。
技术方案
为了解决上述技术问题,依据本发明的一个方面,提供了包含如下的隔膜:多孔基底;以及包括涂布在所述多孔基底的至少一个表面上的含微胶囊的层,其中所述微胶囊由具有热稳定剂的核心部、围绕所述核心的壳层、以及围绕所述壳层的间隔层组成。
所述间隔层可通过浸渍在电解质溶液中而软化,并在高于200℃的温度下或在高于50kg/cm2的压力下破裂。
所述壳层可在70-100℃的温度下或在3-10kg/cm2的压力下破裂。
所述隔膜还可在所述多孔基底和所述含微胶囊的层之间包含多孔涂层,所述多孔涂层包含有机颗粒或无机颗粒、和粘合剂聚合物的混合物。
所述含微胶囊的层还可包含有机颗粒或无机颗粒、和粘合剂聚合物的混合物。
所述热稳定剂可以是选自由磷酸化合物、酚类化合物、环胺化合物、氨基脲、胺化合物、硝基化合物、亚磷酸盐化合物、不饱和烃化合物、基于硫的化合物组成的组中的一种或多种。
所述热稳定剂可以是磷酸三苯酯。
所述壳可以是由选自由聚烯烃、聚乙烯醇(PVA)、聚氯乙烯(PVC)组成的组中的一种以上而制得。
所述间隔可以是由选自由聚偏二氟乙烯、聚偏二氟乙烯-共-六氟丙烯、聚偏二氟乙烯-共-三氯乙烯、聚甲基丙烯酸甲酯、聚丙烯酸丁酯、聚丙烯腈、聚乙烯吡咯烷酮、聚乙酸乙烯酯、聚乙烯-共-乙酸乙烯酯、聚环氧乙烷、聚丙烯酸、聚乙烯醇、聚芳酯、乙酸纤维素、乙酸丁酸纤维素、乙酸丙酸纤维素、氰乙基支链淀粉、氰乙基聚乙烯醇、氰乙基纤维素、氰乙基蔗糖、支链淀粉、羧甲基纤维素组成的组中的一种以上而制得。
依据本发明的另一方面,提供了制备隔膜的方法,其特征在于,所述方法包括:将上述微胶囊分散在有机溶剂中以形成分散液的步骤;以及将所述分散液施加于多孔基底上的步骤。
另外,本发明提供了制备隔膜的方法,其特征在于,所述方法包括:将上述微胶囊、无机颗粒或有机颗粒、和粘合剂聚合物分散在有机溶剂中以形成浆料的步骤;以及将所述浆料施加于多孔基底上的步骤。
另外,本发明提供了制备隔膜的方法,其特征在于,所述方法包括:将无机颗粒或有机颗粒、和粘合剂聚合物分散在有机溶剂中以形成浆料的步骤;将所述浆料施加于多孔基底上的步骤;以及在对所述浆料进行干燥之前或之后进一步施加通过在有机溶剂中分散上述微胶囊而获得的分散液。
依据本发明的又一方面,提供了一种二次电池,所述二次电池包括正极(cathode)、负极(anode)、设置在所述负极和所述正极之间的隔膜、及电解质溶液,其特征在于,所述隔膜为上述隔膜。
在本发明中,基于所述电解质溶液的总重量计,所述热稳定剂的含量可以为0.01-1重量%。
所述二次电池可以是锂二次电池。
发明效果
当使用本发明的隔膜制造二次电池时,施加于所述隔膜中的微胶囊即使在压层电极组件的过程以后,仍可保持完好而不会破裂。因此,负载着于所述微胶囊中的热稳定剂可在所述二次电池过热时释放以抑制所述二次电池的起火燃烧,由此将由于所述二次电池的起火燃烧或爆炸而造成的损害降低至最小。
另外,本发明的一实施方案的隔膜的特征在于,负载着热稳定剂的微胶囊被配置在所述二次电池过热时可最有效地达到热稳定效果之处。
附图说明
图1是示意性地示出了依据本发明的由核心-壳层-间隔层组成的微胶囊的图。
具体实施方式
下文中,将详细描述本发明。在描述前,应理解,本说明书和所附权利要求书中使用的术语不应被解释为受限于一般含义和字典含义,而应在允许发明人为了最佳解释可适当地定义术语的原则基础上,基于与本发明的技术方面相应的含义和概念进行解释。
本发明的隔膜包含负载着热稳定剂并具有由核心-壳层-间隔层组成的结构的微胶囊。
参照图1,就所述微胶囊而言,壳层2围绕所述核心1周围,间隔层3围绕所述壳层2,并且在所述核心1负载着热稳定剂。当使用所述微胶囊的二次电极过热时,这类微胶囊通过所述间隔层和/或所述壳层的破裂而释放所述热稳定剂。
本文使用的术语“破裂”不仅是所述间隔层和/或所述壳层遭到破坏的现象,还可认为是指可释放内部组分如热稳定剂的任意现象,并且这种任意现象的非限制性实例可包括溶胀、熔融、断裂和开裂,但不限于此。
本文使用的术语“间隔”层为构成微胶囊的最外层并围绕所述壳层的层。
所述间隔层是用于保护所述壳层以使所述壳层在电极组件的层压(lamination)过程中不会破裂的组件。其结果,其可防止热稳定剂在所述电池过热之前被过早释放。如果所述热稳定剂被意外地过早地释放,或者如果所述电池被有意设计以使得在所述电池过热前释放所述热稳定剂,则这是不利的,因为过早释放的热稳定剂对所述电池的性能产生不利影响。
所述间隔层可以包含如下材料而形成:该材料应承受高于200℃的温度和高于50kg/cm2的压力,并在干燥状态下具有刚性,但浸渍于电解质溶液之后这种刚性消失或降低。或者,所述间隔层可以包含如下材料而形成:该材料应承受高于250℃的温度和高于70kg/cm2的压力,并在干燥状态下具有刚性,但浸渍于电解质溶液之后这种刚性消失或降低。
如果不存在所述间隔层、或所述间隔层在低于上述数值范围的温度和/或压力下破裂,则所述间隔层在电极组件的层压过程中破裂,从而所述热稳定剂在早于所需时间点时过早释放。
另外,如果所述间隔层由即使在用电解质溶液浸渍后仍保持刚性的材料形成,则这是不利的,因为在电池的热损坏(thermal abuse)状态下,直至所述微胶囊发挥效果会花费太长时间。因此,所述间隔层应该通过浸渍电解质溶液来软化以使刚性消失或降低。
所述间隔层可由不溶于电解质、在电池内部环境中具有惰性并且能够在上述条件下熔融或破裂的多种聚合物制成。这类聚合物的非限制性实例可选自由聚偏二氟乙烯、聚偏二氟乙烯-共-六氟丙烯、聚偏二氟乙烯-共-三氯乙烯、聚甲基丙烯酸甲酯、聚丙烯酸丁酯、聚丙烯腈、聚乙烯吡咯烷酮、聚乙酸乙烯酯、聚乙烯-共-乙酸乙烯酯、聚环氧乙烷、聚丙烯酸、聚乙烯醇、聚芳酯、乙酸纤维素、乙酸丁酸纤维素、乙酸丙酸纤维素、氰乙基支链淀粉、氰乙基聚乙烯醇、氰乙基纤维素、氰乙基蔗糖、支链淀粉、羧甲基纤维素组成的组中的至少一种,但不限于此。
在本发明的一个实施方案中,所述间隔层可具有20-100nm的厚度。如果所述间隔层的厚度低于所述下限值,则在层压过程中的温度和压力下无法保持所述核心-壳层-间隔层的结构。如果所述间隔层的厚度高于所述上限值,则所述间隔区的软化可能受阻,尽管其被所述电解质溶液浸渍。依据本发明,所述间隔层的厚度在本发明中是重要的,因为所述热稳定剂应在电池热损坏时被释放。
本文使用的术语“壳”层是指存在于所述间隔层和所述核心之间并围绕所述核心的组件。
所述壳层在电极组件的层压过程中可通过所述间隔层而保持完好。当所述间隔层通过电解质溶液的浸渍而被软化,并且所述电池因为热损坏而发生体积膨胀和内压增高时,所述壳层破裂以释放负载于所述微胶囊中的热稳定剂。对于该步骤,所述壳层应在70-100℃的温度下熔融或分解,或应在3-10kg/cm2的压力下破裂。如果所述壳层被设计成在低于上述数值范围的温度或压力下破裂,则所述热稳定剂会不必要地过早释放,对电池性能造成不利影响;如果所述壳层被设计成在高于上述数值范围的温度或压力下破裂,则即使在电池过热时也不能释放所述热稳定剂,从而不能达到所需效果。
所述壳层可由不溶于电解质、在电池内部环境中具有惰性并且能够在上述条件下熔融或破裂的多种聚合物制成。这类聚合物的非限制性实例可包括选自由聚烯烃如聚乙烯、聚丙烯;聚乙烯醇(PVA);聚氯乙烯(PVC)组成的组中的一种或多种。
在本发明的一个实施方案中,所述壳层可具有20-100nm的厚度。如果所述壳层的厚度太厚或太薄,则所述壳层无法在所需温度和压力下破裂。
在最终制备的电池中,在所述电池由于热损坏而发生体积膨胀,并且所述电池的温度或压力升高至高于上述温度或压力的数值范围,则所述壳层发生破裂。
可通过原料本身的性质或分子尺寸(在某些情况下,通过制备方法)来控制所述壳层和/或所述间隔层破裂时的特定条件。
用作核心材料的所述热稳定剂是指,能够捕获当电池在其充电或放电过程中暴露于高温下时所形成的不稳定自由基的组分,并且优选地,所述热稳定剂不会释放到电解液中。由此,可防止多孔涂层、隔膜或电池中使用的粘合剂聚合物或聚合物组分因氧化或转化为聚烯(造成分解)而形成的自由基所造成的劣化,以及由此所致的电池性能的劣化。
所述热稳定剂能够以通过物理结合而凝聚形成的聚集体的形式包含在多孔涂层中。
在本发明的一个实施方案中,所述热稳定剂的聚集体可以是具有相对小直径的一次颗粒形态的热稳定剂通过物理结合而获得的二次颗粒。这类聚集体可在加热和/或压缩过程中被粒化成一次颗粒,并广泛分散在所述多孔涂层中。
在本发明的另一实施方案中,可通过与所述多孔涂层中使用的粘合剂聚合物组分相同或不同的特定粘合剂聚合物来粘合具有相对小直径的热稳定剂,获得所述聚集体。
所述热稳定剂的非限制性实例可以是选自由磷酸化合物、酚类化合物、环胺化合物、氨基脲、胺化合物、硝基化合物、亚磷酸盐化合物、不饱和烃化合物、基于硫的化合物组成的组中的一种或多种。
优选地,所述磷酸化合物是磷酸三苯酯。所述磷酸三苯酯可有效用于抑制电池起火,但其过量添加时可对电池性能产生不利影响。因此,特别优选的是,所述磷酸三苯酯以微胶囊的形式用于本发明的隔膜中。
所述酚类热稳定剂的优选实例可包括:2,2-二(4'-羟基苯基)丙烷、氢醌、甲氧基苯酚、叔-丁基羟基-苯甲醚、正十八烷基-3-(4-羟基-3,5-二-叔-丁基苯基)丙酸酯、季戊四醇-四-[3-(3,5-二叔丁基-4-羟苯基)丙酸酯]、1,2-丙二醇双-[3-(3,5-二-叔-丁基-4-羟苯基)丙酸酯]、硬脂酰氨基N,N-双-[亚乙基3-(3,5-二-叔-丁基-4-羟基苯基)丙酸酯]、2,5-二叔-丁基氢醌、4,4'-亚丁基双(3-甲基-6-叔-丁基苯酚)、3,5-二-叔-丁基-4-羟基甲苯、2,2'-亚甲基-双(4-乙基-6-叔-丁基苯酚)、三甘醇-双-[3-(3-叔-丁基-5-甲基-4-羟苯基)丙酸酯]、新戊四醇-四[3-(3,5-二叔丁基-4-羟基-苯基)丙酸酯],2,6-二-叔-丁基-4-甲基苯酚、叔-丁基邻苯二酚、4,4-硫代双(6-叔-丁基-间甲酚)、生育酚、去甲二氢愈创木酸,但不限于此。
所述环胺类热稳定剂的实例可包括:苯基萘基胺、N,N'-二苯基-对-苯二胺和4,4'-双(二甲基苄基)二苯胺,基于所述氨基脲的热稳定剂的实例可包括:氢氟化物、盐酸化物、硝酸化物、酸式硫酸化物、硫酸化物、氯化物、甲酸化物、酸式草酸化物、酸式马来酸化物和马来酸氨基脲;氨基脲衍生物,如1-乙酰基氨基脲、1-氯代乙酰基氨基脲、1-二氯乙酰基氨基脲、1-苄酰基氨基脲和缩氨基脲等。
所述胺类热稳定剂的实例可包括:碳酰肼、硫代氨基脲、硫代缩氨基脲衍生物、硫代碳酰肼和硫代碳酰肼衍生物等,所述硝基类热稳定剂的实例可包括:硝基苯甲醚、亚硝基二苯胺、硝基苯胺和N-亚硝基苯基羟胺铝盐等。
所述不饱和烃类热稳定剂的实例并不做特别限定,例如可包括:苯乙烯、1,3-己二烯和甲基苯乙烯等,所述基于硫的热稳定剂的实例可包括:二月桂基硫代二丙酸酯、二肉豆蔻基硫代丙酸酯、硫代二丙酸二硬脂酰酯、十二烷硫醇和1,3-二苯基-2-硫脲等。
所述亚磷酸酯类热稳定剂的实例可包括:亚磷酸三苯酯、亚磷酸二苯基异癸基酯、亚磷酸苯基二异癸基酯、4,4'-亚丁基-双(3-甲基-6-叔-丁基苯基-二-十三烷基)磷酸酯、环新戊四烷-二(十八烷基)亚磷酸酯、三(壬基苯基)亚磷酸酯和三(二壬基)亚磷酸酯、二-(十八烷基)-3,5-二-叔丁基-4-羟基苄基膦酸酯,和二-正十八烷基-1-(3,5-二叔-丁基-4-羟基-苯基)-乙烷膦酸酯等,但不限于此。
在本发明的一实施方案中,所述核心可具有10-800nm的直径。如果所述核心的直径大于该数值范围,则含有微胶囊的层的厚度因微胶囊的尺寸而增加,并且所述隔膜的电阻也增加;如果所述核心的直径小于该数值范围,则所述热稳定剂的负载量不足,使得难以获得所需效果。
以所述非水电解质溶液的总重量计,所述热稳定剂优选以0.01-1重量%的量存在。如果所述热稳定剂的含量太少,则难以获得所需效果。如果所述热稳定剂的含量过多,则也不是优选的,因为其吸收过多量的电解质溶液并溶胀,从而减弱所述电极和隔膜之间的粘着性,并且可能在电池中引起各种副反应。
所述微胶囊优选具有约1至50μm的直径。考虑到所述热稳定剂的均匀分布,所述微胶囊具有小的直径以使每单位重量具有大的表面积是有利的。但是,如果所述微胶囊颗粒具有小于上述下限值的直径,则难以制备这类微胶囊,并且当电池过热时,所述间隔层或所述壳层难以破裂。另外,如果所述微胶囊具有大于上述上限值的直径,则所述微胶囊可能太容易因为压缩而破裂。
根据本发明的一实施方案,可将所述微胶囊施加于所述隔膜中的多孔基底的至少一个表面上。
另外,根据本发明的另一实施方案,在多孔基底上形成有多孔涂层的情况下,所述微胶囊可掺入到所述多孔涂层。
此外,根据本发明的又一实施方案,所述微胶囊可位于所述多孔涂层的表面上。
当所述热稳定剂被配置于临近发热的位置时,所述热稳定剂的释放可在电池发生热损坏时快速启动。因此,所述含热稳定剂的微胶囊优选配置于电极附近。
在由无机颗粒和粘合剂聚合物的混合物所形成的多孔涂层中,所述无机颗粒不受特别限制,只要它们是电化学稳定的。
也就是说,可用于本发明的无机颗粒只要在所应用的电化学装置的操作电压范围(例如,基于Li/Li+为0至5V)中不会发生氧化-还原反应,则不受特别限制。特别是,使用具有高介电常数的无机颗粒时,可增加电解质盐(如锂盐)在液体电解质中的解离速率,由此提高了所述电解质溶液的离子电导率。
为此,优选所述无机颗粒包含介电常数为5以上、优选10以上的介电常数无机颗粒。介电常数为5以上的无机颗粒的非限定实例包括BaTiO3、Pb(Zr,Ti)O3(PZT)、Pb1-xLaxZr1-yTiyO3(PLZT,0<x<1,0<y<1)、Pb(Mg1/3Nb2/3)O3-PbTiO3(PMN-PT)、氧化铪(HfO2)、SrTiO3、SnO2、CeO2、MgO、NiO、CaO、ZnO、ZrO2、SiO2、Y2O3、Al2O3、SiC和TiO2的无机颗粒,它们可单独使用或以其中的两种或多种的混合物的形式使用。
此外,作为所述无机颗粒可以使用具有传递锂离子的能力的无机颗粒,即,含有锂离子但并不存储锂的、具有使锂原子移动的功能的无机颗粒。所述具有传递锂离子的能力的无机颗粒的非限制性实例包括:磷酸锂(Li3PO4)、锂钛磷酸盐(LixTiy(PO4)3,0<x<2,0<y<3)、锂铝钛磷酸盐(LixAlyTiz(PO4)3,0<x<2,0<y<1,0<z<3)、(LiAlTiP)xOy类玻璃(0<x<4,0<y<13)如14Li2O-9Al2O3-38TiO2-39P2O5、锂镧钛酸盐(LixLayTiO3,0<x<2,0<y<3)、锂锗硫代磷酸盐(LixGeyPzSw,0<x<4,0<y<1,0<z<1,0<w<5)如Li3.25Ge0.25P0.75S4、氮化锂(LixNy,0<x<4,0<y<2)如Li3N、SiS2类玻璃(LixSiySz,0<x<3,0<y<2,0<z<4)如Li3PO4-Li2S-SiS2、P2S5类玻璃(LixPySz,0<x<3,0<y<3,0<z<7)如LiI-Li2S-P2S5,和它们的混合物。
另外,无机颗粒的粒径没有特别的限制,但优选平均粒径在0.001至10μm的范围内,以形成具有均匀厚度的涂层并获得合适的孔隙率。如果所述粒径小于0.001μm,则分散性可能会降低。如果所述粒径大于10μm,则涂层厚度可能会增加。
此外,所述无机颗粒和粘合剂聚合物的重量比优选在50:50-99:1的范围内,更加优选为70:30-95:5。如果所述无机颗粒和粘合剂聚合物的重量比小于50:50,则所述粘合剂聚合物的含量变大,使得所形成的涂层的孔径和孔隙率降低。如果所述无机颗粒的量超过99重量份,则所述粘合剂聚合物的量变少,使得所形成的涂层的抗剥离性能减弱。
所述微胶囊的制造方法只要是各种制造负载着热稳定剂的胶囊的方法,则没有任何特别限制。例如,通过乳化将相变材料分散在水溶液中,并且在所述相变材料的油相的表面上进行聚合以制得壳体。所述聚合可通过界面聚合、原位聚合或凝聚的方式进行。然后,能够在所述壳的表面上进行聚合以形成分隔层,其中所述聚合是根据本领域中常规已知的聚合方法进行,而没有任何特别限制。
在将负载着热稳定剂的微胶囊分散于分散液中,并施加于多孔基底的至少一个表面上,或在所述多孔基底上形成包含无机颗粒或有机颗粒的多孔涂层的情况下,所述微胶囊以包含于所述多孔涂层的浆料的状态施加于所述多孔基底,或者以分散液的形式施加于所述多孔涂层的表面上。
所述隔膜的多孔基底可以是用于电化学装置的平面多孔聚合物基底中的任意一种,例如,可使用具有高离子渗透性、良好的机械强度、0.01至10μm的孔径和5-300μm的厚度的绝缘薄膜。例如,由聚烯烃类的聚合物如乙烯均聚物、丙烯均聚物、乙烯/丁烯共聚物、乙烯/己烯共聚物、以及乙烯/甲基丙烯酸酯共聚物制成的多孔聚合物膜可单独使用或以层压的形式使用。另外,可使用传统的多孔非织造物,如由具有高熔点的玻璃纤维或聚对苯二甲酸乙二酯纤维制成的非织造物,但不限于此。
本发明的一实施方案提供了施加有所述微胶囊的隔膜的制造方法。
所述热稳定剂负载于所述微胶囊中并且施加于所述隔膜。
为此,将所述负载着热稳定剂的微胶囊分散于有机溶剂(如N-甲基-2-吡咯烷酮(NMP)、N,N-二甲基甲酰胺、四氢呋喃、二甲基乙酰胺、二甲基亚砜、六甲基磺酰胺、四甲基脲、丙酮、甲乙酮及它们的混合物)中,以获得分散液,并且将所制作的分散液施加于多孔基底。由于所述微胶囊的分隔层具有粘着性,则可将所述微胶囊溶于有机溶剂的分散液施加于所述多孔基底的至少一个表面上或多孔涂层上,而不添加额外的粘合剂聚合物。如果需要,可额外使用粘合剂聚合物。
若所述隔膜为包含无机颗粒或有机颗粒和粘合剂聚合物的多孔涂层形成于多孔基底的至少一个表面上的隔膜时,可将负载着热稳定剂的所述微胶囊掺入到用于所述多孔涂层的浆料中,并将所述浆料施加到所述多孔基底的至少一个表面上,或者将用于所述多孔涂层的浆料施加到多孔基底的至少一个表面之后立即、或在所述浆料干燥后,可将包含所述微胶囊的分散液施加于其上。
其中分散有无机颗粒并且粘合剂聚合物溶于溶剂中的用于多孔涂层的浆料可通过将所述粘合剂聚合物溶解于溶剂中,接着将所述无机颗粒添加并分散至其中而制得。可在添加所述无机颗粒之前,将它们粉碎成适当的尺寸,但优选的是,可在将所述无机颗粒添加到粘合剂聚合物的溶液之后,通过球磨的方式将其粉碎并分散。
涂布所述分散液或所述浆料的方法不受特别限制,可使用本领域中常规已知的多种涂布方法,例如浸涂、模涂、辊涂、刮刀式涂布(commacoating)或它们的组合。
随后,将所述分散液或浆料干燥以获得隔膜。
本发明的一方面提供了包含其中施加有微胶囊的隔膜的二次电极。
将所述隔膜设置在正极和负极之间,并根据所需的电池类型对包括正极、隔膜和负极的电极组件进行折叠、绕卷或层压,接着,将其置入电池盒中,注入电解质溶液,从而制作二次电池。
例如所述负极和正极的电极可通过如下制备:将电极活性材料、粘合剂聚合物、和任选的导电材料和填料混合以获得电极浆料,并将所述浆料涂布于集电器。例如,可将所述浆料涂布到集电器如金属箔上,然后进行干燥、压制,从而获得各个电极。
所述正极通过以下方式制备:将正极活性材料、导电材料和粘合剂聚合物的混合物施加到正极集电器上,随后进行干燥。如果需要,所述正极还可包含添加剂如填料。
所述正极集电器通常具有3至500μm的厚度。这类正极集电器不受特别限制,只要其具有高电导率而不会在电池中引起任何化学变化。所述正极集电器的实例包括不锈钢、铝、镍、钛、烧结碳;或其表面用碳、镍、钛或银处理的铝或不锈钢。此外,所述集电器可在其表面上具有精细凹凸部分以增加与所述正极活性材料的粘着性,并且可以是膜、薄板、箔片、网、多孔结构、泡沫、非织造物等各种形式。
所述正极活性材料的实例可包括:层状化合物如氧化锂钴(LiCoO2)和氧化锂镍(LiNiO2)、或被一种或多种过渡金属取代的化合物;锂锰氧化物如Li1+xMn2-xO4(0≤x≤0.33)、LiMnO3、LiMn2O3和LiMnO2的化合物;锂铜氧化物(Li2CuO2);钒氧化物如LiV3O8、LiFe3O4、V2O5和Cu2V2O7;LiNi1-xMxO2(M=Co、Mn、Al、Cu、Fe、Mg、B或Ga,并且0.01≤x≤0.3)的Ni-部位型锂镍氧化物;LiMn2-xMxO2(M=Co、Ni、Fe、Cr、Zn或Ta,并且0.01≤x≤0.1)或Li2Mn3MO8(M=Fe、Co、Ni、Cu或Zn)的锂锰复合氧化物;LiMn2O4,其中一部分Li被碱土金属离子取代;二硫化物;以及Fe2(MoO4)3,但并不限定与此。
以包含所述正极活性材料的混合物的总重量计,通常以1至50重量%的量添加所述导电材料。这类导电材料不受特别限制,只要其具有导电性而不在电池中引起任何化学变化。所述导电材料的实例可包括:石墨,例如天然石墨或人造石墨;炭黑,例如炭黑、乙炔黑、科琴黑、槽黑、炉黑、灯黑和热炭黑;导电纤维,例如碳纤维和金属纤维;金属粉末,例如氟化碳粉末、铝粉及镍粉;导电晶须,如氧化锌和钛酸钾;导电氧化物,例如氧化钛;以及聚亚苯基衍生物。在某些情况下,当所述正极活性材料在其上具有第二导电涂层,则所述导电材料的添加可省略。
所述粘合剂聚合物是帮助所述活性材料和导电材料粘合并帮助它们粘合至所述集电器的组分。以包含所述正极活性材料的混合物的总重量计,通常以1至50重量%的量添加所述粘合剂聚合物。所述粘合剂聚合物的实例可包括: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、聚乙烯吡咯烷酮、四氟乙烯、聚乙烯、聚丙烯、乙烯-丙烯-二烯烃三元共聚物(EPDM)、磺化EPDM、苯乙烯-丁二烯橡胶、氟化橡胶以及其他各种共聚物。
所述填料是用于抑制所述正极膨胀的任选成分。这类填料不受特别限制,只要其是纤维材料而不在电池中引起任何化学变化。所述填料的实例包括:烯烃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。
通过将负极材料施加于负极集电器上、随后进行干燥来制备所述负极。如果需要,所述负极还包含其他如上所述的组分。
所述负极集电器通常具有3至500μm的厚度。这类负极集电器不受特别限制,只要其具有高电导率而不会在电池中引起任何化学变化。所述负极集电器的实例包括:铜、不锈钢、铝、镍、钛、烧结碳;或其表面用碳、镍、钛或银处理的铝或不锈钢;以及铝-铬合金。类似于所述正极集电器,所述负极集电器可在其表面上具有精细凹凸部分以增加与所述负极活性材料的粘着性,并且可以是膜、薄板、箔片、网、多孔结构、泡沫、非织造物等各种形式。
所述负极活性材料的实例可包括:碳,如非石墨化碳和基于石墨的碳;金属复合氧化物如LixFe2O3(0≤x≤1)、LixWO2(0≤x≤1)和SnxMe1-xMe'yOz(Me:Mn、Fe、Pb、Ge;Me':Al、B、P、Si、元素周期表的第I族、第II族和第III族元素、卤原子;0<x≤1;1≤y≤3;并且1≤z≤8);金属锂;锂合金;硅基合金;锡基合金;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;以及Li-Co-Ni类材料。
另外,本发明提供了锂二次电池,其包含用含锂盐的非水电解质溶液浸渍的电极组件。
所述非水电解质溶液包含非水溶剂和锂盐。
所述非水溶剂的实例可包括:非质子有机溶剂如N-甲基-2-吡咯烷酮、碳酸丙烯酯、碳酸乙烯酯、碳酸丁烯酯、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franc、2-甲基四氢呋喃、二甲基亚砜、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-咪唑啉酮、碳酸丙烯酯衍生物、四氢呋喃衍生物、乙醚、丙酸甲酯和丙酸乙酯。
所述锂盐是溶解于上述非水溶剂中的材料,并且可包括,例如,LiCl、LiBr、LiI、LiClO4、LiBF4、LiB10Cl10、LiPF6、LiCF3SO3、LiCF3CO2、LiAsF6、LiSbF6、LiAlCl4、CH3SO3Li、CF3SO3Li、(CF3SO2)2NLi、氯硼烷锂、低级脂肪族羧酸锂、四苯基硼酸锂和酰亚胺。
另外,为了改善充电/放电特性和阻燃性,可将添加剂如吡啶、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、硝基苯衍生物、硫、醌亚胺染料、N-取代的噁唑烷酮、N,N-取代的咪唑烷、乙二醇二烷基醚、铵盐、吡咯、2-甲氧基乙醇和三氯化铝用于非水电解质溶液中。如果需要,为了赋予不燃性,所述非水电解液还可包含含卤素的溶剂如四氯化碳和三氟乙烯。此外,为了改善高温储存特性,所述非水电解质溶液可进一步包含二氧化碳气体。
Claims (15)
1.一种隔膜,其特征在于,
所述隔膜包括:
多孔基底;和
涂布在所述多孔基底的至少一个表面上的含微胶囊的层,其中所述微胶囊由具有热稳定剂的核心部、围绕所述核心的壳层、以及围绕所述壳层的间隔层组成。
2.根据权利要求1所述的隔膜,其特征在于,
所述间隔层通过浸渍在电解质溶液中而软化,并在高于200℃的温度下或在高于50kg/cm2的压力下破裂。
3.根据权利要求1所述的隔膜,其特征在于,
所述壳层在70-100℃的温度下或在3-10kg/cm2的压力下破裂。
4.根据权利要求1所述的隔膜,其特征在于,
所述隔膜还在所述多孔基底和所述含微胶囊的层之间包含多孔涂层,所述多孔涂层包含有机颗粒或无机颗粒、和粘合剂聚合物的混合物。
5.根据权利要求1所述的隔膜,其特征在于,
所述含微胶囊的层还包含有机颗粒或无机颗粒、和粘合剂聚合物的混合物。
6.根据权利要求1所述的隔膜,其特征在于,
所述热稳定剂是选自由磷酸化合物、酚类化合物、环胺化合物、氨基脲、胺化合物、硝基化合物、亚磷酸盐化合物、不饱和烃化合物、基于硫的化合物组成的组中的一种或多种。
7.根据权利要求1所述的隔膜,其特征在于,
所述热稳定剂是磷酸三苯酯。
8.根据权利要求1所述的隔膜,其特征在于,
所述壳由选自由聚烯烃、聚乙烯醇(PVA)、聚氯乙烯(PVC)组成的组中的一种以上而制得。
9.根据权利要求1所述的隔膜,其特征在于,
所述间隔选自由聚偏二氟乙烯、聚偏二氟乙烯-共-六氟丙烯、聚偏二氟乙烯-共-三氯乙烯、聚甲基丙烯酸甲酯、聚丙烯酸丁酯、聚丙烯腈、聚乙烯吡咯烷酮、聚乙酸乙烯酯、聚乙烯-共-乙酸乙烯酯、聚环氧乙烷、聚丙烯酸、聚乙烯醇、聚芳酯、乙酸纤维素、乙酸丁酸纤维素、乙酸丙酸纤维素、氰乙基支链淀粉、氰乙基聚乙烯醇、氰乙基纤维素、氰乙基蔗糖、支链淀粉、羧甲基纤维素组成的组中的一种以上而制得。
10.一种制备隔膜的方法,其特征在于,
所述方法包括:将权利要求1的微胶囊分散在有机溶剂中以形成分散液的步骤;以及将所述分散液施加于多孔基底上的步骤。
11.一种制备隔膜的方法,其特征在于,
所述方法包括:将权利要求1的微胶囊、无机颗粒或有机颗粒、和粘合剂聚合物分散在有机溶剂中以形成浆料的步骤;以及将所述浆料施加于多孔基底上的步骤。
12.一种制备隔膜的方法,其特征在于,
所述方法包括:将无机颗粒或有机颗粒、和粘合剂聚合物分散在有机溶剂中以形成浆料的步骤;将所述浆料施加于多孔基底上的步骤;以及在对所述浆料进行干燥之前或之后进一步施加通过在有机溶剂中分散权利要求1的微胶囊而获得的分散液。
13.一种二次电极,其特征在于,
所述二次电池包括正极、负极、设置在所述正极和所述负极之间的隔膜、及电解质溶液;
其中所述的隔膜为权利要求1-10任一项中所定义的隔膜。
14.根据权利要求13所述的二次电池,其特征在于,
基于所述电解质溶液的总重量计,所述热稳定剂的含量为0.01-1重量%。
15.根据权利要求14所述的二次电池,其特征在于,
所述电化学装置是锂二次电池。
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