CN104380519B - 包含电解质添加剂的二次电池 - Google Patents
包含电解质添加剂的二次电池 Download PDFInfo
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- CN104380519B CN104380519B CN201380031982.4A CN201380031982A CN104380519B CN 104380519 B CN104380519 B CN 104380519B CN 201380031982 A CN201380031982 A CN 201380031982A CN 104380519 B CN104380519 B CN 104380519B
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- electrolyte
- secondary cell
- battery
- phosphate
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Classifications
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- H01M4/044—Activating, forming or electrochemical attack of the supporting material
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Abstract
本发明公开了一种二次电池,其具有包含正极、负极和置于其间的隔膜的电极组件及电解质,其中负极包含作为负极活性材料的锂钛氧化物(LTO),且电解质包含作为添加剂的磷酸酯基化合物。
Description
技术领域
本发明涉及包含电极组件和电解质的二次电池,所述电极组件包含正极、负极和置于正极与负极之间的隔膜,其中所述负极包含作为负极活性材料的锂钛氧化物(LTO),并且所述电解质包含作为添加剂的磷酸酯基化合物。
背景技术
移动装置技术的发展和对此需求的增加已经引起了对作为能源的二次电池的需求急剧增加。在这些二次电池中,展示高能量密度、高运行电势、长循环寿命及低自放电率的锂二次电池可商购获得并被广泛使用。
此外,对环境问题关注的不断增加近来已经引起与电动车辆(EV)和混合电动车辆(HEV)相关的大量研究,所述电动车辆(EV)和混合电动车辆(HEV)作为是空气污染主要原因的使用矿物燃料的车辆如汽油车辆、柴油车辆的替代品。这种电动车辆通常使用镍-金属氢化物(Ni-MH)二次电池作为电源。然而,正在积极开展对于具有高能量密度、高放电电压和输出稳定性的锂二次电池的使用相关的大量研究,并且一些锂二次电池可商购获得。
锂二次电池可根据采用的电解质类型分为:本身包含液体电解质的锂离子电池,以凝胶形式包含液体电解质的锂离子聚合物电池,以及包含固态电解质的锂聚合物电池。特别地,因为锂离子聚合物或凝胶聚合物电池的各种优势,例如与液体电解质电池相比,因流体泄露的低可能性而具有的高安全性,以及能实现非常薄且轻质的电池,所以锂离子聚合物或凝胶聚合物电池的使用正在增加。
通过将包含正极和负极的电极组件浸渍于包含锂盐的液体电解质中制造锂离子电池,所述正极和负极之间置有多孔隔膜,所述正极和负极各自通过将活性材料施加到集电器上形成。
根据用于电解质浸渍的基体材料的类型,制造锂离子聚合物电池的方法被分为:非交联聚合物电池制造方法,和直接交联聚合物电池制造方法。具有高自由基聚合反应性的丙烯酸酯基材料和甲基丙烯酸酯基材料以及具有高导电性的醚基材料通常被用作聚合物基体材料。特别地,在直接交联聚合物电池的制造过程中,通过如下制造电池:将由电极片组成的卷型或堆叠型电极组件和多孔隔膜放入袋中,向袋中注入可热聚合的聚氧化乙烯基单体或低聚物交联剂和电解质成分,以及对注入的材料实施热固化。以这种方式制造电池的优势在于,可不改变地使用常规锂离子电池的电极片和隔膜。然而,直接交联聚合物电池的制造过程的问题在于,交联剂不完全固化并残留在电解质中,增加了粘度。这使得难以均匀浸渍,从而大大劣化电池性能。
碳基材料通常用作锂二次电池用负极活性材料。然而,碳基材料具有相对于锂为0V的低电势,并且因此还原电解质,从而产生气体。还使用具有相对高的电势的锂钛氧化物(LTO)作为锂二次电池用负极活性材料以解决这些问题。
然而,当将LTO用作负极活性材料时,LTO充当催化剂,在活化和充放电工艺期间产生大量的氢气,这导致二次电池安全性降低。
因此,迫切需要提供在维持电池整体性能的同时通过解决上述问题而保证电池安全性的技术。
发明内容
技术问题
因此,实施了本发明以解决上述问题及其它尚未解决的技术问题。
作为各种广泛深入研究和实验的结果,本发明人发现,当使用包含作为负极活性材料的锂钛氧化物(LTO)和作为电解质添加剂的磷酸酯基化合物的二次电池时,实现期望的效果。由此完成了本发明。
技术方案
根据本发明,上述和其它目的可通过提供包含具有正极、负极和置于其间的隔膜的电极组件以及电解质的二次电池实现,其中所述负极包含作为负极活性材料的锂钛氧化物(LTO),并且所述电解质包含作为添加剂的磷酸酯基化合物。
在一个具体的实施方案中,电解质可以是但不限于液体电解质、凝胶电解质和固体电解质中的任意一种。具体地,电解质可以为液体电解质或凝胶聚合物电解质。
当电解质为液体电解质时,通过电解质与负极活性材料的副反应可促进电解质的分解,从而如上所述产生气体。这种气体可导致二次电池的安全问题如膨胀或爆炸。因此,根据本发明的二次电池使用其中添加有磷酸酯基化合物的液体电解质以解决这些问题。
当电解质为凝胶聚合物电解质时,向凝胶聚合物电解质中添加作为交联剂而反应的磷酸酯基化合物。这在实现电极界面稳定性的同时提供优异的循环特性效果,从而大大抑制在高温存储期间通过气体产生而导致的膨胀。结果是,还实现了电池使用寿命和安全性大大改善的效果。
在此,据信,因为磷酸酯基化合物与自由基具有高反应性,其增加了聚合物反应的程度,从而提高了最终电解质的电化学稳定性。此外,用作负极活性材料的LTO充当催化剂以促进磷酸酯基化合物的交联聚合,从而最大化上述效果。
特别地,当电解质是凝胶聚合物电解质时,因为电解质与电极接触的区域面积减少,所以在重复充放电期间电解质与电极的副反应减少;因为电解质为凝胶聚合物形式,所以由于蒸汽压降低还抑制了膨胀。
在一个实施方案中,磷酸酯基化合物可包含选自式(1)的磷酸酯基丙烯酸酯、式(2)的焦磷酸酯基丙烯酸酯和磷酸酯基氨基甲酸酯丙烯酸酯中的至少一种:
其中R1和R2各自独立地为氢、甲基或F,且n为1~20的整数。
电解质还可以包含能与磷酸酯基化合物聚合的多官能化合物。
当能与磷酸酯基化合物聚合的多官能化合物被另外用作电解质添加剂时,多官能化合物和磷酸酯基化合物的电化学特性和机械特性可彼此互补,从而进一步提高电池的整体特性。
具体地,当使用磷酸酯基化合物和能与磷酸酯基化合物聚合的多官能化合物制备凝胶聚合物电解质时,实现具有更高弹性的物理性质。也就是,磷酸酯基化合物具有能与锂离子容易配合的结构,因此展现更高的结合力,所述磷酸酯基化合物和具有高弹性的多官能化合物通过交联在一起而聚合,由此磷酸酯基化合物和多官能化合物的电化学特性和机械特性彼此互补。
在一个实施方案中,多官能化合物可以包含选自(甲基)丙烯酸酯化合物、不饱和碳酸化合物和乙烯基化合物中的至少一种。
(甲基)丙烯酸酯化合物可包括每个分子具有至少两个丙烯酸酯基的(甲基)丙烯酸酯化合物,且(甲基)丙烯酸酯化合物可以为式3的单体或其低聚物:
其中R3、R4和R5各自独立地为氢、取代或未取代的C1-C4烷基,且m为1~20的整数。
此外,(甲基)丙烯酸酯化合物可包含但不限于选自以下材料中的至少一种:二乙二醇二丙烯酸酯(Di(EG)DA)、二乙二醇二甲基丙烯酸酯(Di(EG)DM)、乙二醇二甲基丙烯酸酯(EGDM)、二丙二醇二丙烯酸酯(Di(PG)DA)、二丙二醇二甲基丙烯酸酯(Di(PG)DM)、乙二醇二乙烯醚(EGDVE)、乙氧基化(6)三羟甲基丙烷三丙烯酸酯(ETMPTA)、二乙二醇二乙烯醚(Di(EG)DVE)、三乙二醇二甲基丙烯酸酯(Tri(EG)DM)、双季戊四醇五丙烯酸酯(DPentA)、三羟甲基丙烷三丙烯酸酯(TMPTA)、三羟甲基丙烷三甲基丙烯酸酯(TMPTM)、丙氧基化(3)三羟甲基丙烷三丙烯酸酯(PO(3)TMPTA)、丙氧基化(6)三羟甲基丙烷三丙烯酸酯(PO(6)TMPTA)、聚(乙二醇)二丙烯酸酯(PA1)和聚(乙二醇)二甲基丙烯酸酯。
多官能化合物可以与磷酸酯基化合物一起形成各种类型的共聚物,例如无规共聚物、嵌段共聚物和接枝共聚物。
基于电解质的总重量,电解质可包含0.1重量%~1重量%,更特别地为0.1重量%~0.5重量%的能与磷酸酯基化合物聚合的多官能化合物。
基于电解质的总重量,电解质可包含0.01重量%~30重量%,更特别地为0.01重量%~20重量%的磷酸酯基化合物。
当电解质是液体电解质时,如果磷酸酯基化合物的含量过低,则不能充分实现提高安全性的效果。相反地,如果磷酸酯基化合物的含量过高,则虽然提高了安全性,但因为锂盐相对更低,整体电池特性会降低。
当电解质为凝胶聚合物电解质时,如果磷酸酯基化合物的含量过低,则不易形成凝胶聚合物,使得当使用液体电解质时发生电池膨胀的现象可能更加严重,并且难以形成具有期望厚度的基体。相反地,如果磷酸酯基化合物的含量过高,则凝胶聚合物的密度增加,并且锂离子传导率(或电导率)相应地减少,引起锂的沉淀,结果是电池性能降低。此外,粘度增加,从而会难以将电解质均匀应用于相应部分。
当将多官能化合物添加到磷酸酯基化合物时同样如此。因此,基于电解质的总重量,电解质包含的磷酸酯基化合物和多官能化合物的总量可以为0.01~30%,更特别地为0.1~5%。
液体电解质可包含电解质(增塑剂)和锂盐。当电解质为凝胶聚合物电解质时,电解质还可包含聚合引发剂。
电解质还充当增塑剂。例如,电解质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(PC)、碳酸亚乙酯(EC)、碳酸亚丁酯(BC)、碳酸二甲酯(DMC)、碳酸二乙酯(DEC)、碳酸甲乙酯(EMC)、γ-丁内酯、1,2-二甲氧基乙烷、四氢呋喃、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、丙酸甲酯和丙酸乙酯。这些材料可以单独使用或作为两种以上的混合物使用。
锂盐是溶于非水电解质中并且分解成锂离子的材料。锂盐的实例包括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、四苯基硼酸锂和酰亚胺。这些材料可单独使用或作为两种以上的混合物使用。
基于包含在电解质中的固体成分的总重量,电解质包含的锂盐可以为0.01重量%~30重量%,更特别地为0.1重量%~20重量%。
聚合引发剂的实例可以包括偶氮类化合物如2,2-偶氮二(2-氰基丁烷)、2,2-偶氮二(甲基丁腈)、2,2’-偶氮异丁腈(AIBN)和偶氮二甲基-戊腈(AMVN),过氧类化合物如过氧化二苯甲酰、过氧化乙酰、过氧化二月桂酰、二叔丁基过氧化物、枯基过氧化氢和过氧化氢及氢过氧化物。特别地,AIBN、2,2’-偶氮二(2,4-二甲基戊腈)(V65)、二-(4-叔丁基环己基)-过氧二碳酸酯(DBC)等可以作为聚合引发剂。
聚合引发剂可在40℃~80℃的温度下分解以形成自由基,然后可以通过自由基聚合与单体反应以形成凝胶聚合物电解质。通常,自由基聚合通过连续反应实施,所述连续反应包括:涉及具有高反应活性或活性位点的瞬态分子的形成的引发反应,涉及通过向活性链末端添加单体而在链的末端再形成活性位点的增长反应,涉及活性位点向其他分子转移的链转移反应,以及涉及活性链中心破坏的终止反应。当然,也可以在没有聚合引发剂的情况下实施聚合反应。
此外,为了提高充放电特性和阻燃性,例如,可以向电解质中添加吡啶、亚磷酸三乙酯、三乙醇胺、环醚、乙二胺、正甘醇二甲醚、六磷酰三胺(hexaphosphoric triamide)、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。在适当情况下,为了赋予不燃性,非水电解质还可包含含卤素的溶剂如四氯化碳或三氟乙烯等。此外,为了提高高温储存特性,非水电解质还可包含二氧化碳气体。
根据本发明的二次电池可以为锂离子电池。锂离子电池可通过如下制造:在电池壳中安装电极组件,向电池壳中注入磷酸酯基化合物、电解质和锂盐的混合物,随后密封,并实施形成过程以活化电池,以及实施老化过程以稳定被活化的电池。
然而,当电解质为凝胶聚合物电解质时,在凝胶反应之后实施活化过程。当将磷酸酯基化合物用作电解质添加剂时,在省去凝胶反应的同时可以采用其中通过润湿和充放电引起膜形成的方法。在基本方法中,将电池充电到单体会发生电化学分解反应的水平,然后进行除气。
形成过程是通过重复充放电循环而活化电池的过程。老化过程是通过使电池静置一段时间,使在形成过程中活化的电池稳定的过程。
形成过程和老化过程的实施条件没有特别限制,并且在本领域已知的常规范围内是可调节的。
在一个具体实施方案中,将混合物注入电池壳中(初次注入),并且使得电池结构静置一段时间(例如10小时),从而实现混合物均匀浸渍到电池壳中。然后将电池充电活化。在用于活化的充电过程中,除去在负极用保护膜的形成期间产生的气体。其后,使得电池再次静置一段时间(例如12小时)并充电活化,从而完成电池制造。
根据本发明的二次电池可以是锂离子聚合物电池。具体地,锂离子聚合物电池可使用以下方法制造,所述方法包括:(a)在电池壳中安装电极组件,(b)向电池壳中注入磷酸酯基化合物、聚合引发剂、电解质和锂盐的混合物,随后密封,和(c)使磷酸酯基化合物聚合以形成凝胶聚合物电解质。
具体地,步骤(c)可包括:(c1)对电池实施热固化、通过电子束或伽马射线的照射而进行的光固化或在30~80℃下进行的稳定反应,以使磷酸酯基化合物聚合,和(c2)实施形成过程以活化电池,以及实施老化过程以稳定活化的电池。
具体地,交联反应可在惰性条件下实施。因为在惰性气氛下根本上阻止了自由基与充当自由基捕获剂的大气中的氧的反应,所以可将反应程度提高至基本上无未反应的单体存在的水平。这阻止了由残留在电池内的大量未反应单体导致的充放电性能的劣化。
惰性气氛条件没有特别限制。可以使用低反应性的已知气体。例如,可以将选自氮气、氩气、氦气和氙气中的至少一种用作惰性气体。
磷酸酯基化合物通过交联聚合反应结合以形成具有三维网状结构的交联聚合物,并且随后用电解质将该聚合物均匀浸渍。
交联聚合物电解质是电化学稳定的,因此能稳定存在于电池中,即使在重复充放电循环后也不损坏。结果是,可以提高电池安全性并且实现优异的机械性能如伸长和弯曲性能。此外,因为锂离子通过极性凝胶聚合物电解质连续迁移和转移,所以电池性能劣化可被最小化。
按照如上所述以相同的方式实施形成和老化过程。在形成过程期间,电池充电时从用作正极的锂金属氧化物释放出的锂离子迁移并嵌入用作负极的碳电极。此时,由高反应性锂与碳负极反应产生的化合物如Li2CO3、LiO和LiOH在负极表面上形成固态电解质界面(SEI)膜。在此情况下,未反应的交联剂可进行额外的反应。
在一个具体实施方案中,将混合物注入电池壳中(初次注入),使电池结构静置一段时间(例如3小时),由此实现混合物均匀浸渍到电池壳中。然后在上述指定的条件下实施热聚合。然后将电池充电活化。在充电活化过程中,除去在负极用保护膜形成期间产生的气体,并且将一定量的补充混合物第二次注入电池壳中。其后,使得电池再次静置一段时间(例如12小时),并充电活化,从而完成电池制造。
通常通过向包含正极和负极及置于其间的隔膜的电极组件中加入电解质而制造二次电池。
例如可通过将正极活性材料、导电材料和粘合剂的混合物涂布到集电器上,随后干燥及压制,从而制备正极。如果需要,可向混合物中添加填料。
正极集电器通常制造成3~500μm的厚度。可使用任何正极集电器而没有特别限制,只要提供高导电性且在电池中不引起化学变化即可。正极集电器的实例包括不锈钢,铝,镍,钛,烧结碳或用碳、镍、钛、银等进行表面处理的铝或不锈钢制成。正极集电器可以在其表面具有微小的不规则处以提高对正极活性材料的附着力。另外,可以以例如膜、片、箔、网、多孔结构、泡沫和无纺布的各种形式使用正极集电器。
正极活性材料的实例包括但不限于:层状化合物如独自或被一种以上过渡金属置换的锂钴氧化物(LiCoO2)和锂镍氧化物(LiNiO2);锂锰氧化物如Li1+xMn2-xO4(其中0≤x≤0.33)、LiMnO3、LiMn2O3和LiMnO2;锂铜氧化物(Li2CuO2);钒氧化物如LiV3O8、LiV3O4、V2O5和Cu2V2O7;由LiNi1-xMxO2(M=Co、Mn、Al、Cu、Fe、Mg、B或Ga,且0.01≤x≤0.3)表示的Ni位点型锂镍氧化物;由LiMn2-xMxO2(M=Co、Ni、Fe、Cr、Zn或Ta,且0.01≤x≤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取代的LiMn2O4;二硫化物化合物;和Fe2(MoO4)3。
基于包含正极活性材料的混合物的总重量,通常以0.01~50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在制造的电池中不引起化学变化即可。导电材料的实例包括石墨如天然或人造石墨;炭黑类材料如乙炔黑、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、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;以及聚亚苯基衍生物。
粘合剂是有助于活性材料对导电材料和集电器粘合的成分。基于包含正极活性材料的混合物的总重量,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、三元乙丙橡胶(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,只要该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。
例如,通过将负极活性材料涂布至负极集电器,随后干燥和压制,从而制备负极。如上所述,根据需要,负极还可包含其他成分。
负极集电器通常制造成3~500μm的厚度。可使用任何负极集电器而没有特别限制,只要提供合适的导电性而在制造的电池中不引起化学变化即可。负极集电器的实例包括铜,不锈钢,铝,镍,钛,烧结碳,用碳、镍、钛或银进行表面处理的铜或不锈钢,或铝-镉合金。与正极集电器类似,负极集电器可以在其表面上具有微小的不规则处以提高对负极活性材料的结合力。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。
如上所述,锂钛氧化物可以用作负极活性材料。
特别地,锂钛氧化物可以是Li4Ti5O12、LiTi2O4或其混合物。更特别地,锂钛氧化物可以是Li4Ti5O12。
负极活性材料的实例可包括碳如非石墨化碳或石墨化碳的混合物;金属复合氧化物如LixFe2O3(0≤x≤1),LixWO2(0≤x≤1)或SnxMe1-xMe’yOz(Me:Mn,Fe,Pb或Ge;Me’:Al,B,P,Si,周期表的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或Bi2O5;导电聚合物如聚乙炔和Li-Co-Ni基材料。
根据本发明的二次电池可以制造成各种形式。例如,电极组件可以制造成卷结构、堆叠结构、堆叠/折叠结构等。电池可被结构化以使得电极组件被安装在由圆柱体罐、长方体罐或包含金属层和树脂层的层压片制成的电池壳中。这种电池的结构在本领域内是广泛已知的,因此在此省略对其的详细描述。
二次电池可以为锂二次电池。
如下所述,二次电池不仅可以用作小型装置用电源,而且可以用作中型或大型装置用电源。
本发明还提供包含所述二次电池作为单元电池的电池模块和包含所述电池模块的电池组。
电池组还可用作需要高温稳定性、长循环寿命和高倍率特性的中型或大型装置用电源。
中型或大型装置的具体实例包括但不限于:由电动机驱动的电动工具、包括混合电动车辆(HEV)和插电式混合电动车辆(PHEV)的电动车辆(EV)、包括电动自行车(E-自行车)和电动踏板车(E-踏板车)的电动双轮车辆、电动高尔夫球车和电力储存系统。
附图说明
图1是显示根据实验例2在45℃的室内循环特性的对比图;以及
图2是显示根据实验例3在60℃的室内与高温存储寿命相关的气体产生程度的对比图。
具体实施方式
现在将通过实施例对本发明进行进一步描述。然而,应该注意给出以下实施例仅用于例示本发明而不限制本发明的范围。
<实施例1>
以95:2.5:2.5的重量比将负极活性材料(Li1.33Ti1.67O4)、导电材料(超导电乙炔炭黑(Denka black))和粘合剂(PVdF)添加到NMP中,随后混合以制备负极混合物。然后将负极混合物在厚度为20μm的铜箔上涂布形成厚度为60μm的涂层,随后轧制及干燥以制造负极。
此外,以95:2.5:2.5的重量比将作为正极活性材料的LiNi0.5Mn1.5O4、导电材料(超导电乙炔炭黑)和粘合剂(PVdF)添加到NMP中,随后混合以制备正极混合物。然后将正极混合物涂布至厚度为20μm的铜箔上,随后轧制及干燥以制造正极。
然后将聚乙烯膜(Celgard,厚度:20μm)作为隔膜置于负极和正极之间以形成电极组件。将通过溶解在体积比为1/2的EC/EMC溶剂中的1M LiPF6形成的液体电解质注入其中安装有电极组件的袋中以制造袋形电池,所述液体电解质中添加有作为磷酸酯基材料的磷酸酯基丙烯酸酯(在式(1)中,R1为H,且n为1),其添加量基于电解质的总重量为5重量%。
<实施例2>
以与实施例1中相同的方式制造袋形电池,不同之处在于将焦磷酸酯基丙烯酸酯(在式(2)中,R1为H,且n为1)用作磷酸酯基材料。
<实施例3>
以与实施例1中相同的方式制造袋形电池,不同之处在于另外将作为多官能化合物的双季戊四醇五丙烯酸酯(DPentA)以基于溶剂重量为0.2重量%的量添加至电解质中。
<实施例4>
以与实施例2中相同的方式制造袋形电池,不同之处在于另外将作为多官能化合物的双季戊四醇五丙烯酸酯(DPentA)以基于溶剂重量为0.2重量%的量添加至电解质中。
<实施例5>
以与实施例1中相同的方式制造袋形电池,不同之处在于在注入电解质后,以基于溶剂重量为0.1重量%的量将作为聚合引发剂的2,2’-偶氮异丁腈(AIBN)添加至电解质中,然后在70℃的温度下实施5小时的高温反应以制备凝胶聚合物电解质。
<实施例6>
以与实施例2中相同的方式制造袋形电池,不同之处在于在注入电解质后,以基于溶剂重量为0.1重量%的量将作为聚合引发剂的2,2’-偶氮异丁腈(AIBN)添加至电解质中,然后在70℃的温度下实施5小时的高温反应以制备凝胶聚合物电解质。
<比较例1>
以与实施例1中相同的方式制造袋形电池,不同之处在于使用其中没有添加磷酸酯基丙烯酸酯(在式(1)中,R1为H,且n为1)的电解质。
<比较例2>
以与实施例6中相同的方式制造袋形电池,不同之处在于在将磷酸酯基丙烯酸酯(在式(1)中,R1为H,且n为1)以40重量%的量添加到电解质中之后注入电解质。
<实验例1>
对在实施例1~6和比较例1和2中制造的电池(设计容量:265mAh)在2.75V下实施形成过程。在一定C倍率下,在1.6V~2.75V的范围内对电池充放电以确认其放电容量。结果示于下表1中。
表1
放电容量 | |
实施例1 | 259mAh |
实施例2 | 255mAh |
实施例3 | 256mAh |
实施例4 | 252mAh |
实施例5 | 255mAh |
实施例6 | 256mAh |
比较例1 | 250mAh |
比较例2 | 230mAh |
<实验例2>
在5C的C倍率下,在1.6V~2.75V的范围内,在45℃的室内对电池充放电的同时,测定实施例1和3以及比较例1和2中制造的电池的循环特性。结果示于图1中。
<实验例3>
对在实施例1和3以及比较例1和2中制造的电池(设计容量:265mAh)在2.75V下实施形成过程。电池在100%SOC、60℃高温下存储后,测定通过副反应导致的气体产生程度。结果示于图2中。
由图2和3可以看出,比较例1产生了过量的气体,且比较例2循环特性显著劣化,而根据本发明的实施例1~6产生少量的气体,确保了高安全性,还展现了优异的循环特性。
本领域技术人员可以以上述内容为基础,在本发明的范围内进行各种应用和变化。
工业应用性
从上述可以看出,本发明的二次电池因为将锂钛氧化物(LTO)用作负极活性材料,并将磷酸酯基化合物用作添加剂,所以二次电池实现了电极界面稳定性,从而阻止气体和副产物的产生。因此,所述二次电池不仅展现高安全性而且展现提高的使用寿命和高功率特性。
Claims (21)
1.一种二次电池,其包含电极组件和电解质,所述电极组件包含正极、负极和置于其间的隔膜,
其中所述负极包含作为负极活性材料的锂钛氧化物(LTO),且
所述电解质包含作为添加剂的磷酸酯基化合物,
其中所述磷酸酯基化合物包含选自式1的磷酸酯基丙烯酸酯、式2的焦磷酸酯基丙烯酸酯和磷酸酯基氨基甲酸酯丙烯酸酯中的至少一种,
其中R1和R2各自独立地为氢、甲基或F,且n为1~20的整数。
2.根据权利要求1所述的二次电池,其中所述电解质还包含能与所述磷酸酯基化合物聚合的多官能化合物。
3.根据权利要求2所述的二次电池,其中所述多官能化合物包含选自(甲基)丙烯酸酯化合物、不饱和碳酸化合物和乙烯基化合物中的至少一种。
4.根据权利要求3所述的二次电池,其中所述(甲基)丙烯酸酯化合物包含每个分子具有至少两个丙烯酸酯基的(甲基)丙烯酸酯化合物。
5.根据权利要求4所述的二次电池,其中所述(甲基)丙烯酸酯化合物包含由式3表示的单体或其低聚物,
其中R3、R4和R5各自独立地为氢、或取代或未取代的C1-C4烷基,且m为1~20的整数。
6.根据权利要求4所述的二次电池,其中所述(甲基)丙烯酸酯化合物包含选自以下材料中的至少一种材料:二乙二醇二丙烯酸酯、二乙二醇二甲基丙烯酸酯、乙二醇二甲基丙烯酸酯、二丙二醇二丙烯酸酯、二丙二醇二甲基丙烯酸酯、乙氧基化(6)三羟甲基丙烷三丙烯酸酯、三乙二醇二甲基丙烯酸酯、双季戊四醇五丙烯酸酯、三羟甲基丙烷三丙烯酸酯、三羟甲基丙烷三甲基丙烯酸酯、丙氧基化(3)三羟甲基丙烷三丙烯酸酯、丙氧基化(6)三羟甲基丙烷三丙烯酸酯、聚(乙二醇)二丙烯酸酯和聚(乙二醇)二甲基丙烯酸酯。
7.根据权利要求1所述的二次电池,其中基于电解质的总重量,所述电解质包含0.01重量%~30重量%的所述磷酸酯基化合物。
8.根据权利要求2所述的二次电池,其中基于电解质的总重量,所述电解质包含0.1重量%~1重量%的能与所述磷酸酯基化合物聚合的所述多官能化合物。
9.根据权利要求1所述的二次电池,其中所述电解质为液体电解质或凝胶聚合物电解质。
10.根据权利要求9所述的二次电池,其中所述电解质为液体电解质。
11.根据权利要求10所述的二次电池,其中所述液体电解质包含充当增塑剂的电解质和锂盐。
12.根据权利要求9所述的二次电池,其中所述电解质为凝胶聚合物电解质,且所述添加剂作为交联剂发生反应。
13.根据权利要求12所述的二次电池,其中所述凝胶聚合物电解质包含聚合引发剂、充当增塑剂的电解质和锂盐。
14.根据权利要求11或13所述的二次电池,其中基于包含在电解质中的固体成分的总重量,所述电解质包含0.01重量%~30重量%的锂盐。
15.根据权利要求1所述的二次电池,其中所述二次电池为锂离子聚合物电池。
16.一种制造权利要求15的二次电池的方法,该方法包括:
(a)在电池壳中安装电极组件;
(b)向所述电池壳中注入所述磷酸酯基化合物、聚合引发剂、电解质和锂盐的混合物,随后密封;以及
(c)使所述磷酸酯基化合物聚合以形成凝胶聚合物电解质。
17.根据权利要求16所述的二次电池,其中步骤(c)包括:
(c1)对电池实施热固化、通过电子束或伽马射线的照射而进行的光固化或在30℃~80℃下进行的稳定反应,以使所述磷酸酯基化合物聚合;以及
(c2)实施形成过程以活化电池,以及实施老化过程以稳定被活化的电池。
18.一种电池模块,其包含权利要求1的二次电池作为单元电池。
19.一种电池组,其包含权利要求18的电池模块。
20.一种包含权利要求19的电池组的装置。
21.根据权利要求20所述的装置,其中所述装置为电力存储系统。
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BR112014030392B1 (pt) | 2021-06-08 |
KR101558861B1 (ko) | 2015-10-12 |
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US10862165B2 (en) | 2020-12-08 |
JP2015525452A (ja) | 2015-09-03 |
IN2014DN10019A (zh) | 2015-08-14 |
KR20140008264A (ko) | 2014-01-21 |
US10056648B2 (en) | 2018-08-21 |
CN104380519A (zh) | 2015-02-25 |
JP6042533B2 (ja) | 2016-12-14 |
EP2874228B1 (en) | 2016-12-21 |
US20180323471A1 (en) | 2018-11-08 |
US20150079480A1 (en) | 2015-03-19 |
EP2874228A4 (en) | 2016-03-02 |
WO2014010936A1 (ko) | 2014-01-16 |
BR112014030392B8 (pt) | 2023-01-17 |
KR20150088773A (ko) | 2015-08-03 |
BR112014030392A2 (pt) | 2017-07-25 |
EP2874228A1 (en) | 2015-05-20 |
TWI485906B (zh) | 2015-05-21 |
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