CN103765654B - 具有优异的生产率和安全性的二次电池 - Google Patents
具有优异的生产率和安全性的二次电池 Download PDFInfo
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- CN103765654B CN103765654B CN201280042038.4A CN201280042038A CN103765654B CN 103765654 B CN103765654 B CN 103765654B CN 201280042038 A CN201280042038 A CN 201280042038A CN 103765654 B CN103765654 B CN 103765654B
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- insulator
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- electric
- electrolyte
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Abstract
本发明公开了一种二次电池,其具有其中具有正极/隔膜/负极结构的卷状物安装在圆筒状电池壳中、并且板状绝缘体安装在所述卷状物顶部的结构,其中所述绝缘体具有多孔结构,在所述多孔结构中多个细孔在纵向上、或者在横向和纵向上连通。
Description
技术领域
本发明涉及具有优异的生产率和安全性的二次电池。更具体地,本发明涉及具有如下结构的二次电池:其中具有正极/隔膜/负极结构的卷状物(jelly-roll)安装在圆筒状电池壳中、并且板状绝缘体(insulator)安装在所述卷状物的顶部,其中所述绝缘体具有多孔结构,在所述多孔结构中多个细孔在纵向上、或者在横向和纵向上连通。
背景技术
与移动装置相关的技术的开发以及为此的需求增加已经使得对作为能源的二次电池的需求快速增加。在二次电池中,将具有高能量密度、高驱动电压以及优越的存储和寿命特性的锂二次电池广泛用作包括移动装置的各种电类产品的能源。
根据电池壳的形状,二次电池可分成分别安装在圆筒状和矩状金属罐中的圆筒状和矩状电池,以及安装在由铝层压片制成的袋状壳中的袋状电池。其中,圆筒状电池具有容量相对高和结构稳定性优越的优势。安装在电池壳中的电极组件是使得能够充放电的发电装置,其具有正极/隔膜/负极层压体结构,并且分成:卷状物型,其中包含设置在各自由涂布有活性材料的长片制成的正极和负极之间的隔膜的电极组件被卷绕;堆叠型,其中将多个正极和多个负极依次层压,使得隔膜被设置在正极和负极之间;以及堆叠/折叠型,其为卷状物型和堆叠型的组合。其中,卷状物型电极组件具有制造容易和每单位重量的能量密度高的优势。
在这点上,图1中示出常规的圆筒状二次电池。图2和图3的平面图中示出通常用于圆筒状二次电池的绝缘体。
参考图2和图3,通过如下制造圆筒状二次电池100:将卷状物型(卷绕型)电极组件120安装在电池壳130中,将电解质注射到电池壳130中,并且将具有电极端子(例如正极端子;未示出)的盖组件(cap assembly)140结合到壳130的开放顶部。
通过如下获得电极组件120:将隔膜123插在正极121和负极122之间,并且将所得结构卷绕成圆形。将圆筒状中心销150插入到卷状物的核心(中心)。中心销150通常由金属制成以赋予预定强度,并且具有圆曲板材料的中空形圆筒状结构。这种中心销150安置和支撑电极组件,并且用作使得能够排放在充放电和运行期间由内部反应所产生的气体的通道。
另外,板状绝缘体180a被安装在电极组件120的顶部,并且在其中心具有与中心销150的通孔(through hole)151连通以便排放气体的开口181a,并且将电极组件120的正极极耳(cathode tap)142连接到盖组件140的盖板145。
然而,布置在卷状物顶部的绝缘体180a是阻断使得在将电解质注射到电池的过程中能够使电解质渗透到电池中的通道的结构。因此,电解质仅通过与中心销150连通的开口181a以及除绝缘体180a以外的区域而渗透到电池中,由此注射电解质会不利地需要长时间并因此导致生产率劣化。
为了提高电解质的渗透性,如图3中所示,提出具有其中在开口181b周围形成多个通孔182b的结构的部分连接构件180b。
然而,发现这种结构具有严重的安全性问题。也就是说,在制造和/或组装盖组件140、电池壳130等的过程中产生的导电杂质粒子如金属粉末会通过贯穿绝缘体180b的通孔182b而渗透到电极组件120中,由此不利地导致出现短路或电池寿命劣化。
因此,对提高电解质的注射处理性并且防止在组装电池的过程中引入异物从而延长寿命的二次电池的需求日益增大。
发明内容
技术问题
因此,为了解决有待解决的上述和其它技术问题而作出了本发明。
作为用于解决上述问题的各种广泛而深入的研究和实验的结果,本发明人开发了具有下述特定形状的绝缘体,并且发现所述绝缘体会大大提高电解质的注射性、防止在卷状物中引入在诸如熔接(beading)的组装过程期间产生的异物,并从而防止电池缺陷且提高安全性。已经基于该发现完成了本发明。
技术方案
根据本发明的一个方面,提供一种具有如下结构的二次电池:其中具有正极/隔膜/负极结构的卷状物安装在圆筒状电池壳中、并且板状绝缘体安装在所述卷状物顶部,其中所述绝缘体具有多孔结构,在所述多孔结构中多个细孔在纵向上、或者在横向和纵向上连通。因此,在根据本发明的二次电池中,通过多个具有特定形状的细孔注射电解质,结果,注射时间能够缩短并由此提高注射性。
在所述多孔结构中,细孔的尺寸、位置和数量以及其间的距离没有限制,只要其不对异物引入的防止、电解质的注射性和气体的排放造成损害即可。
优选地,所述细孔提供作为绝缘体的固有功能的电绝缘性,并在电解质注射期间对电解质具有高渗透性且具有1μm~100μm的尺寸,从而防止具有100μm以上尺寸的异物的渗透。
在此情况中,在电解质注射期间不存在将异物引入到卷状物中的危险。由此,有利地,可省略筛选并除去异物以消除由异物的引入造成的短路风险的过程并由此提高生产率。
在具体实施方式中,细孔可以在绝缘体的整个表面上彼此间隔,从而防止具有100μm以上尺寸的异物的引入,并改善电解质的注射性和气体排放。
当将电解质注射到在绝缘体的整个表面上形成的细孔中时,可使注射通道进一步分支,提高了注射性,可缩短注射时间,在细孔之间的预定距离下注射速度是恒定的,电解质可均匀地浸渗到卷状物中,且结果,有利地提高了电池性能。
另外,在绝缘体的整个表面上彼此间隔的细孔提供通道,从而使得能够排放在电解质分解期间产生的气体。就气体扩散来说,当通过分支的排放通道排放气体时可以增大排放速度。
在本发明中,表述“细孔在纵向上或者在纵向和横向上连通”是指,细孔至少在板状绝缘体中在垂直方向上连通。因此,注射到绝缘体中的电解质能够通过至少在纵向上连通的细孔而移动到绝缘体的下部。如上述所限定的,这种细孔可以不仅在纵向上,还在横向上(在板状绝缘体中在水平方向上)连通。
全部细孔不必都连通,并且优选50%以上的细孔连通,且更优选70%以上的细孔连通。可以理解,这些细孔是一种开口型孔。
这种连通细孔可以通过各种方法制造。例如,将化学或物理发泡剂添加到用于形成由聚合物树脂或聚合物复合材料制成的材料(其作为用于绝缘体的材料)的熔融物或溶液中,随后发泡,或者将可溶性填料添加到所述熔融物或溶液中并然后将填料除去,但形成细孔的方法不限于此。
在具体实施方式中,所述连通的细孔可以由发泡剂的处理来形成。物理发泡剂的实例包括用于诸如发泡聚苯乙烯(EPS)和EPP的产品的丁烷、戊烷等。化学发泡剂的实例包括无机发泡剂如碳酸氢钠(NaHCO3)以及有机发泡剂如偶氮二甲酰胺(ADAC)、P,P’-氧基双苯磺酰肼(OBSH)和对甲苯磺酰肼(TSH)。
通常,随着孔隙率增大,绝缘体的密度下降且机械性能劣化。基于该原因,通过向聚合物树脂或聚合物树脂复合材料中添加增强填料,能够保持孔隙率并能够确保期望的机械性能。增强填料可以具有粒状或纤维状形状,且其含量没有特别限制。例如,基于绝缘体的总重量,填料的含量为0.5~20重量%,优选1~10重量%。
绝缘体可以由任意绝缘材料制成而没有特别限制,且例如由电绝缘树脂或电绝缘聚合物复合材料制成。具体地,聚合物树脂可以为选自如下的一种或多种:聚乙烯(PE)、聚丙烯(PP)、聚丁烯(PB)、聚苯乙烯(PS)、聚对苯二甲酸乙二醇酯(PET)、天然橡胶和合成橡胶。
另外,绝缘体的总厚度为0.1mm~0.5mm。当绝缘体的厚度过小时,可能不会充分发挥绝缘体的固有电绝缘功能,并且当其厚度过大时,不利地,在尺寸相同的电池壳中,卷状物尺寸减小并且电池容量由此减小。
优选地,绝缘体包含开口以使得电极端子能够穿过。
优选地,可以将根据本发明的二次电池应用于通过将含锂电解质浸渗在卷状物中而制造的锂二次电池。
通常,锂二次电池包含正极、负极、隔膜、含锂水性电解质等。
例如,通过如下制造正极:通过将含有正极活性材料并任选地含有导电材料、粘合剂、填料等的正极混合物与溶剂如NMP混合以制备浆料,并将所述浆料涂布至正极集电器,随后进行干燥和轧制。
正极活性材料的实例包括但不限于层状化合物如锂钴氧化物(LiCoO2)或锂镍氧化物(LiNiO2)或被一种以上过渡金属置换的所述化合物;锂锰氧化物如Li1+yMn2-yO4(其中y是0~0.33)、LiMnO3和LiMn2O3,以及LiMnO2;锂铜氧化物(Li2CuO2);钒氧化物如LiV3O8、LiFe3O4、V2O5和Cu2V2O7;由LiNi1-yMyO2(其中M=Co、Mn、Al、Cu、Fe、Mg、B或Ga,y=0.01~0.3)表示的Ni位点型锂镍氧化物;由式LiMn2-yMyO2(其中M=Co、Ni、Fe、Cr、Zn或Ta,y=0.01~0.1)或Li2Mn3MO8(其中M=Fe、Co、Ni、Cu或Zn)表示的锂锰复合氧化物;其中Li的一部分被碱土金属离子置换的LiMn2O4;二硫化合物;Fe2(MoO4)3等。
通常将正极集电器制成具有3μm~500μm的厚度。可以使用任意正极集电器而没有特别限制,只要其具有合适的导电性而不在制造的电池中造成不利的化学变化即可。正极集电器的实例包括不锈钢,铝,镍,钛,烧结碳,以及用碳、镍、钛或银表面处理过的铝或不锈钢。这些集电器在其表面上包含细小的不规则以增强对电极活性材料的粘合。另外,可以以包括膜、片、箔、网、多孔结构、泡沫和无纺布的各种形式使用集电器。
基于包含正极活性材料的混合物的总重量,通常以1重量%至30重量%的量使用导电材料。可以使用任意导电材料而没有特别限制,只要其具有合适的导电性而不在电池中造成不利的化学变化即可。导电材料的实例包括导电材料,包括石墨;碳黑如碳黑、乙炔黑、科琴黑、槽法碳黑、炉黑、灯黑和热裂法碳黑;导电纤维如碳纤维和金属纤维;金属粉末如氟化碳粉末、铝粉末和镍粉末;导电晶须如氧化锌和钛酸钾;导电金属氧化物如二氧化钛;以及聚苯撑衍生物。
粘合剂是增强电极活性材料对导电材料和集电器的粘合的组分。基于包含正极活性材料的混合物的总重量,通常以1重量%至30重量%的量添加粘合剂。粘合剂的实例包括聚乙二烯(polyvinylidene)、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、氟橡胶以及各种共聚物。
填料是任选地用于抑制电极膨胀的组分。可以使用任意填料而没有特别限制,只要所述填料不在制造的电池中造成不利的化学变化并且是纤维材料即可。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。
隔膜设置在正极和负极之间。将具有高离子渗透性和机械强度的绝缘薄膜用作隔膜。所述隔膜典型地具有0.01μm~10μm的孔径和5μm~300μm的厚度。将具有耐化学性和疏水性的、由烯烃聚合物如聚丙烯和/或玻璃纤维或聚乙烯制成的片或无纺布用作隔膜。当将诸如聚合物的固体电解质用作电解质时,所述固体电解质也可以充当隔膜和电解质两者。
例如,通过如下制造负极:通过将含有负极活性材料的负极混合物与溶剂如NMP混合以制备浆料,并将所述浆料涂布至负极集电器,随后进行干燥和轧制。负极混合物可以进一步任选地含有上述组分。
负极活性材料的实例包括碳如硬碳、石墨基碳;金属复合氧化物如LixFe2O3(0≤x≤1)、LixWO2(0≤x≤1)、SnxMe1-xMe’yOz(Me:Mn,Fe,Pb,Ge;Me’:Al,B,P,Si,I、II和III族元素,卤素;0<x≤1;1≤y≤3;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;Li-Co-Ni基材料等。
通常将负极集电器制成具有3μm~500μm的厚度。可以使用任意负极集电器而没有特别限制,只要其具有合适的导电性而不在制造的电池中造成不利的化学变化即可。负极集电器的实例包括铜,不锈钢,铝,镍,钛,烧结碳,以及用碳、镍、钛或银表面处理过的铜或不锈钢,以及铝-镉合金。类似于正极集电器,所述集电器在其表面上包含细小的不规则以增强对电极活性材料的粘合。另外,可以以包括膜、片、箔、网、多孔结构、泡沫和无纺布的各种形式使用集电器。
同时,电解质由非水电解质和锂盐组成。优选电解质的实例包括非水有机溶剂、有机固体电解质、无机固体电解质等。
非水溶剂的实例包括非质子性有机溶剂如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、γ-丁内酯、1,2-二甲氧基乙烷、四羟基franc、2-甲基四氢呋喃、二甲亚砜、1,3-二氧戊烷、甲酰胺、二甲基甲酰胺、二氧戊烷、乙腈、硝基甲烷、甲酸甲酯、乙酸甲酯、磷酸三酯、三甲氧基甲烷、二氧戊烷衍生物、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聚乙烯衍生物、聚氧化乙烯衍生物、聚氧化丙烯衍生物、磷酸酯聚合物、聚搅拌赖氨酸(poly agitation 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。
锂盐是易溶于上述非水电解质中的材料并且其实例包括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。
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(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。如果必要,为了赋予不燃性,非水电解质可以进一步包含含卤素的溶剂如四氯化碳和三氟乙烯。此外,为了提高高温存储特性,非水电解质可另外含有二氧化碳气体、氟代碳酸亚乙酯(FEC)、丙烯磺酸内酯(PRS)或氟代碳酸亚丙酯(FPC)。
本发明还提供包含所述二次电池作为电源的装置,并且就优越的寿命和安全性来说,优选将根据本发明的装置用于移动装置如移动电话和可携式电脑以及电动自行车(E-自行车)、电动车辆(EV)、混合动力车辆(HEV)、插电式混合动力车辆和电力存储装置。
锂二次电池、以及包含锂二次电池作为单元电池的中型和大型电池模块和装置的结构和制造方法在本领域中是熟知的并因此将其详细描述省略。
发明效果
如根据前述内容显而易见,根据本发明的二次电池不需要筛选并除去异物的过程并能够使电解质的注射通道分支,由此有利地大大提高生产率。
根据本发明的二次电池没有由引入异物导致的短路风险并且改善了气体排放,由此提高了安全性。
此外,因为卷状物均匀地浸渗在电解质中,所以根据本发明的二次电池改善了倍率特性。
此外,根据本发明的二次电池能够保持孔隙率并确保期望的机械强度,由此提高生产率。
附图说明
根据以下详细描述并结合附图,将更加清楚地理解本发明的上述和其它目的、特征和其它优势,其中:
图1是示出代表性圆筒状二次电池的示意性截面图;
图2是示出根据一个实施方式的用于图1二次电池的绝缘体的平面图;
图3是示出根据另一实施方式的用于图1二次电池的绝缘体的平面图;并且
图4是示出根据本发明的一个实施方式的绝缘体的平面图。
具体实施方式
现在,将参考以下实施例更详细地描述本发明。提供这些实施例仅为了说明本发明并且不应将其解释为限制本发明的范围和主旨。
图4是示意性示出根据本发明的一个实施方式的绝缘体的平面图。
参考图4和图1,二次电池100具有其中具有正极121/隔膜123/负极122结构的卷状物120安装在圆筒状电池壳130中的结构,其中绝缘体180c安装在卷状物120的顶部。
绝缘体180c包含厚度为约0.4mm的聚对苯二甲酸乙二醇酯(PET),在其一侧设置有开口181c,并且在其整个表面上设置有多个直径为10μm~30μm的彼此间隔预定距离的细孔182c。
因此,电解质在注射之后通过所述多个细孔182c渗透到绝缘体180c的整个表面,由此使得注射性大大改善并且防止短路。
现在,将参考以下实施例更详细地描述本发明。提供这些实施例仅为了说明本发明并且不应将其解释为限制本发明的范围和主旨。
[实施例1]
如图4中所示,使用PET作为材料并使用ADAC作为发泡剂制造厚度为0.4mm的绝缘体,所述绝缘体包含在其一侧穿孔的宽度为6mm并且长度为2.5mm的矩状开口,并且在其整个表面上包含多个直径为约10μm~约30μm的、以约10μm~约30μm预定距离均匀分布的细孔。然后,将绝缘体安装在其中正极/隔膜/负极结构基于中心销卷绕的卷状物的顶部,并且在将在电池组装的过程中产生的细金属粉末置于绝缘体上的状态下制造18650标准(直径18mm、长度65mm)的圆筒状二次电池。
[实施例2]
以与实施例1中相同的方式制造绝缘体和二次电池,不同之处在于制备了在其整个表面上包含多个以约120μm预定距离均匀分布的、直径为100μm的细孔的绝缘体。
[比较例1]
以与实施例1中相同的方式制造绝缘体和二次电池,不同之处在于不包含多个细孔,如图2中所示。
[比较例2]
以与实施例1中相同的方式制造绝缘体和二次电池,不同之处在于形成三个直径为2.5mm的通孔以代替细孔,如图3中所示。
[比较例3]
以与实施例1中相同的方式制造绝缘体和二次电池,不同之处在于制备了在其整个表面上包含多个以约120μm预定距离均匀分布的、直径为150μm的细孔的绝缘体。
[试验例1]
对实施例1和实施例2以及比较例1~比较例3中制造的二次电池进行电解质浸渗试验。下表1中示出结果。通过如下进行电解质浸渗试验:将1M LiPF6碳酸酯电解质注射到所制造的圆筒状电池壳中,测量卷状物的浸渗比达到100%所用的时间,重复这个过程四次并计算四个值的平均值。
另外,将盖组件焊接至所制造的二次电池的开放顶部以制造10个样品。对样品进行充放电试验并且确认短路的产生。下表1中示出结果。
[表1]
如从表1可见,与比较例1相比,根据本发明的实施例1~实施例2的电池的电解质浸渗时间大大缩短。也就是说,可见电解质有效地渗透通过在绝缘体中形成的多个细孔。
与比较例1的电池相比,尽管比较例2的电池显示浸渗改善,但是短路增加;而尽管比较例3的电池也显示与实施例1和实施例2相当的浸渗,但是显示更高的短路比。发现其原因在于金属粉末渗透到相对大的孔中,从而导致卷状物中的短路。
另一方面,比较例1的电池虽然在安装在电池上的绝缘体中没有贯穿细孔,但是与实施例1和实施例2的电池相比,比较例1的电池显示高的短路比。认为短路比高的原因归因于以下事实:在实施例1和实施例2的电池中,当金属粉末陷入在细孔中时,金属粉末的移动受到抑制,而在比较例1的电池中,金属粉末会在绝缘体的光滑表面上自由移动、并由此通过开口或绝缘体的周围移动至卷状物。
虽然为了例示性目的而公开了本发明的优选实施方式,但是本领域技术人员应了解,在不偏离如在随附权利要求书中公开的本发明的范围和主旨的情况下,可能有各种修改、增加和替代。
Claims (10)
1.一种二次电池,具有其中具有正极/隔膜/负极结构的卷状物安装在圆筒状电池壳中、并且板状绝缘体安装在所述卷状物顶部的结构,
其中所述绝缘体具有多孔结构,在所述多孔结构中多个细孔在纵向上、或者在横向和纵向上连通,且所述绝缘体还包含增强填料以提高机械强度,以及
其中所述增强填料具有粒状或纤维状形状。
2.如权利要求1所述的二次电池,其中所述细孔形成在所述绝缘体的整个表面上。
3.如权利要求1所述的二次电池,其中所述绝缘体包含电绝缘聚合物树脂或电绝缘聚合物复合材料。
4.如权利要求3所述的二次电池,其中所述聚合物树脂为选自如下的至少一种:聚乙烯、聚丙烯、聚丁烯、聚苯乙烯、聚对苯二甲酸乙二醇酯、天然橡胶和合成橡胶。
5.如权利要求1所述的二次电池,其中所述绝缘体具有0.1mm~0.5mm的厚度。
6.如权利要求1所述的二次电池,其中所述绝缘体包含开口以使得电极端子能够穿过。
7.如权利要求1所述的二次电池,其中所述电池为锂二次电池。
8.一种移动装置,包含权利要求1~7中任一项的二次电池作为电源。
9.如权利要求8所述的移动装置,其中所述移动装置选自:移动电话、可携式电脑、电动自行车、电动车辆、混合动力车辆和电力存储装置。
10.如权利要求9所述的移动装置,其中所述混合动力车辆是插电式混合动力车辆。
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KR10-2011-0097269 | 2011-09-27 | ||
PCT/KR2012/007434 WO2013048045A1 (ko) | 2011-09-27 | 2012-09-18 | 우수한 제조 공정성과 안전성의 이차전지 |
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KR102254262B1 (ko) * | 2017-05-24 | 2021-05-21 | 주식회사 엘지에너지솔루션 | 이차전지 및 그 이차전지의 절연부재 제조 방법 |
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JP5968440B2 (ja) | 2016-08-10 |
EP2738859A4 (en) | 2014-06-11 |
KR101275775B1 (ko) | 2013-06-17 |
EP2738859B1 (en) | 2015-04-22 |
US20140178725A1 (en) | 2014-06-26 |
EP2738859A1 (en) | 2014-06-04 |
TWI459615B (zh) | 2014-11-01 |
KR20130033553A (ko) | 2013-04-04 |
JP2014527705A (ja) | 2014-10-16 |
US9236630B2 (en) | 2016-01-12 |
CN103765654A (zh) | 2014-04-30 |
TW201334266A (zh) | 2013-08-16 |
WO2013048045A1 (ko) | 2013-04-04 |
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