CN101087687B - 层状产品和二次电池 - Google Patents
层状产品和二次电池 Download PDFInfo
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- CN101087687B CN101087687B CN2005800448089A CN200580044808A CN101087687B CN 101087687 B CN101087687 B CN 101087687B CN 2005800448089 A CN2005800448089 A CN 2005800448089A CN 200580044808 A CN200580044808 A CN 200580044808A CN 101087687 B CN101087687 B CN 101087687B
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- laminar product
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Abstract
本发明涉及一种层状产品,其中至少铝箔、化学转化层、对金属具有粘合性的烯烃树脂层和热粘结树脂层被连续层压在基底层上。在烯烃树脂层和热粘结树脂层之间形成通过具有交联基团的含氟共聚物和与交联基团反应的固化剂形成的氟树脂层。
Description
技术领域
本发明涉及二次电池,更特别地,涉及封装具有电解质(如液体电解质和固体电解质)的锂电池主体的层状产品和包括这种层状产品的二次电池。
背景技术
锂电池也称为锂二次电池,是一种由用作电解质的固体聚合物、凝胶聚合物、液体等组成并通过锂离子的运动产生电的电池,并包括其中正极/负极活性材料由大分子聚合物形成的这类电池。锂二次电池由具有以下组成的锂电池主体构成:正极集电器材料(铝,镍)/正极活性物质层(正极材料如金属氧化物、炭黑、金属硫化物、电解质溶液和聚合物例如聚丙烯腈)/电解质(碳酸盐电解质如聚碳酸异丙烯酯、碳酸亚乙酯、碳酸二甲酯和甲基碳酸亚乙酯,由锂盐制成的无机固体电解质或凝胶电解质)/负极活性物质层(负极材料如锂金属、合金、碳、电解质溶液和聚合物例如聚丙烯腈)/负极集电器材料(铜、镍或不锈钢);和容纳这些元件的外部护套元件.具有高容积效率和重量效率的锂二次电池广泛用于电子装置和电子零件,尤其是用于蜂窝式电话、笔记本型个人计算机、摄像机等.
锂电池的外部护套元件主要被分成通过金属接合工艺密封具有圆筒形状、矩形六面体形状等的金属罐的一种类型和热粘合并密封具有弹性的层状产品的另一种类型,从容易取出金属端子、容易密封和弹性的观点看,已开始使用通过层压塑料薄膜和金属箔如铝等形成的层状产品,其可被成形为适合电子装置或电子零件空间的合适形状,从而能在一定程度上自由设计电子装置或电子零件的形状来容易地实现小型和重量轻.
由于层状产品要求锂电池所需的性质如防汽性质、密封性质、抗穿孔性质、绝缘性质、耐热和耐冷性质、抗电解质性质(耐电解质溶液性质)和耐腐蚀性质(耐电解质变质和水解产生的氢氟酸性质)作为必不可少的基本性质,因此通常使用这种层状产品,其具有由基底层、阻挡层和内层构成的结构,其中基底层提供抗穿孔性质和防止从外部传导电流,阻挡层由金属箔如铝等制成,其确保防汽性质,内层具有对以伸出方式连接到锂电池主体的各个正极和负极的金属端子的优良粘合性质,或内层具有热粘合性质以便确保密封性质.
对于锂电池结构,可使用如图2(b)中所示的袋型,其中上述层状产品被加工成具有如图2(a)所示的具有周边热粘合部分的袋形状[图2(a)显示了枕头型封装袋;但是,可使用三通型或四通型封装袋],锂电池主体(未示出)容纳在其中,金属端子连接到各自的正极和负极上,伸出到外面,开口部分通过热粘合工艺密封;或可使用如图3(b)中所示的模制型,其中层状产品被模压形成如图3(a)所示的凹面部分,锂电池主体(未示出)容纳在凹面部分中,金属端子连接到各自的正极和负极上,伸出到外面,凹面部分涂有制成分离元件的片形状层状产品,四个周边被热粘合来密封.尽管图中未示出,但模制型包括另外一种模制型,其中代替覆盖凹面部分的片形状封装元件,使用如图3(a)所示的模压材料,从而在通过热粘合四个周边密封的两个侧面上形成凹面部分.图2和3中显示的袋型或模制型视为本发明的锂电池的模式.图2和3中显示的引用数字11、12、13和14代表层状产品,符号D代表锂电池,符号S代表周围热粘合部分,符号T代表金属端子.
在任何一种上述模式的锂电池中,当用层状产品密封锂电池主体时,必须进行密封过程,金属端子分别连接到锂电池主体的正极和负极上,允许伸到外面,金属端子被热粘合,同时夹在层状产品之间.由于这个原因,通常使用这种方法,即对金属具有优良粘合性质的热粘合树脂例如已用不饱和羧酸接枝改性的酸改性烯烃树脂用于层状产品的内层,以便被热粘合和密封,或使用另一种方法,其中对金属粘合性质较差的普通烯烃树脂(指由碳和氢制成的直链或支链烯烃树脂,下文中,称为普通聚烯烃树脂)用于内层,对金属具有优良粘合性质的由上述酸改性烯烃树脂制成的金属端子部分密封粘合薄膜夹在金属端子合内层之间,以便被热粘合和密封。
但是,在这种情况下,为了确保通过热粘合过程密封金属端子,且金属端子夹在层状产品之间,必须准备与热、压力和时间有关的所需热量,并且在热量太高的情况下,金属端子接触由金属箔如铝制成的层状产品阻挡层,导致短路问题;因此,需要热粘合和密封过程的严格条件管理。由于这个原因,需要能减轻这些条件管理的层状产品,也就是即使在过量热量情况下也不容易短路的层状产品.另一个问题在于当任何力被施加到部分热粘合(热粘合部分)的内部端部分时,往往在内部端部分中出现裂纹,结果电解质溶液从裂开部分侵入来腐蚀由金属箔如铝制成的阻挡层,损害作为电池的功能.
还存在一个问题,如前所述,由于层状产品的层结构由基底层和金属箔如铝制成的阻挡层和内层构成,并使用六氟磷酸锂溶液作为锂电池主体中的电解质溶液,其与湿气反应产生氢氟酸,结果这种氢氟酸渗透到层状产品的内层内,引起金属箔和内层之间粘着力下降,导致剥离和随之的电池短寿命;因此,要求用于锂电池的层状产品具有阻挡湿气从外部空气中侵入其中的性能.
由于这个原因,对于金属箔如铝制成的阻挡层和内层的层压方法,通常采用热层压方法(例如,见专利文献2),与使用已知的聚酯材料等的干层压用途粘合剂的干层压方法(例如,参见专利文献1)相比,其能减少端面的湿气渗透,但生产率(加工能力)较差。这样的原因解释如下:已知的干层压用途粘合剂在干燥后的施加厚度为约3-5μm;但是,来自粘合剂端面的湿气渗透是明显的,结果从端面侵入的湿气渗透到内层与电解质溶液反应产生氢氟酸,随着时间流逝导致金属箔如铝制成的阻挡层和内层之间分离.
还进行了另外的尝试,其中在层状产品的金属箔如铝制成的阻挡层的内层侧面上形成耐腐蚀涂层薄膜,以便防止阻挡层和内层之间的分离(例如,见专利文献3).专利文献3公开的这种技术具有通过形成经过铬处理的涂层薄膜作为耐腐蚀涂层薄膜的布置,防止了金属箔如铝制成的阻挡层和内层之间的分离;但是,经过铬处理的这种涂层薄膜通过使用常规已知的铬酸盐处理溶液来形成,铬酸盐处理溶液主要由氧化铬和聚丙烯酸、或氧化铬和磷酸、或氧化铬组成,从而这种技术对防止金属箔如铝制成的阻挡层和内层之间的分离在特定的固定时间内有效,并形成重要的方法;但是,作为加速试验的结果,出现了问题,其中粘合强度随时间流逝降低.
[专利文献1]日本专利公布No.7-19589
[专利文献2]日本专利公布No.4-58146
[专利文献3]日本专利申请公开No.2000-357494
发明公开内容
发明要解决的问题
本发明涉及用于一类锂电池的层状产品,其中锂电池主体夹有金属端子,金属端子分别连接到其正极和负极上并伸到外面,被热粘合密封,本发明的目的是提供一种层状产品,其中使粘合强度在金属箔内侧上的部分中更强,并且其在耐电解质溶液性能、抗破裂性能、防止金属箔和端子之间短路的抗短路性能和水蒸汽不透性能方面优良。另一目的是提供用在锂电池中的层状产品,其具有上述性能并且还在生产率方面良好。
解决问题的手段
为了达到上述目的,根据本发明的层状产品具有这样的结构,其中至少基底层、铝箔、化学转化层、对金属具有粘合性的烯烃树脂层和热粘结树脂层被连续层压,并在烯烃树脂层和热粘结树脂层之间插入通过具有交联基团的含氟共聚物和与交联基团反应的固化剂形成的氟树脂层。
对于这种布置,由于在层压对金属具有粘合性的烯烃树脂层和热粘结树脂层时在中间插入水蒸汽不透性能、耐热性和粘合性优良的氟树脂层;因此,可提供很难具有湿气透过并且耐电解质溶良性能、抗破裂性能和抗短路性能优良的层状产品.
对于本发明的层状产品,可使用酸改性聚烯烃树脂作为烯烃树脂层。
对于本发明的层状产品,可使用聚烯烃树脂或酸改性聚烯烃树脂作为热粘结树脂层。
对于本发明的层状产品,可使用包含至少一种氟-烯烃单体和含羟基单体作为单体成分的材料作为含氟共聚物。
对于本发明的层状产品,可使用有机多异氰酸酯化合物作为固化剂。
对于本发明的层状产品,可通过使用包含胺化酚醛聚合物、三价铬化合物和磷化合物的化学转化溶液形成化学转化层.利用这种布置,可提供在铝箔和对金属具有粘合性的烯烃树脂层之间粘结强度优良的层状产品.
可使用本发明的层状产品形成下面的二次电池.换句话说,二次电池特征在于具有用多个引线密封电池容器的结构,引线分别连接到电池主体的正极和负极上,伸出电池容器外,在这种结构中,电池容器由层状产品制成,其中通过连续层压至少基底层、铝箔、化学转化层、对金属具有粘合性的烯烃树脂层和热粘结树脂层形成层状产品,并在烯烃树脂层和热粘结树脂层之间插入通过具有交联基团的含氟共聚物和与交联基团反应的固化剂形成的氟树脂层.
发明效果
在本发明的层状产品中,由于在对金属具有粘合性的烯烃树脂层和热粘结树脂层之间形成通过具有交联基团的含氟共聚物和与交联基团反应的固化剂形成的氟树脂层,因此可得到以下效果:在金属箔内侧上的部分中粘结强度更强,和可获得优良性能,如耐电解质溶液性能、抗破裂性能、抗短路性能和水蒸汽不透性能.使用本发明的层状产品的二次电池可靠性优异并具有较长的寿命.
附图简述
图1为显示根据本发明的层状产品的一种实施方案的层状结构的截面示意图.
图2A为显示常规锂电池结构的一个例子的透视示意图.
图2B为显示常规锂电池结构的另一个例子的透视示意图.
图3A为显示常规层状产品结构的一个例子的透视示意图.
图3B为显示常规锂电池结构的一个例子的透视示意图.
(附图标记)
1层状产品
2基底层
3铝箔
4化学转化层
5对金属具有粘合性的烯烃树脂层
6氟树脂层
7热粘结树脂层
实施发明的最佳方式
参考图,下面的说明将详细地讨论本发明.
图1为显示根据本发明的层状产品的一种实施方案的层状结构的截面示意图,层状产品1具有铝箔3、化学转化层4、对金属具有粘合性的烯烃树脂层5、氟树脂层6和热粘结树脂层7被顺序层压到基底层2上的结构。
基底层由因良好的机械强度而在双轴方向上扩展的聚酯薄膜或聚酰胺薄膜或这些薄膜的层压薄膜制成,形成基底层以便保护将在下文中描述的铝箔,以及提高抗穿孔性能,尤其是抵抗外部施加的穿孔力。对于聚酯薄膜,其例子包括由聚对苯二甲酸乙二醇酯(下文中称为PET)、聚对苯二甲酸丁二醇酯、聚萘二甲酸乙二醇酯(下文中称为PEN)、聚萘二甲酸丁二醇酯、聚碳酸酯等制成的薄膜.对于聚酰胺薄膜,其例子包括由尼龙6(下文中称为ON)、尼龙6,6和尼龙6,10制成的薄膜.基底层2的厚度优选设为6μm或以上.这样做的原因解释如下:薄于6μm的厚度会导致在层中出现针孔的可能性和保护铝箔抵抗外力作用的降低,尤其是模制型的情况下(见图3),在铝箔中往往出现针孔和撕裂,导致成型失败;因此,优选设定厚度为12μm或以上。当基底层厚过25μm时,不管它是单层还是多层薄膜,从保护铝箔抵抗外力以引起体积和重量能量密度降低的角度来看不能获得显著的作用;因此,从成本和效果之间关系的角度看,应用这种基底层是不优选的.上述聚酯薄膜和聚酰胺薄膜可在其需要表面上进行易粘结处理如电晕放电处理、臭氧处理和等离子处理.
下面的描述将讨论铝箔.形成铝箔以便防止水蒸汽从外部进入到电池内部,从确保适宜的水蒸气不透性能和加工操作中的可加工性的角度看,优选设计铝箔具有20-100μm的厚度。当厚度薄于20μm时,铝箔本身可能会有针孔,导致较高的水蒸气侵入风险,同时,当厚度厚于100μm时,在铝箔针孔防止方面不能得到明显效果,不能进一步提高水蒸汽不透性能以导致体积和重量能量密度降低;因此,从成本和效果之间的关系的角度看,应用这种基底层是不优选的.
与不包含铁成分的铝箔相比,铝箔优选包含0.3-9.0wt%、优选0.7-2.0wt%范围内的铁成分,这种铝箔铺展性优异,并且不会由于弯曲出现针孔;因此,尤其为了得到在压模时没有偏向厚度地均匀形成的模制产品(见图3),优选在层状产品1中使用包含铁成分的铝箔。在铁含量小于0.3wt%的情况下,在防止针孔出现以及铺展性方面不能得到效果,超过9.0wt%的铁含量导致铝箔弹性下降和随后的成型适用性下降。
通过冷轧工艺制造铝箔,它的弹性、韧性和硬度根据退火条件(通常所说的回火工艺)变化,要在本发明中使用的铝箔优选不被制备成未经退火处理的硬化产品,而是被制成通过轻微或完全退火处理被相对软化的铝箔.可根据需要适当地确定决定铝箔弹性、韧性和硬度的退火条件,取决于层状产品1是用作袋型产品(见图2)还是用作模制型产品(见图3)。
下面的描述将讨论化学转化层.化学转化层用于使铝箔牢固地粘着到对金属具有粘合性的烯烃树脂层(下文中称为金属-粘合烯烃树脂层)上,以便防止由于电解质溶液产生的氢氟酸和电解质溶液水解引起的分层,以及用于防止模制型产品情况下压模操作时的分层。通过铬-转化处理或非铬转化处理(涂覆型)在铝箔的表面上形成化学转化层,铬-转化处理如铬酸铬酸盐处理、磷酸铬酸盐处理和涂覆型铬酸盐处理,非铬转化处理使用材料如锆、钛和锌磷酸盐;从对金属-粘合烯烃树脂层的牢固粘结性和由于不需要水洗过程而能连续加工的能力得到的低加工成本角度看,化学转化层优选通过涂覆型形成处理来形成,尤其通过使用包含胺化酚醛聚合物、三价铬化合物和磷化合物的处理溶液.
首先,下面的描述将讨论胺化酚醛聚合物.对于胺化酚醛聚合物,可普遍使用那些常规已知的聚合物;例如,使用由下面的式(1)、(2)、(3)和(4)表示的重复单元组成的一种或二种或多种胺化酚醛聚合物。优选地,使用用式(1)表示的胺化酚醛聚合物。在式中,X代表氢原子、羟基、烷基、羟基烷基、烯丙基或苄基,更优选地,代表氢原子、羟基和羟基烷基中的任何一个.R1和R2代表羟基、烷基和羟基烷基,并可为相同基团或不同基团。
在下面的式(1)-(4)中,用X、R1和R2代表的羟基烷基的例子包括具有1-4个碳原子的直链或支链烷基,如甲基、乙基、正丙基、异丙基、正丁基、异丁基和叔丁基.用X、R1和R2代表的羟基烷基的例子包括具有1-4个碳原子的直链或支链烷基,其中一个羟基被取代,如羟基甲基、1-羟基乙基、2-羟基乙基、1-羟基丙基、2-羟基丙基、3-羟基丙基、1-羟基丁基、2-羟基丁基、3-羟基丁基和4-羟基丁基.
用下面的式(1)或(3)代表的胺化酚醛聚合物为包含约80mol%或以下的重复单元的胺化酚醛聚合物,优选重复单元的比例为约25-约55mol%.数均胺化酚醛聚合物优选设为约500-1,000,000,优选约1000-20,000.通过聚缩制造胺化酚醛聚合物,例如,酚醛化合物或萘酚化合物与甲醛首先形成由用下面的式(1)或(3)代表的重复单元构成的聚合物,然后通过使用甲醛和胺(R1R2NH)将水溶性官能团(-CH2NR1R2)引入到这种聚合物内.可使用一种胺化酚醛聚合物,或以混合方式使用它的两种或多种.
式1
式2
式3
式4
下面的描述将讨论三价铬化合物.对于三价铬化合物,可普遍使用那些常规已知的化合物,其例子包括:硝酸铬、氟化铬、硫酸铬、醋酸铬、草酸铬、磷酸氢铬、铬酸乙酰基醋酸酯(acetylacetatechromate)、氯化铬和硫酸铬钾,并优选使用硫酸铬和氟化铬.
下面的描述将讨论磷化合物.对于磷化合物,可普遍使用那些常规已知的化合物,其例子包括:浓磷酸如磷酸和聚磷酸,和它们的盐.对于盐,其例子包括:铵盐和碱金属盐如钠盐和钾盐.
通过使用包含胺化酚醛聚合物、三价铬化合物和磷化合物的处理溶液形成的化学转化层4每1m2层按一定比率包含约1-200mg胺化酚醛聚合物、铬转化中的约0.5-50mg三价铬化合物和磷转化中的约0.5-50mg磷化合物,并优选每1m2层按一定比率包含约5.0-150mg胺化酚醛聚合物、铬转化中的约1.0-40mg三价铬化合物和磷转化中的约1.0-40mg磷化合物.在这种情况下,对于干燥温度,优选在150-250℃、优选170-250℃的温度下进行加热过程(焙烧过程).
对于化学转化层的形成方法,通过使用常规已知的涂覆方法施加处理溶液,适当选择棒涂、辊涂、凹板式涂覆或浸涂.在形成化学转化层前,对铝箔表面预先进行已知的脱脂处理,如碱浸渍方法、电解洗涤法、酸洗法、电解酸洗法和酸活化法;因此,化学转化层的功能理想地被发挥到最大,并保持长的时间.
下面的描述将讨论金属粘合烯烃树脂层。对于金属粘合烯烃树脂层,可使用酸改性聚烯烃树脂,例如,通过不饱和羧酸接枝改性的聚烯烃树脂,和酸改性聚烯烃树脂,如乙烯或丙烯和丙烯酸或甲基丙烯酸之间的共聚物,并优选使用通过不饱和羧酸接枝改性的聚烯烃树脂形成层.这样做的原因是因为,与酸改性聚烯烃树脂如乙烯或丙烯和丙烯酸或甲基丙烯酸之间的共聚物相比,通过不饱和羧酸接枝改性的聚烯烃树脂耐热性较好.金属粘合烯烃树脂层的厚度优选设在5-20μm的范围内,优选为10-15μm,小于5μm的厚度不能提供充分的层压强度,而超过20μm的厚度往往引起端面湿气渗透增加,导致电池功能下降。通过考虑对氟树脂层的粘合性,氟树脂层将在下文中描述,对金属粘合烯烃树脂层的暴露表面进行易粘结处理,如电晕放电处理、臭氧处理和等离子处理。
下面的描述将讨论氟树脂层.氟树脂层用于将金属粘合树脂层5和热粘结树脂层彼此粘结,以及用于使金属箔内侧上的部分中粘结强度更强.要在本发明中使用的氟树脂为用具有交联基团的含氟共聚物和能与交联基团反应的固化剂形成的氟树脂。对于具有交联基团的含氟共聚物,可使用溶于常用有机溶剂并包含羟基、环氧基、羧基、酰胺基、氨基或水解甲硅烷基作为交联基团的那些聚合物.含氟共聚物至少包含氟烯烃单体和可与氟烯烃单体共聚的含交联基团单体作为它的单体成分.含交联基团单体的例子包括:含羟基的单体,如2-羟基乙基乙烯基醚、3-羟基丙基乙烯基醚、2-羟基丙基乙烯基醚、2-羟基-2-甲基丙基乙烯基醚、4-羟基丁基乙烯基醚、5-羟基戊基乙烯基醚、6-羟基己基乙烯基醚、2-羟基乙基烯丙基醚和4-羟基丁基烯丙基醚;含环氧基的单体,如缩水甘油基乙烯基醚和缩水甘油基(甲基)丙烯酸酯;含羧基的单体,如丙烯酸和甲基丙烯酸;含酰胺基的单体,如(甲基)丙烯酰胺和N-羟甲基丙烯酰胺;含氨基的单体,如氨基烷基乙烯基醚和氨基烷基烯丙基醚;和含水解甲硅烷基的单体,如三甲氧基乙烯基硅烷、三乙氧基乙烯基硅烷和γ-甲基丙烯酰氧丙基三甲氧基硅烷;在这些中,优选使用含羟基的单体。这种材料允许使用凹板式涂覆法容易加工,并提供合适的固化速度.
为了提高涂层性能和薄膜-涂层特性(硬度、弹性等),除了氟烯烃单体和含交联基团的单体外,本发明中使用的含氟共聚物还可与能与上述两种单体共聚的单体共聚.本发明的含氟共聚物优选至少包含用1)式:CF2=CFX[在式中,X表示氟原子、氯原子、氢原子或三氟甲基]代表的氟烯烃单体和用2)式:CH2=CHR1[在式中,R1表示-OR2或-CH2OR2(这里,R2为具有羟基的烷基)]代表的用作含交联基团单体的含羟基单体作为单体成分,和如果需要时,还包含至少一种选自以下的单体:用3)式:CH2=CR(CH3)[在式中,R表示具有1-8个碳原子的烷基]表示的β-甲基-取代的α-烯烃单体、用4)式:CHR3=CHOR3(CH3)[在式中,R3表示具有1-8个碳原子的烷基]表示的乙烯基醚、5)式:CH2=CHR3[在式中,R3为-OR4或-CH2OR4(在式中,R4表示具有羧基的烷基)]表示的单体或没有交联官能团并可与单体1)、2)、3)、4)和5)中任何一种共聚的其它单体6).更优选地,共聚物包含所有单体1)-6)。
对于氟烯烃单体,其例子包括四氟乙烯、三氟乙烯和六氟乙烯。优选地,使用三氟乙烯,更优选地,使用用上式1)表示的X为氯原子的三氟乙烯.这种材料提供了高的粘结强度.对于β-甲基-取代的α-烯烃单体,其例子包括异丁烯、2-甲基-1-戊烯和2-甲基-1-己烯.对于可与氟烯烃单体、β-甲基-取代的α-烯烃单体和含羟基的单体共聚的其它单体,其例子包括:羧酸,如醋酸乙烯酯、丙酸乙烯酯、(异)丁酸乙烯酯、己酸乙烯酯、月桂酸乙烯酯、硬脂酸乙烯酯、苯甲酸乙烯酯、六氟丙酸乙烯酯和三氟乙酸乙烯酯;乙烯基酯;马来酸或富马酸的二酯,如马来酸或富马酸的二甲酯、二乙酯、二丙酯、二丁酯、二三氟甲酯、二三氟甲酯和二六氟丙酯;烷基乙烯基醚,如甲基乙烯基醚、乙基乙烯基醚、正丙基乙烯基醚、异丁基乙烯基醚和叔丁基乙烯基醚;环烷基乙烯基醚,如环戊基乙烯基醚和环己基乙烯基醚;具有芳香基团的乙烯基醚,如苄基乙烯基醚;或氟代烷基乙烯基醚,如全氟乙基乙烯基醚和全氟丙基乙烯基醚;而且除了这些外,可使用巴豆酸、醋酸乙烯酯、马来酸、苯乙烯等。
要在本发明中使用的含氟共聚物包含用1)式和2)式代表的单体作为基本成分,通过在需要时向其中加入至少一种选自单体3)-6)中的单体以便通过常规已知的方法共聚得到,已知方法如乳液聚合法、溶液聚合法和悬浮液聚合法.设计含氟共聚物使通过GPC测量的数均分子量在1000-500000的范围内,优选为3000-100000.
对于要在本发明中使用的固化剂,可使用能与交联基团反应形成交联键的那些化合物.对于用于含羟基的单体的固化剂,可使用包含异氰酸酯基或羧基的那些化合物,优选使用具有异氰酸酯基的有机多异氰酸酯化合物。有机多异氰酸酯化合物的例子包括:2,4-甲苯二异氰酸酯、二苯基甲烷-4,4’-二异氰酸酯、亚二甲苯基二异氰酸酯、异佛尔酮二异氰酸酯、赖氨酸甲酯二异氰酸酯、甲基环己基二异氰酸酯、三甲基六亚甲基二异氰酸酯、六亚甲基二异氰酸酯和正-戊烷-1,4-二异氰酸酯、和它们的三聚物,还可使用它们的加合物或滴定化合物或具有两个或多个异氰酸酯基的这些聚合物或形成嵌段的异氰酸酯.优选地,可使用异佛尔酮二异氰酸酯或六亚甲基二异氰酸酯的三聚物.这是因为这些物质具有与含氟聚合物的良好相容性,提供了适宜的固化速度,并且耐溶剂性和耐化学性优良.对于用于含环氧基的单体的固化剂,其例子包括:具有羟基、羧基、酰胺基、氨基或异氰酸酯基的化合物.对于用于含羧基的单体的固化剂,其例子包括:具有羟基、氨基、异氰酸酯基或环氧基的化合物.对于用于含酰胺基的单体的固化剂,其例子包括具有环氧基的化合物。对于用于含氨基的单体的固化剂,其例子包括具有羧基、环氧基或异氰酸酯基的化合物.对于用于含水解甲硅烷基的单体的固化剂,其例子包括具有氨基或异氰酸酯基的化合物.
对于具有羟基的上述化合物,其例子包括1,4-双-2’-羟基乙氧基苯和对苯二酸双羟基乙酯.对于具有羧基的化合物,其例子包括脂肪族二元酸,如富马酸、琥珀酸、己二酸和壬二酸,和酸酐,如邻苯二甲酸酐。对于具有环氧基的化合物,其例子包括对苯二甲酸二缩水甘油酯和安息香酸二缩水甘油酯(paraoxy benzoic acid diglycidyl ester).
下面的描述将通过用包含羟基的含氟共聚物作为例子来说明本发明中使用的氟树脂层的制备方法.将包含羟基的含氟共聚物和固化剂溶解到已混合乙酸酯、酮、醚、芳香烃等中的一种或两种或多种的溶剂中,从而固化剂被加入到含氟共聚物中以便在0.1-5.0当量的范围内,优选为0.5-1.5当量,相对于含氟共聚物中的1当量羟基(-OH基),通过使用常规已知的涂覆方法如辊涂法、凹板式涂覆法和棒涂法将得到的溶液施加到已经过易粘结处理的金属粘合烯烃树脂层的面上,在其上干燥;这样,就形成了氟树脂层.适当地设定氟树脂层的涂层数量,使得干燥过程后的涂层数量成为3.0-5.0g/m2.这样做的原因解释如下:为了保持层压强度,需要3.0g/m2或以上的涂层数量,从防止端面湿气侵入和成本的角度看,涂层数量优选设定为5.0g/m2或以下.氟树脂层的厚度被设为2-6μm,优选3-5μm。
下面的描述将讨论热粘结树脂层.对于热粘结树脂层,将根据热粘结和密封这些元件时是否在热粘结树脂层和金属端子之间插入金属端子部分密封粘合薄膜来不同地确定树脂种类,金属端子分别连接到锂电池主体的正极和负极,并伸到外面.在中间插入金属-端子部分密封粘合薄膜的情况下,在需要时适当地选择并使用由简单物质或烯键式树脂的混合物制成的薄膜,烯键式树脂如低密度聚乙烯、中密度聚乙烯、高密度聚乙烯、线性低密度聚乙烯和乙烯-丁烯共聚物,和丙烯树脂,如均聚丙烯、乙烯-丙烯共聚物和乙烯-丙烯-丁烯共聚物,在不插入金属-端子-部分密封粘合薄膜的情况下,可使用由与金属粘合烯烃树脂层相同种类的树脂制成的薄膜.对于热粘合树脂层的厚度,设为5-20μm,优选10-15μm,小于5μm的厚度不能提供足够的层压强度,而超过20μm的厚度往往引起端面湿气渗透增加,导致电池性能下降.可通过常规已知的干法层压方法层压中间插入氟树脂层的金属粘合烯烃树脂层和热粘结树脂层.
尽管图中未示出,但可通过已知的干法层压方法使用已知的干法层压粘合剂如聚酯试剂、聚醚试剂和聚氨酯试剂形成基底层和铝箔的层压层。在层状产品被施加到模制型薄膜上时(见图3),上述化学转化层4优选形成在层压基底层2的一侧上的铝箔表面上.作出这种布置以便防止压模时铝箔3和外层2之间的分层,在袋型情况下(见图2),没有必要要求形成这种结构.在层压产品被施加到模制型薄膜上时(见图3),在防止压模时层状产品部分粘着到金属模具上并因此制备没有偏向厚度(厚度偏离)的均匀压模产品的尝试中(也就是提高压模时成型性的尝试),例如,可通过已知的涂覆方法如凹板式涂覆法、辊涂法或在形成图案形状层时的凹版印刷方法来施加润滑剂在基底层2的表面上形成润滑剂层,润滑剂如烃材料类流体石蜡、脂肪酸材料类硬脂酸和芥酸、脂肪酸酰胺材料类硬脂酰胺和芥酸酰胺、金属皂、天然蜡和硅酮,它们被溶解到合适的溶剂中并形成到可涂状态.
在连续层压基底层/铝箔/化学转化层/金属粘合烯烃树脂层/氟树脂层/热粘结树脂层的层压过程后,在高于用作金属粘合烯烃树脂层的树脂的软化点的温度下对层状产品进行热处理,优选在高于其熔点的温度下,从而可提高化学转化层和金属粘合烯烃树脂层之间的层间粘合强度;因此,变得可以提供耐化学性、耐热性和耐溶剂性优良并长时间保持稳定性能的薄膜.
[实施例]
下面的描述将借助实施例详细地讨论本发明.
[由二层组成的基底层的制备]
层压厚度为9μm的双轴向拉伸PET薄膜和厚度为15μm的双轴向拉伸ON薄膜,中间插入双组分可固化聚氨酯-粘结剂,制备由两个层[双轴向拉伸PET薄膜9μm/双轴向拉伸ON薄膜15μm]组成的基底层。
[第一中间层状产品的制备]
通过使用包含胺化酚醛聚合物、三价铬化合物和磷化合物的化学转化溶液预先处理铝箔(厚度为100μm),从而在其两个面上形成化学转化层,将厚度为12μm的双轴向拉伸PEN薄膜层压到箔的一个面上,在其间插入双组分可固化聚氨酯-粘结剂,制备第一中间层状产品[双轴向拉伸PEN薄膜12μm/化学转化层/铝箔100μm/化学转化层].
[第二中间层状产品的制备]
通过使用包含胺化酚醛聚合物、三价铬化合物和磷化合物的化学转化溶液预先处理铝箔(厚度为100μm),从而在其两个面上形成化学转化层,将由两个层组成的基底层的ON面层压到箔的一个面上,在其间插入双组分可固化聚氨酯-粘结剂,制备第二中间层状产品[双轴向拉伸PEN薄膜9μm/双轴向拉伸ON薄膜15μm/化学转化层/铝箔100μm/化学转化层].
[第三中间层状产品的制备]
通过使用包含胺化酚醛聚合物、三价铬化合物和磷化合物的化学转化溶液预先处理铝箔(厚度为80μm),从而在其两个面上形成化学转化层,将由两个层组成的基底层的ON面层压到箔的一个面上,在其间插入双组分可固化聚氨酯-粘结剂,制备第三中间层状产品[双轴向拉伸PEN薄膜9μm/双轴向拉伸ON薄膜15μm/化学转化层/铝箔80μm/化学转化层].
[第四中间层状产品的制备]
通过使用包含胺化酚醛聚合物、三价铬化合物和磷化合物的化学转化溶液预先处理铝箔(厚度为40μm),从而在其两个面上形成化学转化层,将由两个层组成的基底层的ON面层压到箔的一个面上,在其间插入双组分可固化聚氨酯-粘结剂,制备第四中间层状产品[双轴向拉伸PEN薄膜9μm/双轴向拉伸ON薄膜15μm/化学转化层/铝箔40μm/化学转化层]。
[第五中间层状产品的制备]
通过使用包含胺化酚醛聚合物、三价铬化合物和磷化合物的化学转化溶液预先处理铝箔(厚度为40μm),从而在其两个面上形成化学转化层,将厚度为25μm的双轴向拉伸ON薄膜层压到箔的一个面上,在其间插入双组分可固化聚氨酯-粘结剂,制备第五中间层状产品[双轴向拉伸ON薄膜25μm/化学转化层/铝箔40μm/化学转化层]。
在下面的实施例1-6中,使用含氟烯烃羟基的乙烯基醚共聚物作为含氟共聚物,使用作为异氰酸酯固化剂的六亚甲基二异氰酸酯的三聚物作为固化剂,除非另外限定.
实施例1
将已通过不饱和羧酸接枝改性的聚丙烯(下文中称为PPa)加热并通过T型模挤出机熔融挤出到第一中间层状产品的化学转化表面上,以便具有15μm的厚度,对PPa面进行电晕放电处理,并向得到的经过电晕放电处理的PPa面上施加氟树脂溶液,其中异氰酸酯固化剂被加入到含氟共聚物中,以便相对于在其上要被干燥的多元醇的1当量羟基(-OH基)为1.1当量,形成3.0g/m2的干重,进一步加热厚度为30μm的未拉伸聚丙烯薄膜(下文中称为CPP薄膜)并加压粘结到氟树脂层的表面上制备本发明的层状产品[双轴向拉伸PEN薄膜12μm/化学转化层/铝箔100μm/化学转化层/PPa 15μm/氟树脂层3.0g/m2/CPP薄膜30μm].
实施例2
将已通过不饱和羧酸接枝改性的聚乙烯(下文中称为PEa)加热并通过T型模挤出机熔融挤出到第二中间层状产品的化学转化表面上,以便具有12μm的厚度,对PEa面进行电晕放电处理,并向得到的经过电晕放电处理的PEa面上施加氟树脂溶液,其中异氰酸酯固化剂被加入到含氟共聚物中,以便相对于在其上要被干燥的多元醇的1当量羟基(-OH基)为1.1当量,形成3.0g/m2的干重,进一步加热厚度为30μm的CPP薄膜并加压粘结到氟树脂层的表面上制备本发明的层状产品[双轴向拉伸PET薄膜9μm/双轴向拉伸ON薄膜15μm/化学转化层/铝箔100μm/化学转化层/PEa 15μm/氟树脂层3.0g/m2/CPP薄膜30μm]。
实施例3
加热PEa并通过T型模挤出机熔融挤出到第三中间层状产品的化学转化表面上,以便具有12μm的厚度,然后对PEa面进行电晕放电处理,并向得到的经过电晕放电处理的PEa面上施加氟树脂溶液,其中异氰酸酯固化剂被加入到含氟共聚物中,以便相对于在其上要被干燥的多元醇的1当量羟基(-OH基)为1.1当量,形成3.0g/m2的干重,进一步加热厚度为30μm的未拉伸聚乙烯薄膜(下文中称为PE薄膜)并加压粘结到氟树脂层的表面上制备本发明的层状产品[双轴向拉伸PET薄膜9μm/双轴向拉伸ON薄膜15μm/化学转化层/铝箔80μm/化学转化层/PEa 15μm/氟树脂层3.0g/m2/PE薄膜30μm].
实施例4
加热PPa并通过T型模挤出机熔融挤出到第三中间层状产品的化学转化表面上,以便具有12μm的厚度,然后对PPa面进行电晕放电处理,并向得到的经过电晕放电处理的PPa面上施加氟树脂溶液,其中异氰酸酯固化剂被加入到含氟共聚物中,以便相对于在其上要被干燥的多元醇的1当量羟基(-OH基)为1.1当量,形成3.0g/m2的干重,进一步加热厚度为30μm的PE薄膜并加压粘结到氟树脂层的表面上制备本发明的层状产品[双轴向拉伸PET薄膜9μm/双轴向拉伸ON薄膜15μm/化学转化层/铝箔80μm/化学转化层/PPa 12μm/氟树脂层3.0g/m2/PE薄膜30μm].
实施例5
通过热层压方法在第四中间层状产品的化学转化面上层压厚度30μm的PPa薄膜,然后对PPa面进行电晕放电处理,并向得到的经过电晕放电处理的PPa面上施加氟树脂溶液,其中异氰酸酯固化剂被加入到含氟共聚物中,以便相对于在其上要被干燥的多元醇的1当量羟基(-OH基)为1.1当量,形成3.0g/m2的干重,进一步加热厚度为30μm的CPP薄膜并加压粘结到氟树脂层的表面上制备本发明的层状产品[双轴向拉伸PET薄膜9μm/双轴向拉伸ON薄膜15μm/化学转化层/铝箔40μm/化学转化层/PPa薄膜30μm/氟树脂层3.0g/m2/CPP薄膜30μm]。
实施例6
通过热层压方法在第四中间层状产品的化学转化面上层压厚度30μm的PEa薄膜,然后对PEa面进行电晕放电处理,并向得到的经过电晕放电处理的PPa面上施加氟树脂溶液,其中异氰酸酯固化剂被加入到含氟共聚物中,以便相对于在其上要被干燥的多元醇的1当量羟基(-OH基)为1.1当量,形成3.0g/m2的干重,进一步加热厚度为30μm的CPP薄膜并加压粘结到氟树脂层的表面上制备本发明的层状产品[双轴向拉伸PET薄膜9μm/双轴向拉伸ON薄膜15μm/化学转化层/铝箔40μm/化学转化层/PEa薄膜30μm/氟树脂层3.0g/m2/CPP薄膜30μm]。
对比实施例1
将双组分可固化聚氨酯粘结剂施加到第五中间层状产品的化学转化面上,在其上干燥至具有3.0g/m2的干重,加热厚度为30μm的CPP薄膜并加压粘结到粘结剂层的表面上制备对比实施例的层状产品[双轴向拉伸ON薄膜25μm/化学转化层/铝箔40μm/化学转化层/粘结剂层3.0g/m2/CPP薄膜30μm].
对比实施例2
加热并通过T型模挤出机熔融挤出PPa到第五中间层状产品的化学转化面上,以便形成15μm的厚度,并通过夹心层压方法在这上面形成厚度30μm的CPP薄膜,制备对比实施例的层状产品[双轴向拉伸ON薄膜25μm/化学转化层/铝箔40μm/化学转化层/PPa 15μm/CPP薄膜30μm].
对比实施例3
加热并通过T型模挤出机熔融挤出PEa到第五中间层状产品的化学转化面上,以便形成15μm的厚度,并通过夹心层压方法在这上面形成厚度30μm的PE薄膜,制备对比实施例的层状产品[双轴向拉伸ON薄膜25μm/化学转化层/铝箔40μm/化学转化层/PEa 15μm/PEa薄膜30μm]。
通过使用下面的评价方法评价上述实施例1-6和对比实施例1-3中形成的层状产品的耐电解质溶液性、抗破裂性能、抗短路性能、透湿性、体积电阻率和成型性,评价结果共同显示在表1中。
表1
耐电解质溶液性 | 抗破裂性能 | 抗短路性能 | 透湿性 | 成型性 | |
实施例1 | 没有剥离 | ○ | 10秒 | 30ppm | 6mm |
实施例2 | 没有剥离 | ○ | 20秒 | 40ppm | 10mm |
实施例3 | 没有剥离 | ○ | 15秒 | 30ppm | 10mm |
实施例4 | 没有剥离 | ○ | 15秒 | 30ppm | 10mm |
实施例5 | 没有剥离 | ○ | 20秒 | 40ppm | 6mm |
实施例6 | 没有剥离 | ○ | 20秒 | 40ppm | 6mm |
对比实施例1 | 剥离 | ×(3V) | 3秒 | 300ppm | 6mm |
对比实施例2 | 没有剥离 | ×(3V) | 3秒 | 30ppm | 6mm |
对比实施例3 | 没有剥离 | ×(3V) | 3秒 | 30ppm | 6mm |
[评价方法]
(耐电解质溶液性评价方法)
用层状产品形成内部尺寸为30×50mm和热密封宽度为7mm的三路密封袋,并装满3g电解质溶液[其中六氟磷酸盐被溶解在混合溶液[碳酸亚乙酯/碳酸二乙酯/碳酸二甲酯=1/1/1(容量比)]中形成1mol/升六氟磷酸盐溶液],在85℃的恒温器中存放2200小时后,将其打开,目测观察层内侧与铝箔的任何剥离.
(抗破裂性能的评价方法)
将层状产品切成具有每个边100mm的方形形状的试验样品.通过使用具有33×55mm的矩形形状的阳模和与阳模间隙为0.5mm的阴模,将每个条状块放在阴模上以便使热粘结树脂层侧面位于阳模侧面上,用0.1MPa的压力(面压力)挤压条状块,从而形成10个样品,每一个都为深度为3mm的模制产品.将具有每个边为100mm的方形形状的试验样品放在模制产品上面,使得面向热粘结树脂层.然后,通过用7mm宽的金属对金属基加热板制成的热密封机热密封一端边(密封条件:190℃;1.0MPa;3秒),形成热粘结部分,即刻以10N/100mm宽度将这种热粘结部分彼此分开180度,然后按相同的方式热密封与热粘结部分正交的方向上的部分,从而形成一个一边可被打开的模制体。倒入电解质溶液[其中六氟磷酸盐被溶解在混合溶液[碳酸亚乙酯/碳酸二乙酯/碳酸二甲酯=1/1/1(容量比)]中形成1mol/升六氟磷酸盐溶液],从而将分开180度的模制体的热粘结部分浸没在其中。施加电压在1-100V之间变化,测量水解质溶液和层状产品铝箔之间的电阻。即使在100V的施加电压下,10MΩ或以上的电阻被评价为良好,并用○指示.当即使10个模制产品中的一个具有0.1MΩ或以下的电阻时,这些样品被评价为差,并用×指示.用×指示的那些样品与0.1MΩ或以下的施加电压值显示在一起.
(抗短路性能的评价方法)
将层状产品切成具有每个边60mm的方形形状的样品。放置层状产品,层状产品的密封剂薄膜面彼此面对面排列,将宽度4mm、长度55mm和厚度70μm的镍端子插入在层状产品之间,试验仪的端子连接到镍端子和层状产品的铝箔上.在这种状态下,在与镍端子长度方向正交的方向上在上和下两个面上用7mm宽的金属对金属基加热板制成的热密封机热密封这些(密封条件:190℃;1.0MPa).测量镍箔和层状产品的铝箔之间直到短路时的时间(单位:秒)并进行评价.
(透湿性的评价方法)
将层状产品切成尺寸为120×120mm的方形形状块.在MD方向上将每个块折叠成两半,密封一个短边10mm宽度,同时密封长边3mm宽度,从而形成另外一个短边可被打开的袋。在真空烘箱中干燥袋后,在干燥房间中将3g混合溶液[碳酸亚乙酯/碳酸二乙酯/碳酸二甲酯=1/1/1(体积比)注入到袋内,从而形成开口部分密封10mm宽度的透湿性评价样品。将透湿性评价样品存放在60℃和90%RH的热-恒湿器中7天,通过使用Karl Fischer方法测量样品内部湿气的增加量.短边上的热密封条件是190℃、2.0MPa和3.0秒,长边上的条件为190℃、1.0MPa和3.0秒。
(成型性评价方法)
将层状产品切成尺寸为100×80mm的条状块。通过使用具有33×55mm的矩形形状的阳模和与阳模间隙为0.5mm的阴模,将每个条状块放在阴模上以便使热粘结树脂层侧面位于阳模侧面上,用0.1MPa的压力(面压力)挤压条状块,从而冷模制10个样品,模具深度从0.5mm的模具深度以0.5mm单位变化.10个样品在封装材料中没有起皱或在铝箔中没有针孔和裂纹时的模具深度被定义为限制模具深度。模具深度被显示为评价值。
如表1清楚地所示,与对比实施例1-3相比,实施例1-6的层状产品获得良好效果,尤其是抗破裂性能和抗短路性能.实施例1-6的层状产品还在透湿性(水蒸汽不透性)、耐电解质溶液性和成型性方面获得良好效果.当通过挤出涂覆方法形成金属粘合烯烃树脂层以及通过干法层压方法形成氟树脂层和热粘结树脂层时,实施例1-4的层状产品还生产率良好.
Claims (7)
1.一种层状产品,包括:
被连续层压的至少基底层、铝箔、化学转化层、对金属具有粘合性的烯烃树脂层和热粘结树脂层,
其中在烯烃树脂层和热粘结树脂层之间插入通过具有交联基团的含氟共聚物和与交联基团反应的固化剂形成的氟树脂层,
所述交联基团选自羟基、环氧基、羧基、酰胺基、氨基或水解甲硅烷基。
2.根据权利要求1的层状产品,其中烯烃树脂层为酸改性聚烯烃树脂。
3.根据权利要求1的层状产品,其中热粘结树脂层为聚烯烃树脂或酸改性聚烯烃树脂。
4.根据权利要求1的层状产品,其中含氟共聚物至少包含氟烯烃单体和含羟基单体作为单体成分。
5.根据权利要求1的层状产品,其中固化剂为有机多异氰酸酯化合物。
6.根据权利要求1的层状产品,其中通过包含胺化酚醛聚合物、三价铬化合物和磷化合物的化学转化溶液形成化学转化层。
7.一种二次电池,其中电池容器用多个引线密封,引线分别连接到电池主体的正极和负极上,并伸出电池容器外,
电池容器由层状产品制成,其中通过连续层压至少基底层、铝箔、化学转化层、对金属具有粘合性的烯烃树脂层和热粘结树脂层形成层状产品,和
通过具有交联基团的含氟共聚物和与交联基团反应的固化剂形成的氟树脂层插入在烯烃树脂层和热粘结树脂层之间,
所述交联基团选自羟基、环氧基、羧基、酰胺基、氨基或水解甲硅烷基。
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