CN101536221A - 共挤出的多层电池隔板 - Google Patents

共挤出的多层电池隔板 Download PDF

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Publication number
CN101536221A
CN101536221A CNA2007800424064A CN200780042406A CN101536221A CN 101536221 A CN101536221 A CN 101536221A CN A2007800424064 A CNA2007800424064 A CN A2007800424064A CN 200780042406 A CN200780042406 A CN 200780042406A CN 101536221 A CN101536221 A CN 101536221A
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China
Prior art keywords
polymer
battery separator
film
improve
separator according
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CNA2007800424064A
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English (en)
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CN101536221B (zh
Inventor
罗纳德·W·考尔
威廉·C·小富尔克
石烈
张晓民
科虎·V·恩谷因
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Celgard LLC
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Celgard LLC
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    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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Abstract

一种电池隔板，包括共挤出的微孔膜，所述共挤出的微孔膜具有至少两个由可挤出的聚合物制成的层，并且具有：由＜0.80微米(μm)的标准偏差限定的均匀厚度；或由＞60克的剥离强度限定的层间粘附力。

Description

共挤出的多层电池隔板
发明领域
本文中公开的电池隔板是一种共挤出的多层电池隔板。这种隔板的一个实施方案可用于锂离子电池。
发明背景
多层电池隔板公开在例如美国专利No.4650730；No.5240655；No.5281491；No.5691047；No.5691077；No.5952120；No.6080507；No.6878226；和美国专利公报No.20020136945中。
虽然前述的若干参考文献中提到，可以通过共挤出工艺制备多层隔板，但在商业实践中，共挤出工艺在商业上一直难以实施。特别是，以往共挤出试验的产品伴随着均匀性方面的问题，这种问题限制了由此工艺制备的产品的商业化。据信，这些问题的产生是由于与通过狭孔模具同时挤出至少两种相异聚合物相关的复杂性所致。因此，现有技术中生产共挤出多层电池隔板的尝试得到的是非均匀的产品。如此，没有可供商品化的共挤出多层电池隔板。
因此，需要获得具有均匀物理特性的共挤出多层电池隔板。
发明内容
一种电池隔板，其包括共挤出的微孔膜，所述共挤出的微孔膜具有至少两个由可挤出的聚合物制成的层，并且具有：由<0.80微米(μm)的标准偏差限定的均匀厚度；或由>60克的剥离强度限定的层间粘附力。
发明说明
将就在二次锂离子电池(例如，在手机、笔记本电脑、以及需要轻型储电装置的其他设备中使用的那些)中的应用，对本发明的电池隔板进行描述。然而，应该理解的是，本发明并不因此而受到限制，本发明的电池隔板可用于其他的电池系统(例如，仅举几例如NiMH、NiCd、碱性、一次锂电池)。
一般来说，用于锂离子电池的电池隔板是具有如下典型物理特性的微孔膜：厚度--小于5密耳(125μm)、或小于2密耳(50μm)、或小于1密耳(25μm)，实际下限为约1/3密耳(8μm)；穿刺强度--大于400克或大于550克；平均孔径--0.005～10.000μm、或0.01～5.00μm、或0.05～2.00μm；格利(Gurley)值(ASTM-D726(B))--5～100秒或10～60秒。
本发明的电池隔板是共挤出的多层电池隔板。“共挤出”指的是这样的一种过程，其中使多种聚合物同时聚集在挤压模中，并以这样的一种形式从模中脱出，这里，该形式总体平面结构，具有至少两个分立层，它们在分立层的界面上通过例如形成分立层之界面的聚合物的混合而结合在一起。挤压模可以是平板(或狭缝)模，或者是吹膜(或环形)模。以下将更加详细地描述共挤出过程。“多层”是指，隔板具有至少两个层。“多层”还可以是指，具有3、4、5、6、7、或更多层的结构。每层由进入挤压模内的单独的聚合物原料流形成。各层可以具有不同的厚度。多数情况下，至少两个原料流为相异的聚合物。“相异的聚合物”是指：具有相异化学性质的聚合物(例如，PE与PP，或者PE与PE的共聚物是具有相异化学性质的聚合物)；和/或化学性质相同但特性相异的聚合物(例如，具有不同特性(如，密度、分子量、分子量分布、流变性、添加剂(成分和/或百分比)，等)的两种PE)。然而，聚合物可以相同或完全一致。
可用于本发明电池隔板中的聚合物是可挤出的那些。这种聚合物通常被称为热塑性聚合物。典型的热塑性聚合物包括但不限于：聚烯烃、聚缩醛(或聚氧甲烯)、聚酰胺、聚酯、多硫化物、聚乙烯醇、聚乙烯酯、和聚乙二烯(polyvinylidene)。聚烯烃包括但不限于：聚乙烯(包括例如LDPE、LLDPE、HDPE、UHDPE)、聚丙烯、聚丁烯、聚甲基戊烯、其共聚物、及其共混物。聚酰胺(尼龙)包括但不限于：聚酰胺6、聚酰胺66、尼龙10，10、聚邻苯二甲酰胺(PPA)、其共聚物、及其共混物。聚酯包括但不限于：聚对苯二甲酸乙二酯、聚对苯二甲酸丁二酯、其共聚物、及其共混物。多硫化物包括但不限于：聚苯硫醚、其共聚物、及其共混物。聚乙烯醇包括但不限于：乙烯-乙烯醇、其共聚物、及其共混物。聚乙烯酯包括但不限于：聚醋酸乙烯酯、乙烯-醋酸乙烯酯、其共聚物、及其共混物。聚乙二烯包括但不限于：氟化的聚乙二烯(如聚偏二氯乙烯、聚偏二氟乙烯)、其共聚物、及其共混物。
可以将各种材料添加到聚合物中。添加这些材料用以调节或提高单个层或整体隔板的性能或特性。这种材料包括但不限于：
可以添加降低聚合物熔融温度的材料。一般来说，多层隔板包括设计用于在达到预定温度时关闭其孔隙以阻止离子在电池的电极之间流动的层。这项功能通常被称为“封闭”。在一个实施方案中，三层隔板具有中间封闭层。为了降低该层的封闭温度，可以向聚合物中添加熔融温度低于与之混合的聚合物之熔融温度的材料。这种材料包括但不限于：熔融温度低于125℃的材料，例如，聚烯烃或聚烯烃低聚物。这种材料包括但不限于：聚烯烃蜡(聚乙烯蜡、聚丙烯蜡、聚丁烯蜡、以及它们的共混物)。可以按聚合物之5-50重量％的比率将这些材料装填到聚合物之中。在一个实施方案中，可以达到140℃以下的封闭温度。在另外的实施方案中，可以达到130℃以下的封闭温度。
可以添加改善膜之熔体完整性的材料。“熔体完整性”是指，膜在高温下限制其物理尺寸的损失或恶化，从而使电极保持物理上被隔离的能力。这种材料包括矿物填料。矿物填料包括但不限于：滑石、高岭土、合成二氧化硅、硅藻土、云母、纳米粘土、氮化硼、二氧化硅、二氧化钛、硫酸钡、碳酸钙、氢氧化铝、氢氧化镁等，以及它们的共混物。这种材料可以还包括但不限于细纤维。“细纤维”包括玻璃纤维和短切聚合物纤维。装填比率范围是层之聚合物的1-60重量％。这种材料可以还包括高熔点或高粘度的有机材料，如PTFE(聚四氟乙烯)和UHMWPE(超高分子量聚乙烯)。这种材料可以还包括交联剂或偶联剂。
可以添加用以提高膜强度或韧度的材料。这种材料包括弹性体。“弹性体”包括但不限于：乙烯-丙烯(EPR)、乙烯-丙烯-二烯(EPDM)、苯乙烯-丁二烯(SBR)、苯乙烯-异戊二烯(SIR)、亚乙基降冰片烯(ENB)、环氧树脂、和聚氨酯以及它们的共混物。这种材料可以还包括但不限于细纤维。“细纤维”包括玻璃纤维和短切聚合物纤维。装填比率范围是层之聚合物的2-30重量％。这种材料可以还包括交联剂或偶联剂、或者高粘度材料、或高熔点材料。
可以添加用以改善膜之抗静电性能的材料。这种材料包括例如抗静电剂。“抗静电剂”包括但不限于单硬脂酸甘油酯、乙氧基化的胺、聚醚(例如，可商购自日本三洋化工株式会社的Pelestat 300)。装填比率范围是层之聚合物的0.001-10重量％。
可以添加用以改善隔板表面润湿性的材料。这种材料包括例如润湿剂。“润湿剂”包括但不限于乙氧基化的醇、伯聚羧酸(primarypolymeric carboxylic acides)、二醇(如聚丙二醇和聚乙二醇)、用马来酐官能化的聚烯烃、丙烯酸、甲基丙烯酸缩水甘油酯。装填比率范围是层之聚合物的0.01-10重量％。
可以添加用以改善隔板表面摩擦学性能的材料。这种材料包括润滑剂。”润滑剂”包括例如含氟聚合物(如聚偏二氟乙烯、聚四氟乙烯、低分子量含氟聚合物)、光滑剂(如油酸酰胺、硬脂酸酰胺、芥酸酰胺、
Figure A200780042406D0007092854QIETU
、硬脂酸钙、硅树脂)。装填比率范围是层之聚合物的0.001-10重量％。
可以添加用以改善聚合物加工性的材料。这种材料包括例如含氟聚合物、氮化硼、聚烯烃蜡。装填比率范围是层之聚合物的100ppm至10重量％。
可以添加用以改善膜之阻燃性质的材料。这种材料包括例如溴化的阻燃剂、磷酸铵、氢氧化铵、三水合氧化铝、和磷酸酯。
可以添加用以促进聚合物成核的材料。这种材料包括成核剂。“成核剂”包括但不限于苯甲酸钠、二亚苄基山梨醇(DBS)、及其化学衍生物。装填比率是常规的。
可以添加用以使层着色的材料。这种材料是常规的。
在制造本发明的电池隔板过程中，共挤出聚合物，以形成多层的非多孔前体，然后，处理该前体，以形成微孔。可以采用“湿”法或“干”法形成微孔。湿法(也称：溶剂萃取、相转化、热致相分离(TIPS)、或凝胶萃取)通常涉及：在形成前体之前添加可消除的材料，随后例如通过萃取法消除该材料，以形成孔。干法(也称为Celgard法)通常涉及：挤出前体(不包括任何用于形成孔的可消除的材料)；使前体退火，以及拉伸前体，以形成微孔。以下针对干法讨论本发明。
为了使本发明的共挤出多层电池隔板具有均匀的尺寸特性，使用具有特定剪切速率的挤压模。经确定，在每层18-100磅/小时(8.2-45.4千克/小时)流量下的模剪切速率必须为最低4/秒。在一个实施方案中，在每层18-100磅/小时(8.2-45.4千克/小时)流量下的剪切速率≥8/秒。所有其它参数均是常规上已知的。
实施例
由以下的实施例进一步阐述上述的发明。表1所示为根据本发明的上述讨论制备的11个样品。表2例示使用各种材料以改善隔板熔体完整性，至没有这些材料之隔板。表3例示使用其他的上述材料以改善隔板的各种特性。用于汇总表中资料的测试程序如下所述。
测试程序
格利(Gurley)值：由两种方法测定格利值。在定义为日本工业标准格利值(JIS格利值)的第一种方法中，使用OHKEN透过率测试仪测定格利值。JIS格利值的定义为，在4.8英寸H2O柱的恒定压力下，100cc的空气通过一平方英寸的膜所需的时间，以秒表示。在第二种方法中，按照ASTM D-726的程序测定格利值，格利值的定义为，在4.8英寸H2O柱的恒定压力下，10cc的空气通过一平方英寸的膜所需的时间，以秒表示。
拉伸性能：按照ASTM-882的程序，使用Instron 4201型设备测量MD和TD拉伸强度。
穿刺强度：使用Instron 4442型设备，基于ASTM D3763测量穿刺强度。穿刺强度的单位是牛顿。在拉伸产品的宽度上进行测量，平均穿刺能(穿刺强度)定义为，刺穿测试验样品所需的力。
剥离强度或粘附力：使用Chatillon TCD-200剥离力测试仪测试层内(intra-layer)粘附力。
收缩率：采用改进的ASTM D-2732-96程序，在90℃下测量60分钟的收缩率。
厚度：按照ASTM D374，使用Emveco Microgage 210-A精密测微计测定膜的厚度值。以微米(μm)为单位给出厚度值。取样品宽度上的20个单独的测微计读数之平均值。
孔隙度：按照ASTM D2873之方法测定微孔膜的孔隙度。
高温熔体完整性：采用热机械分析法(TMA)测量高温熔体完整性。在125gm恒定负荷的压迫下，使用TMA压迫探头测量隔板的厚度变化，以5℃/分钟的速率从25至300℃进行温度扫描。将250℃下保持的厚度百分比定义为高温熔体完整性。
润湿性：将一滴典型的锂离子电解液放在膜样品上。记录样品外观从不透明到几乎透明的变化。对于可湿性隔板来说，外观应几乎是均匀半透明的，没有不透明的区域。非可湿性样品则保持其不透明性。
ER(电阻)：电阻的单位是ohm-cm2。表征隔板电阻的方式是，从成品材料上切下小隔板片，然后，将它们放在两个阻塞电极之间。用电池电解液彻底地饱和隔板，所述电解液含有在体积比为3:7的EC/EMC溶剂中的1.0M LiPF6盐。通过4探针AC阻抗技术测量隔板的电阻R(Ω)。为了减少电极/隔板界面上的测量误差，需要通过增加更多的隔板层进行多重测量。然后，在多层测量的基础上，根据下式计算用电解液饱和之隔板的(离子)电阻Rs(Ω)，
R s = &rho; s l A - - - ( 1 )
其中，ρs是隔板的离子电阻率(Ω-cm)，A是电极面积(cm2)，l是隔板膜的厚度(cm)。比值ρs/A是计算隔板电阻(ΔR)随多隔板层(Δδ)之变化的斜率，由下式给出，
Figure A200780042406D00101
还可参见2006年4月7日提交的序列号为No.11/400,465的美国专利申请，涉及“离子电阻”的测试程序，其内容通过引用而被结合在本文中。
拔销(Pin Removal)：拔销测试模拟电池的卷绕过程。拔销力是卷绕之后从绕卷中心拔出销所需的力，以克表示。使用电池卷绕机将隔板卷绕在销(或者芯或心轴)的周围。销是二(2)构件式圆柱心轴，具有0.16英寸直径和平滑的外表面。每个构件具有半圆形截面。将下面讨论的隔板绕在销上。隔板上的(切向)初始力为0.5kgf，此后以每二十四(24)秒卷十(10)英寸的速度卷绕隔板。在卷绕过程中，张力辊接触着被卷绕在心轴上的隔板。张力辊包括位于隔板供料之对面的5/8＂直径的辊、(接触时)被施加1巴空气压力的3/4＂气缸、和使辊与筒互连的1/4＂杆。隔板由两(2)个30mm(宽)×10＂被测试的膜件组成。对五(5)个这种隔板进行测试，取结果的平均数，并报告平均值。以1＂的交叠将每件拼接到卷绕机的隔板供料辊上。在隔板的自由端，即拼接的末端处，用油墨做出1/2＂和7＂的标记，使1/2＂标记对齐销的远侧(即，与张力辊相邻的那一侧)，使隔板接合在销的构件之间，被接合好张力辊开始进行卷绕。当7＂标记离绕卷(卷绕在销上的隔板)约1/2＂时，在该标记处切下隔板，用一片胶带(1＂宽，1/2＂交叠)使隔板的自由端固定于绕卷上。从卷绕机上取下绕卷(即，隔板卷绕在其上的销)。可以接受的绕卷是不起皱和不伸缩的。将绕卷放置到带有重力传感器(501bs x 0.021b；Chatillon DFGS 50)的拉伸强度测试仪(即，北卡罗莱纳州格林斯博罗的Chatillon公司的Chatillon TCD 500-MS型)上。应变速率为每分钟2.5英寸，以每秒100点的速率记录来自重力传感器的数据。将峰值力报告为拔销力。还可以参见：美国专利No.6,692,867，其通过引用结合在本文中。
介质击穿：升高样品上的电压，直至观察到材料的介质击穿。“介电击”穿以伏特数表达。将隔板置于两个电极之间，在电极间施加电压。升高电压，直至观察到隔板的介质击穿。坚固的隔板显示出高破坏电压。任何非均匀性均可导致低破坏电压。
Aquapore孔径：使用可通过PMI(多孔材料公司)获得的Aquapore测量孔径。孔径以微米μm表示。
混合性穿透：“混合性穿透”是使隔板产生短路所需的力，以千克力kgf表示。混合性穿透是由于混合性穿透使隔板产生短路所需的力。在这项测试中，一开始使用第一金属板为底板，在该板的上面放置阴极材料片，在阴极的上面放置隔板，在隔板的上面放置阳极材料片。然后，提供连接至测力计的3mm球端头。球端头通过电阻表与第一金属板相连。对球端头施加压力，该压力记录于测力计上。一旦施加力之后，便会在隔板的每一侧上逐步形成阳极混合料和阴极混合料。当电阻急剧下降时，表明由于混合性穿透造成隔板的短路。混合性穿透衡量的是隔板的强度及其对混合性穿透的抵抗力。这被认为能更准确地模拟真实电池的行为。对于描述隔板在电池中的行为方式而言，这是比穿刺强度更好的指标。这项测试用来表明在电池组装期间隔板容许短路的倾向。还可参见2006年4月7日提交的序列号为No.11/400,465的美国专利申请，其内容通过引用被结合在本文中。
Figure A200780042406D00121
Figure A200780042406D00131
Figure A200780042406D00141
在不偏离本发明实质及其基本属性的情况下，可以按其它方式具体实施本发明，因此，应当参照所附的权利要求书而非上述的说明书来确定本发明的保护范围。

Claims (20)

1.一种电池隔板，其包括：
共挤出的微孔膜，所述共挤出的微孔膜具有至少两个由可挤出的聚合物制成的层，并且具有由<0.80μm的标准偏差限定的均匀厚度。
2.根据权利要求1所述的电池隔板，其中，所述标准偏差是在4-125μm厚度范围上的。
3.根据权利要求3所述的电池隔板，其中，所述标准偏差是4-50μm厚度范围上的。
4.根据权利要求1所述的电池隔板，其中，一个所述层的所述聚合物与所述其它层的所述聚合物是相同或不同的。
5.根据权利要求1所述的电池隔板，其中，一个所述可挤出的聚合物为热塑性聚合物。
6.根据权利要求1所述的电池隔板，其中，一个所述可挤出的聚合物选自：聚烯烃、聚缩醛、聚酰胺、聚酯、多硫化物、聚乙烯醇、聚乙烯酯、聚乙二烯、上述的共聚物、及其共混物。
7.根据权利要求1所述的电池隔板，其中，一个所述聚合物还包含向其中添加的材料。
8.根据权利要求7所述的电池隔板，其中，所述材料选自于适应以下方面的材料：降低聚合物的熔化温度；改善膜的熔体完整性；提高膜的韧性强度；改善膜的抗静电性能；改善隔板的表面润湿性；改善隔板的表面摩擦学性能；改善聚合物的加工性；提高膜的阻燃性；促进聚合物的成核；使膜层着色；及其组合。
9.一种电池隔板，其包括：
共挤出的微孔膜，所述共挤出的微孔膜具有至少两个由可挤出的聚合物制成的层，并且具有由>60克的剥离强度限定的层间粘附力。
10.根据权利要求9所述的电池隔板，其中，一个所述可挤出的聚合物为热塑性聚合物。
11.根据权利要求9所述的电池隔板，其中，一个所述层的所述聚合物与所述其它层的所述聚合物是相同或不同的。
12.根据权利要求9所述的电池隔板，其中，一个所述可挤出的聚合物选自：聚烯烃、聚缩醛、聚酰胺、聚酯、多硫化物、聚乙烯醇、聚乙烯酯、聚乙二烯、上述的共聚物、及其共混物。
13.根据权利要求9所述的电池隔板，其中，一个所述可挤出的聚合物还包含向其中添加的材料。
14.根据权利要求13所述的电池隔板，其中，所述材料选自于适应以下方面的材料：降低聚合物的熔化温度；改善膜的熔体完整性；提高膜的韧性强度；改善膜的抗静电性能；改善隔板的表面润湿性；改善隔板的表面摩擦学性能；改善聚合物的加工性；提高膜的阻燃性；促进聚合物的成核；使膜层着色；及其组合。
15.一种电池隔板，其包括：
多层微孔膜，所述多层微孔膜具有至少两个由聚合物制成的层，其中一个所述聚合物选自：聚甲基戊烯、聚缩醛、聚酯、聚酰胺、聚乙烯醇、聚乙烯酯、多硫化物、聚乙二烯。
16.根据权利要求15所述的电池隔板，其中，一个所述层的所述聚合物与所述其它层的所述聚合物是相同或不同的。
17.根据权利要求15所述的电池隔板，其中，所述膜是干拉伸膜。
18.一种制备微孔多层膜的方法，其包括步骤：
通过挤压模共挤出非多孔的多层前体，最低剪切速率为4秒-1，每层流量为18-100磅/小时(8.2-45.4千克/小时)；以及
处理该非多孔的多层前体，以得到微孔多层膜。
19.根据权利要求18所述的方法，其中，该剪切速率≥8/秒。
20.根据权利要求18所述的方法，其中，该处理还包括：
使非多孔的多层前体退火；以及
拉伸退火的该非多孔的多层前体。
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