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CN109360927A - 用于锂离子二次电池的多层混杂型电池隔板及其制造方法 - Google Patents

用于锂离子二次电池的多层混杂型电池隔板及其制造方法 Download PDF

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Publication number
CN109360927A
CN109360927A CN201811466451.9A CN201811466451A CN109360927A CN 109360927 A CN109360927 A CN 109360927A CN 201811466451 A CN201811466451 A CN 201811466451A CN 109360927 A CN109360927 A CN 109360927A
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China
Prior art keywords
partition
layer
film
battery
polypropylene
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CN201811466451.9A
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English (en)
Inventor
石烈
吉尔·V·沃森
罗纳德·W·考尔
罗尼·E·史密斯
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Celgard LLC
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Celgard LLC
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Publication of CN109360927A publication Critical patent/CN109360927A/zh
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    • H01L23/485—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of lead-in layers inseparably applied to the semiconductor body (electrodes) consisting of layered constructions comprising conductive layers and insulating layers, e.g. planar contacts
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  • Condensed Matter Physics & Semiconductors (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Materials Engineering (AREA)
  • Cell Separators (AREA)
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Abstract

一种用于锂二次电池的多层电池隔板，包括第一层干法的膜，其结合于第二层湿法的膜。第一层可由聚丙烯系树脂制成。第二层可由聚乙烯系树脂制成。隔板可具有不止两个层。隔板可具有约1.5‑3.0范围内的TD/MD拉伸强度之比。隔板可具有约35.0微米或更小的厚度。隔板可具有大于约630gf的刺穿强度。隔板可具有至少约2000V的介电击穿。

Description

用于锂离子二次电池的多层混杂型电池隔板及其制造方法
该申请是分案申请，优先权日是2013年3月15日，原国际申请日是2014年3月14日，母案进入中国国家阶段的日期是2015年9月14日；国际申请号是PCT/US2014/026983，母案的中国国家申请号是201480015019.1；原申请的发明名称是《用于锂离子二次电池的多层混杂型电池隔板及其制造方法》。
相关申请
本申请要求享有2013年3月15日提交的申请号为No.61/792,722的共同待决美国临时专利申请的权益，该临时专利申请的内容以引用的方式并入本文。
发明领域
本发明涉及多层电池隔板，特别是用在锂离子二次电池中的隔板。
发明背景
使用多层微孔膜作为用于锂离子二次电池的电池隔板是已知的，例如，参见专利US5,480,745、US5,691,047、US5,667,911、US5,691,077和US5,952,120，其每一者以引用的方式并入本文。这些专利公开了由一个或多个聚烯烃层组成的单层及多层膜，所述一个或多个聚烯烃层是采用通常被称为干法的无溶剂制造方法制成的。一种这样的公知干法为干法，其涉及使用共挤出模具或非共挤出模具形成薄膜型坯。这种薄膜型坯也被称为前体膜，并且具有无孔微结构。
干法多层隔板膜(如由北卡罗来纳州夏洛特的Celgard LLC制造的隔板)具有由孔径、孔隙率及扭曲度限定的独特的微结构，并且抑制枝晶生长且延长锂离子二次可再充电电池的循环寿命。参见图1。
也可通过湿法制造微孔隔板膜，如US4,588,633、US4,600,633、US4,620,955、US4,539,256、US5,922,492和US2009/0253032中描述的那些方法(其每一者以引用的方式并入本文)，它们公开了采用包括使用溶剂的制造方法制成的单层及多层膜。湿法涉及相转化法，举例如热相转化法(TIP)，其中使聚合材料与加工油或增塑剂合并以形成混合物，所述混合物在铸辊上挤出并冷却以形成前体膜。然后，当拉伸膜并萃取或移除增塑剂时在前体膜中形成孔(可以在移除油之前或之后对这些薄膜进行拉伸)。萃取步骤涉及溶剂的使用，这就是“湿法”名称的来源。湿法隔板具有在扫描电子显微镜(SEM)下呈网状外观的各向异性非定向的孔结构。参见图2。湿法聚乙烯(PE)微孔隔板膜是使用高分子量PE(典型地100,000至500,000)和/或超高分子量PE(典型地分子量>500,000，并且有时分子量≥100万)制成的。采用湿法制成的膜通常是双轴拉伸的，并且具有高的MD和TD拉伸强度。
通过干法和湿法制成的微孔隔板膜具有独特的隔板性能特性，这是由于它们的制造方法是不同的。通过干法或湿法制成的微孔隔板膜现今都常用在锂离子二次可再充电电池中作为电池隔板。
需要开发结合干法微孔膜与湿法微孔膜的性能特性的新型隔板膜，以生产具有平衡的MD和TD拉伸强度、高的总拉伸强度、高刺穿强度、良好的抗氧化性和断路功能的性能优越的隔板膜。
CN101469078A涉及电池隔板的微孔性多层膜，其公开的内容是，其低切断温度和高熔体破坏温度、高稳定性、高渗透性，使得其能够制造高容量和高功率的二次电池，这与本发明之间并没有关联。
CN102141387A涉及通过X射线的检测方法，与本发明的技术方案也没有关联。
CN1286502A、CN102209632A、CN102171855A、CN1883065A同样没有公开本发明与CN101469078A之间的实质性区别。
发明内容
一种用于锂二次电池的多层电池隔板，包括第一层干法的膜，其结合于第二层湿法的膜。第一层可由聚丙烯系树脂制成。第二层可由聚乙烯系树脂制成。隔板可具有不止两个层。隔板的TD/MD拉伸强度之比可在约1.5-3.0范围内。隔板可具有约35.0微米或更小的厚度。隔板可具有大于约630gf的刺穿强度。隔板可具有至少约2000V的介电击穿。
CN101469078A没有公开：“电池隔板的多层微孔聚烯烃膜”、“至少第一聚丙烯系树脂层结合于第二聚乙烯系树脂层”、“所述隔板具有35.0微米或更小的厚度”、“所述隔板具有大于等于630gf的刺穿强度”。
CN101469078A教导“刺穿强度为0.15-0.5N/微米”；而本发明的“刺穿强度”改善为至少630gf，即大约6.67N，这比CN101469078A的刺穿强度已经大出了数量级！
CN101469078A记载“当膜的厚度大于30μm时，隔板的渗透性变低，不适用于二次电池的隔板”。因此，CN101469078A明确教导，隔板的厚度不能大于30微米。相反，本发明的隔板厚度可达35.0微米，超出了CN101469078A教导的上限30μm！
附图说明
为了例示本发明的目的，附图中显示了目前优选的形式；然而要理解的是，本发明并不限于所示的精确布置及实施手段。
图1显示干法微孔隔板膜(现有技术)的照片(扫描电子显微镜，SEM)。
图2显示湿法微孔隔板膜(现有技术)的照片(SEM)。
图3显示混杂型微孔多层式隔板膜(本发明)的照片(SEM，3300x)。
图4是比较本发明隔板与对比专利实施例CE2的电阻(ER)热谱图的图表。
具体实施方式
本发明通常是一种混杂型隔板膜，其将通过干法制造的至少一层膜与通过湿法制造的至少一层膜相结合。这种隔板膜具有通过在多层电池隔板膜构造中将干法隔板膜同湿法隔板膜相结合而获得的优异的整体隔板及电池性能特性。
参考图3，所示为混杂型隔板10的一个实施方案。隔板10具有结合在一起的两个层，即顶层12和底层14。顶层12可通过湿法制成。顶层12可由聚乙烯系树脂制成(下文讨论的)。底层14可通过干法制成。底层14可由聚丙烯系树脂制成(下文讨论的)。
隔板10不限于图3中所示的实施方案。隔板10可具有两个或更多个层，例如两个、三个、四个、五个或更多(任意整数)个。在大多数实施方案中，层的数目可以为两个或三个。
可以改变构造(或各个层是如何堆叠的)。一般来说，隔板可具有一个干法的(DP)层和一个湿法的(WP)层。隔板可具有一个聚乙烯(PE)层和一个聚丙烯(PP)层。一个实施方案示于图3(DP-PP/WP-PE)。在另一实施方案中，隔板可具有DP-PP/WP-PE/DP-PP构造。在其它实施方案中包括且不限于：DP-PP/WP-PE/DP-PP；DP-PP/WP-PE/DP-PP/WP-PE；DP-PP/WP-PE/WP-PE/DP-PP；以及它们的所有排列组合。
如本文所用的干法通常是指将热塑性树脂挤成型坯(环状或平型)、对型坯进行退火处理、拉伸(单轴或双轴地)退火的型坯以形成微孔及任选对微孔膜进行热定型的过程。溶剂萃取是没有必要的，并且不使用增塑剂促进孔形成。干法是公知的，例如参见Kesting,Synthetic Polymeric Membranes,John Wiley&Sons,New York,NY(1985)，第290-297页，该文献的内容以引用的方式并入本文。干法产生的膜具有“狭缝样”的孔，参见图1，并且其在结构上不同于通过湿法制成的膜。
如本文所用的湿法通常是指将热塑性树脂和增塑剂(随后移除增塑剂以形成微孔)挤成平片、在冷却辊上冷却平片、拉伸冷却的平片并以用于增塑剂的溶剂萃取增塑剂以形成微孔膜的过程。湿法基于TIPS或“相转化”法(上文讨论的)。湿法是公知的，例如参见Kesting,Synthetic Polymeric Membranes,John Wiley&Sons,New York,NY(1985)，第237-286页，该文献的内容以引用的方式并入本文。湿法产生的膜具有“圆形”的孔，参见图2，并且其在结构上不同于通过干法制成的膜。
如本文所用的聚乙烯系树脂可以指聚乙烯或聚乙烯的共混物。聚乙烯可由乙烯单体和乙烯共聚单体制成。聚乙烯的共混物可由聚乙烯(至少50％)及其它热塑性树脂制成。聚乙烯可具有任意的分子量。分子量范围可从100,000到5-6百万。聚烯烃分子量可以被表征为正常(约100,000-400,000)、高(约400,000-800,000)和超高(约100万+)。通常情况下，干法使用正常和高分子量范围内的聚烯烃。通常情况下，湿法使用高和超高范围内的聚烯烃。
如本文所用的聚丙烯系树脂可以指聚丙烯或聚丙烯的共混物。聚丙烯可由丙烯单体和丙烯共聚单体制成。聚丙烯的共混物可由聚丙烯(至少50％)及其它热塑性树脂制成。聚丙烯可具有任意的分子量。
如所用的结合于在本文中是指用于将一个层层合到另一层而不封闭层的微孔的任何方法。结合可通过熔接或使用粘合剂进行。熔接是指热(热量)、压力、热及压力、超声和/或红外的。在一个实施方案中，可以通过使用热及压力熔接各层。
隔板可包括惰性或陶瓷颗粒、其它树脂(例如，PVDF)作为层的组分，如本领域中已知的那样。用来制层的树脂可包括其它已知的添加剂(例如，表面活性剂、防结块剂、抗氧化剂等)，如本领域中公知的那样。隔板还可以包括涂层，如本领域中公知的那样。
本发明可具有一组有益且独特的性质，这些性质可使其作为用在锂二次电池中的隔板是特别可取的。这些性质包括且不限于：
TD/MD拉伸强度(TD-横向方向，MD-机器方向)之比可在约1.5-3.0或约1.6-2.5或约1.8-2.2或其中包括的任意子组合范围内。
厚度可小于或等于35微米(μm)或在约5-30微米范围内或在约5-26微米范围内或在约5-15微米范围内或为其中包括的任意子组合。
刺穿强度可大于或等于630gf(克-力)或在约630-1500gf范围内或在约680-1200gf范围内或为其中包括的任意子组合。
介电击穿可以为至少2000V(伏)或在约2000-5000V范围内或在约2200-4500V范围内或为其中包括的任意子组合。
将在以下实施例中进一步例示本发明。
通过热层合选定的基底微孔膜来制备DP-PP/WP-PE双层和DP-PP/WP-PE/DP-PP三层。表1列出了用在双层和三层堆叠构造两者中的单层膜上的隔板特性数据以及本发明的构成的微孔多层隔板膜的隔板特性数据。由使用干法PE和PP微孔层制成的单层膜构成的两个比较商业隔板(厚度38μm的CE1和厚度25μm的CE2)已被包括在表1中用于比较目的。
表1
通过层合不同厚度的湿法PE和干法PP来制备各种厚度的混杂型层合膜。当比较实施例3与CE2时观察到刺穿强度提高两倍，后者的刺穿强度为380gf，前者的刺穿强度为812gf。当比较实施例3与CE1和CE2时还观察到TD拉伸强度的显著提高，后两者的TD拉伸强度分别为125和150kgf/cm2，前者的TD拉伸强度为683kgf/cm2。应当指出的是，本发明微孔隔板膜实施例显示出平衡的MD及TD强度。当用于锂离子电池的电池制造过程中时，这些隔板膜经得起苛刻的电池卷绕，并且抵抗TD方向上的开裂。此外，具有平衡的MD及TD拉伸强度的隔板膜抵抗由在电池卷绕操作期间可能存在的电极颗粒产生的穿透力。虽然全PE湿法多层隔板膜也将会显示出平衡的MD及TD拉伸强度，但这种类型的隔板将不具有由本发明混杂型微孔隔板膜所提供的抗氧化性。
表1中给出关于双层隔板膜实施例(实施例1和实施例2，厚度范围18至21μm)的数据，数据显示出平衡的MD及TD拉伸强度、优异的刺穿强度和高介电击穿。当双层中的PP层抵靠锂离子电池的阴极放置时可提供在电池循环期间的优异的抗氧化性，其导致循环寿命长。图3是实施例2按3,300x放大倍数取得的双层的SEM截面视图，PE层显示为顶层。孔形状及微结构的差别明显，并且与底部PP干法层相比，本领域的技术人员可以很容易地识别出顶部PE湿法层的典型孔结构。
对混杂型多层样品进行热电阻(热ER)测试以显示本发明混杂型膜的热稳定性。热ER是测量多孔膜经历断路的温度，即微孔膜孔熔化并关闭的温度。图4给出热ER曲线图，其中将膜的电阻绘制为温度的函数。本发明隔板在165摄氏度下显示出ER急剧增大，如针对含有聚丙烯的膜所预期的那样，已知含有聚丙烯的膜在大约165摄氏度下断路。此外，本发明混杂型隔板仍旧具有非常高的持久性电阻，这有别于PE1和PE2膜，后两者在130摄氏度下显示出ER急剧减小。在双层及三层构造中干法PP膜与湿法PE膜组合生产出在高温下维持持久水平电阻的混杂型隔板膜，结果电池在高工作温度下的安全性得到提高。
测试方法
厚度(T)
根据ASTM D374使用Emveco Microgage 210-A精密千分尺测量厚度。厚度值以微米单位μm记录。
Gurley值
ASTM Gurley值是通过Gurley透气度测定仪(例如4120型)测量的对空气流的阻力。Gurley值是以秒表示的在12.2英寸水柱的压力下使10cc空气穿过一平方英寸产品所需的时间，并且是根据ASTM D726(B)测定的。
基重(BW)
采用ASTM D3766确定基重，以mg/cm2为单位表示。
收缩率
通过将样品在105摄氏度烘箱中放置一小时，并将第二样品在120摄氏度烘箱中放置一小时，由此在两个温度下测定收缩率。在机器方向(MD)及横向方向(TD)两者上测定收缩率，并记录为％MD收缩和％TD收缩。
拉伸特性
根据ASTM-882程序，使用Instron型号4201测量机器方向(MD)及横向方向(TD)拉伸强度。
刺穿强度
基于方法ASTM D3763，使用Instron型号4442测量刺穿强度(定义为刺穿测试样品所需的力)。跨越膜的宽度进行十次测量并计算出平均刺穿强度。
电阻(ER)
电阻定义为以mohm-cm2表示的填充有电解质的隔板电阻值。
介电击穿(DB)
对隔板膜施加电压，直至观察到样品的介电击穿。坚固的隔板显示出高DB值，其中膜中的任何非均匀性会导致低DB值。
可以其它形式实施本发明而不偏离其实质及基本属性，并且因此应当参考所附的权利要求而不是前述说明书来指示本发明的范围。

Claims (17)

1.一种用于锂二次电池的多层电池隔板，包括至少第一聚丙烯系树脂层，其是由干法制备的带狭缝样孔的膜，第一聚丙烯系树脂层结合于第二聚乙烯系树脂层，其是由湿法制备的带圆孔的膜；所述隔板具有1.5-3.0范围内的MD/TD拉伸强度的比值、35.0微米或更小的厚度、大于等于630gf的刺穿强度和至少2000V的介电击穿电压。
2.如权利要求1所述的隔板，具有至少三个层。
3.如权利要求1所述的隔板，其中，所述聚丙烯系树脂是聚丙烯或含有聚丙烯的共混物。
4.如权利要求1所述的隔板，其中，所述聚乙烯系树脂是聚乙烯或含有聚乙烯的共混物。
5.如权利要求2所述的隔板，具有聚丙烯层/聚乙烯层/聚丙烯层的构造。
6.如权利要求2所述的隔板，具有干法的层/湿法的层/干法的层的构造。
7.如权利要求1所述的隔板，具有1.6-2.5范围内的MD/TD拉伸强度的比值。
8.如权利要求1所述的隔板，具有1.8-2.2范围内的MD/TD拉伸强度的比值。
9.如权利要求1所述的隔板，具有5.0-30.0微米范围内的厚度。
10.如权利要求1所述的隔板，具有5.0-26.0微米范围内的厚度。
11.如权利要求1所述的隔板，具有630-1500gf范围内的刺穿强度。
12.如权利要求1所述的隔板，具有2000-5000V范围内的介电击穿电压。
13.如权利要求1所述的隔板，仅仅具有两个层。
14.一种电池，包括如权利要求1所述的隔板。
15.一种电池，包括如权利要求2所述的隔板。
16.一种电池，包括如权利要求13所述的隔板。
17.一种电池，包括如权利要求6所述的隔板。
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