CN1580343A - 超薄、多孔和机械牢固的无纺布及其制造方法和应用 - Google Patents

超薄、多孔和机械牢固的无纺布及其制造方法和应用 Download PDF

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CN1580343A
CN1580343A CNA2004100700306A CN200410070030A CN1580343A CN 1580343 A CN1580343 A CN 1580343A CN A2004100700306 A CNA2004100700306 A CN A2004100700306A CN 200410070030 A CN200410070030 A CN 200410070030A CN 1580343 A CN1580343 A CN 1580343A
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nonwoven fabric
thickness
fiber
calender
pore diameter
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CN100400734C (zh
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P·克里策
R·费雷
G·弗雷
M·安佩尔格鲁恩
R-P·施沃贝尔
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Carl Freudenberg KG
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Carl Freudenberg KG
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Abstract

介绍一种具有小于等于300μm厚度的，化学和/或热力结合的无纺布，其在至少一个方向的最大拉力最小为15N/5cm，其在这个方向的最大拉力延伸率最多为35％，并且具有至少25％的孔隙度。这种无纺布可以用作隔片材料或膜的基体材料。

Description

超薄、多孔和机械牢固的无纺布 及其制造方法和应用
技术领域
本发明涉及一种超薄、多孔同时机械牢固的无纺布及其制造和应用，例如用作用于电化学电池如蓄电池、电池或燃料电池以及用于电能存储器如超级电容器的隔片。
背景技术
电化学电池必须具有隔片，它在电池内将两个带不同电荷的电极分开，从而防止内部短路。对隔片材料有多个要求，它们可综述如下：
1、对电解液的耐久性，
2、耐氧化性，
3、高的机械牢固性，
4、小的重量和厚度偏差，
5、较小的离子穿透阻力，
6、较大的电子穿透阻力，
7、对由电极上脱落下来的固体颗粒的过滤能力，
8、立即自动的电解液可润湿性，
9、电解液的永久可润湿性，
10、对电解液液体高的储存能力。
纺织平面结构，特别是由合成纤维组成的无纺布，由于对电解液液体良好的耐久/抗性及其高的柔性很好地适合于作为隔片材料。
目前可供选择的材料是纸，但是由于其高的密度只具有小的多孔性，因此特别是对于需要稀疏材料的应用场合不予考虑。另一种可供选择的材料是薄膜，但是它在所采用的聚合物方面受到限制，并且通常只具有小于25％的小的孔隙度以及小于0.5μm的小的孔隙直径。迄今为止用已知的无纺布产品不能达到小于20μm的厚度。具有小得多的厚度和同时具有良好的机械性能以及高的孔隙度的无纺布产品对于许多新的应用场合是值得追求的。
这种类型的无纺布例如可以用作锂电池、碱性电池、超级电容器或燃料电池中的隔片一支承材料，以及用作过滤薄膜的基体材料。
将无纺布用作薄膜的基体和支承材料是已知的。在这种应用场合液体在高的机械压力作用下受挤压穿过这种加固的薄膜，并得到过滤。
在这种使用情况下对支承材料有以下要求：
●相对于待过滤溶液的化学耐久性
●足够的机械强度
●“相容性”，即基体材料与大多用挤出法涂在它上面的薄膜聚合物的良好附着性能
●极其光滑的表面，使得不会有翘起的纤维刺穿薄膜。
在这种应用场合这些性能的重要程度是：
强度＞＞均匀性＝厚度＞构造。
支承材料的机械牢固性理所当然是最重要的。最大拉力的典型数值为＞＞200N/5cm。在采用普通材料时由此得到＞200μm的厚度和＞60g/m2的面重量。
因为在这种系统中所用的薄膜具有非常小的孔隙直径(通常＜＜1μm)和小的孔隙度，存在高的孔隙度以及支承材料孔隙大小的均匀分布是第二位的。因此对于这种材料通常采用粗纤维(纤度大于1.5dtex)。存在迷宫式构造以及这种材料小的厚度对于这种应用场合并不绝对需要。
如果应该用无纺布作为用于例如锂电池、碱性电池和燃料电池中的隔片的基体材料，那么为此它必须满足前面所列的标准。
这里化学性能这样来选择，即
a.在通常高达70℃的持续温度下对电解液(在锂电池时为有机介质、在燃料电池时为强酸性含水溶液、在碱性电池时为强碱性溶液)的化学耐久性，以及抗氧化性，和
b.在隔片与电解液接触时没有或至少只有很小的机械膨胀。其次由材料的形态/几何形状确定的性能这样来选择，即
a.存在小于30μm，尤其是小于20μm的小的厚度(厚度与隔片的离子穿透阻力成线性关系)，
b.在保持孔隙均匀分布的同时存在高的孔隙度(孔隙度直接影响离子穿透阻力；因此这种材料的孔隙度应该＞25％，尤其是＞45％；并且为了保证孔隙均匀分布，最大孔隙尺寸至多为最可能的孔隙尺寸的2.5倍)，
c.存在小的孔隙尺寸，使得在电池内不能进行树枝结构的生长(然而在无纺布用作支承材料时这一点只起不太重要的作用，因为通常加入的凝胶/膏料承担这个任务，但是对于这两种应用场合最大孔隙尺寸通常应该保持500μm)，
d.存在足够大的孔隙尺寸，使得膏料或凝胶可以进入孔隙内(这里最小平均孔隙尺寸应该超过0.5μm)，
e.对于电池的组装存在足够大的机械牢固性(在实际上对于工业处理证明最大拉力至少为15N/5cm是合适的)，
f.在受到机械应力时存在小的材料延伸(太大的延伸值会导致材料的变形；实际表明，在最大拉力时延伸量不应超过35％)，
g.可以方便地制造隔片。
与上面给定的用作薄膜基体或支承材料不同，性能的重要程度如下：
厚度＞＞孔隙度＝均匀性＝构造＝机械强度
普遍而言，具有小于30μm厚度的无纺布可以通过压延/轧光不同类型的材料达到，然而应该注意，例如按标准在用作隔片材料时所用的具有2dtex纤维纤度的聚烯烃纤维便已经有约17μm的纤维直径，50μm厚的材料最多只能由三层这种纤维组成。虽然这种面重量比较重的材料的压延可以造成薄的材料，但是在这种情况下所形成的材料这样致密，使得造成大的离子穿透阻力。
因此如果除小的厚度外还需要足够高的机械强度和高的均匀性以及紧密的孔隙分布，那么不太优先采用网状结构(材料纤维太粗，因此孔隙太大)以及纸(材料太致密)。
锂离子蓄电池的隔片通常由大多由聚烯烃制成的微孔薄膜组成。孔隙度较小，大致为小于25％，因此所造成的电阻大。它们没有明显的离子导电性。在EP-A-811479中介绍了在至少一个表面上用聚烯烃纤维无纺布层压的微孔聚烯烃薄膜及其作为隔片的应用。按照说明聚烯烃无纺布在层压以前具有30至500μm的厚度。
US-A-5500167介绍了一种用于过滤的加基体的微孔薄膜。采用多孔无纺布作基体。关于所用无纺布的厚度没有提供数据；但是对于其制造采用具有20-25μm直径的纤维。因此形成的无纺布具有明显超过50μm的厚度。
由US-B-6277282已知一种用于可逆渗透的薄膜元件，它由许多层组成。一个这种层可以由一无纺布构成。按照说明书这个层的厚度为50至200μm。
对于锂—聚合物蓄电池目前采用由有离子导电能力的聚合物组成的薄膜(例如在DE-A-19916109；DE-A-19916043；DE-A-19855889和相应于EP-A-662250的WO-A-93/13565中介绍过)。在制造时将溶解或分散在有机溶剂中的组成部分涂在一薄膜上，使溶剂按规定蒸发。接着大多进行热力的或紫外线引起的交联过程。这样制成的离子导电薄膜具有比上述微孔薄膜小得多的穿透阻力。通常这种由离子导电聚合物组成的薄膜在一连续工序中层压在电极上。问题主要是这种薄的薄膜机械强度小。在制造时可能产生裂缝或完全撕裂。在第一种情况下在以后的电池上出现不可修负的损坏，在第二种情况下必须停止生产。在实践中通过这样的方法补救，即首先将这种薄膜铺在一膜片上，以后再撕下来，膜片通常不能第二次使用。除了造成废弃物和与之相关的额外费用以外，在薄膜从膜上撕下来时可能出现问题；这里也不排除薄膜的撕裂。
由JP-A-2000-195494已知一种钮扣电池，其中也可以采用无纺布隔片。这种无纺布除耐热结构材料外还由聚合物组成，它在与电解液接触时胀大，从而吸收电解液。关于这种无纺布的厚度没有给出说明。
JP-A-11/176419介绍了一种二次锂电池，它由一多层电极—隔片结构组成。20-200μm厚的隔片由耐热结构材料组成，在这里是PVDF或PVDF-HFP-混合物。这份资料介绍一种在无纺布厚度在50至100μm之间的良好特性。由于无纺布小的撕裂强度不可能达到20μm以下的厚度。
在WO-A-00/177875中介绍了由多层电极—隔片结构组成的二次锂—聚合物电池制造过程的简化。按照这份资料制造薄的电极材料，它们从有机溶液中用由聚烯烃或聚酯组成的(非多孔)膜片铺放在纸上或一非常强烈地压延的致密聚酰胺无纺布上。这里这个“托板(Vorlage)”用作用于接着的电极借助于结合剂的层压(“带连铸”)。在这份资料中得不到关于“托板”几何尺寸的说明。
WO-A-99/31743介绍了分散的电极层在隔片表面上的沉积。在这份资料中同样找不到关于托板几何尺寸的说明。
在DE-A-2547958中介绍了薄纤维无纺布和通过将大体积/膨松和加固的无纺布分成薄层而制造薄纤维无纺布的方法。介绍了具有20g/m2以下重量的无纺布。然而在这份资料中没有看到关于这种无纺布的厚度和机械性能的说明，但是这牵涉到一种大体积和疏松的原材料，因此由此制成的无纺布不具有特别好的机械性能。
发明内容
本发明的目的是提供一种超薄的、同时又机械牢固的高孔隙度无纺布。
本发明的另一个目的是提供一种具有上面规定的性能以及一个规定的孔隙结构的无纺布。
本发明的又一个目的是提供一种超薄无纺布，它是足够机械牢固的，以便可以不用辅助措施如支承膜进行处理，并且它可以用作电化学电池中的隔片材料。
本发明的再一个目的是提供这种新型无纺布的制造方法。
本发明涉及一种具有小于等于30μm，尤其是小于20μm厚度的无纺布，它化学和/或热力结合，其最大拉力在至少一个方向至少为15N/5cm，尤其是至少为20N/5cm，其在该方向的最大拉伸延展率为最多35％，尤其是最多25％，并具有至少25％，尤其是至少40％的孔隙度。
本发明的无纺布是超薄的，通过采用选择的湿无纺布或干无纺布材料在小的厚度时既可以达到无纺布要求的均匀性，又达到足够的机械牢固性。这样制成的无纺布可以用于很多应用场合，尤其是电子类型的应用场合。
制造本发明的无纺布的纤维可以由不同的形成纤维的材料，特别是形成纤维的聚合物制成。纤维材料必须能经受所考虑的应用条件。
可以采用所有形成纤维的材料。例如聚丙烯腈、碳、玻璃、聚酰胺，特别是聚酰胺6和聚酰胺6.6，优先采用聚烯轻，特别优先采用聚酯，特别是聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯。
通常聚烯烃是聚α-烯烃。它们可以作为均聚物，如聚乙烯或特别是聚丙聚，或作为共聚物，如由丙烯和丁烯衍生的共聚物，存在。
聚烯烃的例子是聚丙烯、聚乙烯和烯烃共聚物，它们例如借助于齐格勒—纳塔或茂金属催化剂制造。
制造本发明无纺布的纤维可以作为切断的短纤维、切段短纤维或无端单丝存在。在某些情况下它们可以具有卷曲。也可以是极其不同类型的纤维的组合。
本发明的无纺布可以由任何种类的纤维组成。其直径通常小于20μm，尤其是0.5至18μm，特别优先为1至15μm。除了可以采用特别是由热塑性聚合物组成的均质/单组分纤维。也可以采用异质纤维一尤其是包含至少一个聚烯烃成分的异质纤维，例如双组分纤维。
与存在单组分纤维还是多组分纤维无关，纤维的横截面可以做成圆形、椭圆形、表面开槽的、小带状的、三叶形或多叶形的。
本发明的无纺布可以用不同的堆置方法形成，可以采用湿法无纺布，梳理的短纤维无纺布、熔喷无纺布以及在应用多组分纤维的情况下采用纺粘型非织造物作为各层。
通常本发明的无纺布具有3至25g/m2的面重量。
特别优先采用湿法无纺布或短纤维无纺布。
制造本发明无纺布的纤维或者用机械方法或者用空气动力方法伸长或拉伸。但是也可以设想，拉伸的纤维混入那种既可以是相同的也可以是不同的仅仅局部(部分)或者完全没有经过拉伸的聚合物成分。
借助于纺粘型非织造工艺制造的并包含至少一种最好是仅仅一种双或多组分纤维的无纺布特别优先。
同样优先采用用熔喷工艺制造的无纺布。
此外无纺布优先包含选自聚烯烃、聚酯、聚丙烯腈、聚酰胺、聚酰亚胺、聚碳酸酯、聚砜、碳、玻璃以及它们的混合物的纤维。
在采用由这些材料，特别是聚烯烃或聚酯组成的纤维时在与电解液接触时不发生隔片的胀大。在电池不经受机械压力时或电池带有柔性壳体时这种胀大带来隔片厚度不希望的加大。
本发明的无纺布借助于热力和/或化学连结加固/结合。也就是说它们通过采用粘合纤维、熔合粘接剂和/或化学结合剂结合，和/或纤维通过无纺布制造法或处理法部分熔化，由此形成相互的结合。
本发明的无纺布具有高的孔隙度P。这在本说明书范围内理解为以下表达式：
P＝(1-FG/(d·ρ))·100
其中FG是面重量(kg/m2)，d是厚度(m)，ρ表示密度(kg/m3)。
在本发明无纺布中的最大孔隙直径通常为500μm，特别是最大为300μm。
优先采用其最大孔隙直径最多为平均孔隙直径2.5倍这么大的无纺布。
特别优先采用其最小平均孔隙直径大于0.5μm，特别是大于1.0μm的无纺布。
本发明的无纺布在至少一个方向的最大拉力时通常具有最大为35％的延伸率。
本发明还涉及上面确定的无纺布的制造方法，它包括以下工步：
1.通过公知的湿或干无纺布形成法制造具有小于25g/m2，尤其是3至25g/m2面重量的无纺布，和
2.压/轧延无纺布，以使它加固并减小其厚度。
在工步(1)中得到的纤维层可以在热和压力作用下压延之前通过加固无纺布的已知方法预结合，其中结合可以是部分面积或整面的。
本发明的方法建立在无纺布压延的基础上。
压延成超薄无纺布促使原料无纺布的致密化和在某些情况下在加固条件下熔融活性纤维或纤维组成部分的自焊接。
压延通过热和压力进行。
在采用聚烯烃纤维的情况下根据各自采用的烯烃纤维或纤维组分的不同通常采用100至160℃的压延温度。压延条件完全特别与在各自情况下所用的聚合物的熔化和软化特性相匹配。在采用聚酯，例如聚对苯二甲酸乙二酯时压延温度通常为170至230℃。
压延机基本上由两个光滑轧辊组成。在希望产生形成花纹的表面的个别情况下轧辊也可具有压印图案。
自焊接意思是指无纺布内有关纤维或纤维的一部分在不添加其它粘接剂的情况下焊接。
优先采用这样的方法，其中热力加固和精压在无纺布制造设备内(在线)或在一单独的工序内用一压延机进行，压延机由由同一材料尤其是钢或类似的高合金材料组成的两个轧辊的组合组成。
在另一种优先的方法中热力加固和精压在无纺布制造设备内(在线)或在一单独的工序中用一压延机进行，此压延机由由不同硬度的材料，尤其是钢或类似的高合金材料和由热稳定塑料组成的两个轧辊的组合组成。
在本发明方法的另一种优选方案中无纺布表面被赋予永久的亲水性，尤其是借助于气相氟化、等离子处理、硫化有极性有机族的接枝(Aufpropfung)、或给聚合物熔液添加亲水熔融添加剂。
本发明的无纺布可以用作电化学电池或蓄能器，特别是电池、蓄电池、电容器和/或燃料电池中的隔片材料或隔片基体材料。
另一种应用是将本发明的无纺布用作过滤器膜的基体材料。
这些应用也是本发明的主题。
以下例子说明本发明，但是并不局限于此，应用例：
制造或采用以下无纺布/网(参见表1)：
例1：热力加固/粘合的和接着在120℃及50N/mm线性压力时压延的具有15g/m2面重量和20μm厚度的聚烯烃湿法无纺布(PP纤维和PP/PE-芯部外壳纤维；两种纤维的纤度＜1.0dtex)。
例2-4：具有不同面重量和厚度(参见表2)的不同热力加固的聚酯湿法无纺布(拉伸和未拉伸的聚酯纤维；纤维纤度分别小于1.0dtex或1.5dtex)。这里厚度精压在线地在无纺布铺放后或在一单独的工序中进行。其中在线加固用具有钢—钢，钢—Scappa或钢—硅树脂轧辊组合的压延机在温度为170-225℃时进行。材料在表2中列出。这种材料的一部分不是在线压延，亦即“疏松地”运送，而只有在接着在另一个工序中在170-220℃时才热力定型。这些材料在表3中列出。对于各种材料线性压力在60-70N/mm范围内。
例5-6：由聚丙烯腈纤维(纤维纤度＜1.0dtex)组成的湿法无纺布，它用丙烯酸酯结合剂热定型，接着在180℃和80N/mm线性压力情况下压延。面重量和厚度参见表1。
例7：热加固和接着压延的具有15g/m2面重量和19μm厚度的聚酯干法无纺布(拉伸和未拉伸的聚酯纤维(纤维纤度分别小于1.5dtex)；在225℃和80N/mm线性压力的条件下压延)。
例8：热加固和接着压延的具有15g/m2面重量和18μm厚度的聚酰胺干法无纺布(PA66以及PA66/PA6双组分纤维；纤维纤度1.0和1.7dtex；在230℃和80N/mm线性压力的条件下压延)。
对比例1：由聚酯组成的纺粘型非织造织物(纤维直径约8μm)，它接着在215℃和80N/mm的条件下压延(面重量为14g/m2，厚度为20μm)。
例9：由双组分聚烯烃纤维组成的纺粘型非织造织物(PP和共聚PP；纤维直径约10μm，相应地纤度约为1.0)，它接着在135℃和70N/mm线性压力的条件下压延(面重量为8g/m2，厚度为18μm)。
例10：由PP按熔喷工艺制造的无纺布，具有2至3μm的纤维直径，它接着在20N/mm的线性压力和130℃的温度时压延(面重量：12g/m2；厚度：20μm)。
对比例2：150μm厚的聚酯网，接着在235℃和80N/mm的线性压力下压延(面重量为14g/m2；厚度为28μm)。
对比例3：具有约50μm纱线直径的180μm厚的聚丙烯网，接着在135℃和50N/mm的线性压力下压延(面重量为16g/m2；厚度为30μm)。
对比例4：具有约20μm纱线直径的120μm厚的细网目聚丙烯网，接着在138℃和50N/mm的线性压力下压延(面重量为10g/m2；厚度为20μm)。
面重量的确定：
材料的面重量按EN29073T1确定。
厚度的确定：
材料的厚度根据EN20534确定(测量杆的测量压力为10kpa，施加在2cm2的测量面上)。
机械强度的确定：
材料的最大拉力(HZK)按EN29073T3确定。
孔隙直径的确定：
按标准ASTM E1294(Coulter Porometer)确定平均孔隙直径以及最大孔隙直径(泡点bubble Point)。
表1：不同制造技术制造的超薄无纺布的数据比较
例子编号 制造方式 聚合物   面重量(g/m2)   厚度(μm)   纵向最大拉力(N/5cm)   纵向最大拉力延伸率(％)   平均孔隙直径   最大孔隙直径 孔隙度(％)
  1   湿   PO   13   20   45   25   70   90   45
  2   湿   PES   12   20   30   12   50   65   57
  3   湿   PES   10   16   28   10   38   61   55
  4   湿   PES   8   12   25   10   42   67   52
  5   湿   PAN+Acrylat   12   20   27   12   13   20   48
  6   湿   PAN+Acrylat   10   18   20   14   43   65   52
  7   干   PES   15   19   50   24   90   180   44
  8   干   PA   15   18   26   27   160   260   27
  对比例1   纺粘型   PES   14   20   12   78   200   400   50
  9   纺粘型   PP+CoPP   8   18   22   27   190   350   51
  10   熔喷   PP   12   20   22   15   10   15   34
  对比例2   网   PES   14   28   45   38   1600   2000   64
  对比例3   网   PP   16   30   75   85   1200   1400   41
  对比例4   网   PP   10   20   24   150   650   900   45
上面的应用实例显示，以下制造过程非常适合于制造符合前面所述要求的材料：
●湿法无纺布加上在线或后续的压延。
●干法无纺布加上在线或后续的压延。
●由双组分纤维制成的纺粘型非织造织物，接着热加固。
●熔喷无纺布，接着压延。

Claims (15)

1.具有小于等于30μm的厚度的化学和/或热力结合的无纺布，其在至少一个方向的最大拉力至少为15N/5cm，以及在这个方向的最大拉力延伸率最多为35％，和具有至少为25％的孔隙度。
2.按权利要求1所述的无纺布，其特征为：其厚度最多为20μm。
3.按权利要求1所述的无纺布，其特征为：它是一种湿法无纺布，梳理短纤维无纺布、熔喷无纺布；以及一种在制造中采用多组分纤维的纺粘型非织造织物。
4.按权利要求1所述的无纺布，其特征为：它包含选自聚烯烃、聚酯、聚丙烯腈、聚酰胺、聚酰亚胺、聚碳酸酯、聚砜、碳、玻璃及其混合物的纤维。
5.按权利要求1所述的无纺布，其特征为：它通过采用粘合纤维、熔化粘接剂和/或化学结合剂结合。
6.按权利要求1所述的无纺布，其特征为：无纺布的孔隙度至少为40％。
7.按权利要求1所述的无纺布，其特征为：其最大孔隙直径为500μm，特别是小于300μm。
8.按权利要求1所述的无纺布，其特征为：其最大孔隙直径最多为平均孔隙直径的2.5倍这么大。
9.按权利要求1所述的无纺布，其特征为：其最小平均孔隙直径大于0.5μm特别是大于1.0μm。
10.制造按权利要求1所述的无纺布的方法，包括以下工序：
1)通过已知的湿法、干法无纺布制造法或按权利要求5所述的纺粘法制造具有3至25g/m2面重量的无纺布，和
2)将无纺布压延，以使其加固并减小其厚度。
11.按权利要求10所述的方法，其特征为：在无纺布制造设备中在线地或在一单独工序中用一压延机进行热加固和精压，压延机由两个由相同的材料，尤其是由钢或类似的高合金材料组成的轧辊的组合组成。
12.按权利要求10所述的方法，其特征为：在无纺布制造设备中在线地或在一单独的工序中用一压延机进行热加固和精压，压延机由两个不同硬度的材料，尤其是钢或类似的高合金材料和热稳定的塑料组成的轧辊的组合组成。
13.按权利要求10所述的方法，其特征为：无纺布表面赋予永久亲水性，尤其是借助于气相氟化、等离子处理、硫化极性有机族的接枝，或给聚合物熔液添加亲水的熔融添加剂。
14.按权利要求1所述的无纺布用作电化学电池或蓄能器，特别是电池、蓄电池、电容器和/或燃料电池中的隔片材料或隔片基体材料。
15.按权利要求1所述的无纺布用作过滤器膜的基体材料。
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US8962127B2 (en) 2015-02-24
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