CN101558194A - 改进的纳米纤网 - Google Patents

改进的纳米纤网 Download PDF

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CN101558194A
CN101558194A CNA2007800345429A CN200780034542A CN101558194A CN 101558194 A CN101558194 A CN 101558194A CN A2007800345429 A CNA2007800345429 A CN A2007800345429A CN 200780034542 A CN200780034542 A CN 200780034542A CN 101558194 A CN101558194 A CN 101558194A
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nanowebs
fibre web
woven
web
roller
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CN101558194B (zh
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P·阿罗拉
陈光辉
S·弗里斯克
D·K·小格雷汉
R·A·马林
徐鹤殷
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DuPont Safety and Construction Inc
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EI Du Pont de Nemours and Co
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Abstract

本发明提供了数均直径小于1微米的纤维的非织造纤网。所述纤网的泊松比可小于约0.8，密实度可至少为约20％，基重可至少为约1gsm，厚度可至少为约1微米。

Description

改进的纳米纤网
本发明涉及包含纳米纤维的改进的非织造纤网及加固和稳定化这类纤网的方法。
背景
“纳米纤网”是主要或甚至只包含数均直径小于一微米的纤维的非织造纤网。由于其特别小的孔尺寸和高的表面积与体积比，故纳米纤网已预期用作许多应用如高性能空气过滤、废水过滤、生物污染物过滤膜、电池及其他储能设备的隔离物的基材。但对于这些应用，纳米纤网的一个缺点在于其力学完整性差。
纳米纤维的数均直径小于1000nm，有时小到20nm。在该尺寸下，即便其层化并形成为厚膜，所得结构的力学强度也不足以承受过滤应用如流经其的正常液体或气流的宏观冲击或最终用途制造步骤中卷绕和操作所需的更高强度。通过例如电纺或电喷制得的纳米纤网的固体体积含量(密实度(solidity))也倾向于较低，通常低于约20％。
当在纵向(MD)上施加了张力时，例如当卷绕或后处理时，例如当为某些产品应用而施加表面处理和层压时，无支承的纳米纤网也表现出宽度的过度减小(“颈缩”)。当材料被解卷和再次卷绕时，不同的张力可能导致不同的宽度并潜在地引起片材性质的改变。需要对外加张力更稳定的材料。
当处理片材或当片材在辊或其他表面上移动时，电纺和电喷纳米纤网的低表面稳定性也引起问题。纤维从片材上移出并收集在各种接触表面例如手、辊、导板等上，且片材性质可能潜在地改变和/或工艺装置被纤维所污染。需要具有更稳定表面的材料。
“初生”纳米纤网的开放结构通常产生密实度在20％-10％范围内或甚至更低的结构。由于密实度低，此开放结构对流体流和/或离子流的阻力低，这反过来可报道为总的孔体积百分数大或“多孔”。通常，初生纳米纤网纤维间的最大孔径在约0.5-10微米范围内，甚至高达20微米，平均流量孔径(mean flow pore size)介于约0.05到10微米之间。
一些织物应用需要较小的孔径和因此较高的纤网密实度(接近或甚至在40％-90％范围内)。这些织物对流体具有更高的过滤效率和通常更好的整体阻隔性以及在电池隔离物隔离物及其他储能应用中的抗“短路”性。其他应用在产生对湿气透过的低阻力的同时，需要低的空气流量和低的液体流量且需要更高百分密实度的材料或小孔。常规纳米纤网目前被排除出这些需要更高密实度的应用中，因为通常没有足够的纳米纤网材料经改性为更小的孔径和更高的密实度。相反，可以工业可接受的尺寸和基重生产的非织造纤网如熔喷纤网常用于这类应用中。但熔喷纤网由直径通常在约2-10微米之间的大得多的纤维组成，改性初生熔喷纤网以满足高过滤效率所必要的小孔径限制需要甚至高达约80％的高密实度而导致通过这类改性熔喷纤网的流体流率的显著降低。
“初生”纳米纤网也具有较高的表面曳力(drag)或摩擦，表面摩擦系数高达约2.5。一些材料应用需要更光滑或更软的低摩擦手感。其他应用需要光滑的外表面以便滤饼释放或降低液体流动阻力。对于将用于这些应用中的材料，其需要增进低摩擦和高耐磨性的“光滑”表面。
众所周知，纤网的物理性质可通过压延改进，压延是使片材通过辊或板间的间隙以赋予片材光滑、有光泽的外观或改进选定物理性质的方法。
通过纸或其他纤维材料的压延，人们努力进一步改进所形成的纸的质量或提供标准质量水平以获得更高的运行速度或增大纸的生产量。众所周知，纸或纤维的塑性或模塑倾向可通过提高纸或纤维的温度和/或增塑剂含量而增加。当纸内所含聚合物的温度升到所谓的玻璃化转变温度(Tg)或超过该温度时，力学性质包括塑性将发生相当大的改变，其中所述玻璃化转变温度为材料可变得比低于该温度时更易于模塑或成形或修整的点。
现有技术公开了使纤网纤维的变形仅局限于纤网的表面部分的各种方法和装置。美国专利4,606,264提供了温度梯度压延的方法和装置，其中纸等材料进入铁辊和软辊所形成的至少一个辊隙中。铁辊至少被加热到纤网中的纤维开始变形的温度；对于纸来说，该温度为约350°F。如其中所公开的，优选纤网通过两个连续的辊隙，一个用来磨光纤网的一面，另一个用来磨光相反的面。
许多非织造织物是丝间粘结的以赋予织物完整性。虽然有若干粘结技术，但就倾注于新产品的研究和开发中的规模和时间而言，非织造工业中盛行的是热粘结方法。由于简单及相对于传统化学粘结方法的诸多优势，这些方法已获得广泛的接受。吸引人的特征包括低能量和原材料成本、提高的生产率和产品多用性。由于不使用粘合剂，故化学简化减少了环境考虑。美国专利4,035,219和US 5,424,115提供了非织造纤网的点粘结以增强物理性质的实例。
授予Reed的美国专利2,277,049介绍了使用可熔纤维通过共混类似旦尼尔和切断长度的可熔和不可熔纤维并用溶剂或热处理纤网制备非织造织物的思想。可熔纤维变得发粘而充当粘合剂。压缩并冷却发粘纤网后得到非织造织物。
但接近纳米纤网中纤维熔点(Tm)的温度的使用对纤网的质量有害。纤维的小尺寸以及压延机械中固有的不均匀加热倾向于产生不均匀的熔化和粘结而降低纤网在过滤和电池隔离物隔离物和其他储能应用中的有效性。在低基重并包含细旦纤维的纤网强化领域中现有技术的缺陷示例于EP 1 042 549中，其中使用了带式样的热粘结来产生较不易变形的纤网。系数泊松比乘基重(单位盎司每平方码)公开为限制于低于1.2，但示例的泊松比约为2.5-4。同样，美国专利5,858,515中描述了强化纤网的一种粘结样式但代价是开口区域或多孔性的显著降低。
但这些现有技术方法既未考虑也未涉及纳米纤网结构的稳定化，纳米纤网的易损性质(dilicate nature)已因此阻止了将这些技术应用于其稳定化。使这类细纤网熔化或变形的温度的使用实质导致纤网纤维网络的破坏。
因此需要强化纳米纤网而保持其多孔性和均匀性的方法。
本发明涉及通过改进其物理性质增进纳米纤网的实用性同时保持高的开口区域并因此具有多孔性以及涉及由此产生的纤网。
发明概述
在一个实施方案中，本发明的产品为非织造纳米纤网，所述纤网包含泊松比低于约0.8、密实度至少约20％、基重至少约1克每平方米(gsm)、厚度至少约1μm的聚合物纳米纤维的纤网。
本发明也涉及一种非织造纤网，所述纤网通过经第一辊和第二辊间的辊隙压延聚合物纳米纤网、向纤网的厚度上对纤网施加压力并加热纤网至纳米纤网聚合物的Tg和Torn间的温度下形成，其中所述第一辊和第二辊中的一个为硬辊，另一个辊为硬度低于Rockwell B 70的软辊，其中Torn定义为熔化开始的温度，其中所述纳米纤网在纤网平面中包含熔化区域的面积低于约15％。
本发明也涉及稳定化电喷或电纺聚合物纳米纤网的表面的方法，所述方法包括经第一辊和第二辊间的辊隙压延纤网、在纤网的厚度上对纤网施加压力和加热纤网至其Tg和Torn间的温度，其中所述第一辊和第二辊中的一个为硬辊，另一个辊为软辊。
在另一实施方案中，本发明涉及一种包含聚合物纳米纤维的非织造纳米纤网，所述纤网的密实度至少为约20％、基重至少为约1gsm、厚度介于约1μm和400μm之间、最大孔径为约5微米，其中所述纳米纤网在纤网平面中包含熔化区域的面积小于约15％。
在又一实施方案中，本发明涉及一种包含聚合物纳米纤维的非织造纳米纤网，所述纤网的密实度至少为约20％、基重至少为约1gsm、厚度至少为约1μm、纵向上的断裂拉伸强度至少为约4.1MPa，其中所述纳米纤网在纤网平面中包含熔化区域的面积小于约15％。
附图简述
图1为得自本文中作为对比例1描述的电喷方法的初生纳米纤网的显微照片。
图2为在两个硬辊间压延的纳米纤网的显微照片，其中示出了纳米纤网中的熔化区域。
图3a和3b为以本发明的方式压延的纳米纤网的显微照片。
发明详述
本发明涉及改进聚合物纳米纤网的力学完整性包括表面稳定性、强度和泊松比同时保持其多孔性的方法以便纳米纤网适合于各种高性能应用如用于液体过滤和电池或其他储能设备如电容器等中的隔离物。所述方法避免在粘结点熔融纤网的纳米纤维且不采用胶粘剂粘结而稳定化纳米纤网的表面和其横向宽度尺寸同时不显著影响纳米纤网的多孔性。压延/拉伸方法可用来控制聚合物纳米纤网的孔径和/或密实度。
术语“非织造”指含大量无规分布的纤维的纤网。所述纤维通常可彼此粘结或可未粘结。所述纤维可为短纤维或连续纤维。所述纤维可以不同纤维的组合或以各由不同材料组成的类似纤维的组合包含单一材料或多种材料。
“压延”为纤网通过两辊间的辊隙的方法。所述辊可彼此接触或辊表面间可有固定或可变的间隙。有利的是，在本发明的压延方法中，所述辊隙形成在软辊和硬辊之间。“软辊”为在施加以使两辊一起保持在压延机中的压力下变形的辊。“硬辊”为具有在工艺压力下不发生对工艺或产品有显著影响的变形的表面的辊。“无图案的”辊为在用来制造其的工艺能力内具有光滑表面的辊。与点粘结辊不同，其上没有点或图案，当纤网通过辊隙时，纤网上不蓄意产生图案。
“平纹棉麻织物(scrim)”为支承层，可为可粘结、粘附或层合纳米纤网的任何平面结构。有利的是，本发明中可用的平纹棉麻织物层为纺粘非织造层，但可自非织造纤维等的梳理纤网制成。对一些过滤器应用而言有用的平纹棉麻织物层需要足够的刚度以保持折叠和死褶。
本文中用到的术语“纵向”或“MD”指织物在生产其的机器上被生产的长度方向。术语“横向”或“CD”指织物的宽度，即通常垂直于MD和纤网厚度方向的方向。
本文中用到的术语“泊松比”为横向上织物尺寸稳定性的量度。泊松比越低，织物的尺寸稳定性越好。特别地，泊松比为宽度与长度的相对改变的量度。织物的尺寸稳定性越好，织物在转化方法过程中“颈缩”的倾向越小。泊松比(PR)为无量纲数，通过下式计算：
PR＝{(W0-Wi)/W0}/{(Li-L0)/L0}；
其中W0为初始样品宽度，Wi为伸长长度Li下的样品宽度，L0为初始样品长度，L0的值是四(4)乘W0值的最小值，Li为给定伸长下的样品长度。
“足迹(footprint)”是当其通过两个压延辊之间时被压的纤网区域。足迹可由纤网沿纤网CD的任何点在MD上被压的长度量度。
“熔化区域”指肉眼或显微照片中可见并包含已熔合进彼此中而失去其各自形状的纤维的纤网区域，无论是否穿越整个纤网。例如在两个硬的不锈钢辊间压延的纳米纤网的显微照片在纤维已熔合进彼此中而形成粘合且纤维已失去其纤维特性的地方示出斑点。图2示出了这类显微照片的实例，在其中可以看到熔化的区域，其中纤维基本上彼此熔合。
“粘性粘结”指材料被引进纤网中，在热的作用下或除去溶剂时其在选定区域中将纤维粘结在一起。
“离散的不连续粘结区域”指纤网平面中这样的区域，其中分离的纤维在某些点处彼此粘结，所述区域不形成一个自纤网的任何一个边缘向另一边缘伸展的连续区域。
“离散的不连续未粘结区域”指纤网平面中这样的区域，其中分离的纤维在任何点处均未彼此粘结，所述区域不形成一个自纤网的任何一个边缘向另一边缘伸展的连续区域。
本文中用到的术语“纳米纤维”指数均直径或横截面小于约1000nm、甚至小于约800nm、甚至介于约50nm和500nm之间、甚至介于约100和400nm之间的纤维。本文中用到的术语直径包括非圆形状的最大横截面。
在第一个实施方案中，本发明涉及一种包含聚合物纳米纤维的非织造纤网，所述纤网的泊松比小于约0.8，甚至小于约0.3，甚至小于约0.2，甚至小于约0.1。
在另一实施方案中，本发明涉及一种非织造纤网，所述纤网任选具有离散的不连续粘结或未粘结区域，所述纤网在纤网平面中包含熔化区域的面积小于约15％，且所述纤网不是粘性粘结的。在其他实施方案中，所述非织造纤网在纤网平面中包含熔化区域的面积小于约10％、甚至小于约5％或甚至小于约1％。
本发明的改进的纳米纤网抵抗颈缩以致当在MD上施加100g/cm的张力时，所述改进的纳米纤网表现出的颈缩小于约10％，或甚至小于约5％，或甚至小于约2％，或甚至小于约1％。
本发明的非织造纤网的密实度可介于约10％到约80％之间，甚至介于约20％到约60％之间，甚至介于约20％到约40％之间，纤网的基重可至少为约1gsm，甚至至少约2gsm，甚至至少约5gsm，甚至至少约20gsm。在再一个实施方案中，所述非织造纤网的基重至少为约50gsm。
本发明的非织造纤网的最小厚度为约1微米，无最大厚度。在备选的实施方案中，所述厚度最大可为约800微米或甚至约400微米。
在本发明的又一实施方案中，所述非织造纤网可为任何上面提到的纤网，其MD断裂拉伸应力至少为约600psi(4.1MPa)，甚至至少约1000psi(6.9MPa)，甚至至少约2000psi(13.8MPa)，或MD拉伸模量至少为约10,000psi(69MPa)，甚至至少约20,000psi(138MPa)，甚至至少约40,000psi(276MPa)，或二者。
在再一实施方案中，所述非织造纤网可为任何上面提到的纤网，其表面稳定指数高于约1001bf/nch(17,513N/m)，或表面摩擦系数小于约0.9，或二者。
本发明的改进的纳米纤网以泡点(Bubble Point，BP)量度的最大孔径可在约0.1微米到约15微米范围内，甚至介于约0.5微米到约2.5微米之间，平均流量孔径(MFP)在约0.01微米到约5微米范围内，甚至介于约0.2微米到约3微米之间，或甚至介于约0.2微米和1.5微米之间。本发明的改进的纳米纤网的孔径分布的指示可由BP/MFP比率确定，其可在约1.1到约6范围内，甚至约1.1到约4。
所述初生非织造纤网主要或只包含通过电纺如经典电纺或电喷及在某些情况下通过熔喷方法产生的纳米纤维。经典电纺这种技术在美国专利4,127,706中示出，该专利通过全文引用结合到本文中，其中向溶液中的聚合物上施加了高压以产生纳米纤维和非织造毡。但电纺方法中的总生产能力太低以致在形成较高基重的纤网时不具有工业可行性。
“电喷”方法在国际专利公开号WO 03/080905中有公开，其通过全文引用结合到本文中。包含聚合物和溶剂的聚合物溶液流从储罐被送到喷丝头内的一系列纺丝喷嘴中，喷嘴上施加了高电压且聚合物溶液通过其释放。同时，任选被加热的压缩空气从布置在纺丝喷嘴侧面或外围的空气喷嘴流出。所述空气通常作为吹扫气流向下导入，其包围和运送新流出的聚合物溶液并帮助形成纤网，所述纤网被收集在真空室上方接地的多孔收集带上。电喷方法可以较短的时间形成工业规模和数量的纳米纤网，基重超过约1gsm，甚至高达约40gsm或更高。
基材或平纹棉麻织物可布置在收集器上以收集和合并基材上纺成的纳米纤维纤网以便合并的纤维纤网可用作高性能过滤器、擦拭物等。基材的实例可包括各种非织造布如熔喷非织造布、针刺或水刺非织造布、织造布、针织布、纸等，并可无限制地使用，只要基材上可加上纳米纤维层即可。
可使用如下电喷工艺条件来制造本发明的纤网。
施加到喷丝头上的电压优选在约1-300kV范围内，更优选约10-100kV。聚合物溶液可以约0.01-200kg/cm2、优选约0.1-20kg/cm2的压力释放。这使聚合物溶液可以适当的方式大量释放以便实现大规模生产。本发明的方法可以约0.1-5cc/min-孔的释放速率释放聚合物溶液。
通过空气喷嘴注入的压缩空气的流率为约10-10,000m/min，优选约100-3,000m/min。空气温度优选约300℃，更优选约100℃。模头与收集器距离(DCD)即纺丝喷嘴下端与真空收集器间的距离优选为约1-200cm，更优选10-50cm。
可用来形成本发明的纳米纤网的聚合物材料不受特别限制，包括加聚物和缩聚物材料如聚缩醛、聚酰胺、聚酯、聚烯烃、纤维素醚和酯、聚硫醚、聚芳醚、聚砜、改性聚砜聚合物及其混合物。这些上位类型中的优选材料包括聚(氯乙烯)、聚甲基丙烯酸甲酯(和其他丙烯酸类树脂)、聚苯乙烯和其共聚物(包括ABA型嵌段共聚物)、聚(偏氟乙烯)、聚(偏氯乙烯)、交联和非交联形式的各种水解度(87％-99.5％)的聚乙烯醇。优选的加聚物倾向于玻璃质的(Tg高于室温)。对于聚氯乙烯和聚甲基丙烯酸甲酯、聚苯乙烯聚合物组合物或合金，情况就是这样，或对于聚偏氟乙烯和聚乙烯醇材料，结晶度低。一类优选的聚酰胺缩聚物为尼龙材料如尼龙-6、尼龙-6，6、尼龙6，6-6，10等。当本发明的聚合物纳米纤网通过熔喷形成时，能被熔喷成纳米纤维的任何热塑性聚合物均可使用，包括聚烯烃(如聚乙烯、聚丙烯和聚丁烯)、聚酯(如聚对苯二甲酸乙二醇酯)和聚酰胺(如上面列出的尼龙聚合物)。
为降低纤维聚合物的Tg，向上述各种聚合物中添加本领域熟知的增塑剂可能是有利的。适宜的增塑剂将取决于待电纺或电喷的聚合物以及取决于纳米纤网将引入到的具体的最终用途。例如，尼龙聚合物可用水或甚至从电纺或电喷工艺留下的残余溶剂增塑。可用来降低聚合物Tg的本领域熟知的其他增塑剂包括但不限于脂族二醇、芳族磺酰胺、邻苯二甲酸酯，所述邻苯二甲酸酯包括但不限于选自邻苯二甲酸二丁酯、邻苯二甲酸二己酯、邻苯二甲酸二环己酯、邻苯二甲酸二辛酯、邻苯二甲酸二异癸酯、邻苯二甲酸二(十一烷醇)酯、邻苯二甲酸二(十二烷醇)酯和邻苯二甲酸二苯酯等的那些。George Wypych，2004，Chemtec Publishing编辑的Handbook of Plasticizers(增塑剂手册)(通过引用结合到本文中)公开了可用于本发明中的其他聚合物/增塑剂组合。
本发明的初生纳米纤网可被压延以赋予物理性质的所需改进。在本发明的一个实施方案中，初生纳米纤网被送进两个无图案辊间的辊隙中，在所述两个无图案辊中，一个辊为无图案的软辊，一个辊为无图案的硬辊，硬辊的温度保持在Tg与Torn之间的温度下，以便当通过压延机辊隙时纳米纤网的纳米纤维处于增塑状态下，其中所述Tg在本文中定义为聚合物进行从玻璃态向橡胶态的转化的温度，所述Torn在本文中定义为聚合物开始熔化的温度。可改变辊的组成和硬度以产生所需的最终用途性质。在本发明的一个实施方案中，一个辊为硬金属如不锈钢，另一个辊为硬度低于Rockwell B 70的软金属或涂布了聚合物的辊或复合辊。纤网在两辊间的辊隙中的停留时间通过纤网的线速度控制，所述线速度优选介于约1m/min和约50m/min之间，两辊间的足迹为纤网行进与两辊同时接触的MD距离。足迹由施加在两辊间的辊隙上的压力控制，通常以力每辊的线性CD尺寸量度，优选介于约1mm和约30mm之间。
此外，所述非织造纤网可被拉伸，任选同时加热到纳米纤维聚合物的Tg与最低Torn之间的温度下。拉伸可在纤网被送到压延辊处之前和/或之后在MD或CD中的任一个或两个方向上进行。
试验方法
表面稳定指数(Surface Stability Index，SSI)是被拉拔时纤网表面的纤维脱离的趋势的量度。纤网的表面稳定指数通过如下技术测定。将磁棒置于伸长计(MTS QUESTTM 5)上的下安装点中。将约4”x 6”的钢板置于磁铁之上。在钢板上牢固地粘附一片双面胶带，所述胶带宽约2.5”，长约3”。在双面胶带上轻轻但平整地放上一片至少2”x 2”的待试材料。小心不要破坏受试材料的表面；避免起皱和折叠。
试验探头为钢筒，其末端直径为5/8”(面积＝1.23in2)。在该探头的末端覆盖一片同样的双面胶带，且胶带切割为与探头相适应。将探头安装在伸长计滑动横梁上的50N压力传感器中。降低滑动横梁以便探头停留在样品表面上方500μm-1000μm处。将该起始点指定为零伸长。
让探头以0.050in/min的连续速率向下(向着样品)行进。探头继续下行直至样品与探头间产生了0.5lbs的法向力。探头在此位置保持10秒。然后使探头反向行进并以0.010in/min的连续速率离开样品。该动作继续到滑动横梁达到其起始点为止。
从数据中提取出试验的卸载部分载荷＝0轴附近载荷对伸长曲线的斜率。斜率计算的起点指定为尽可能靠近载荷＝0轴，优选载荷值为正的点。终点沿卸载曲线的线性部分选取，选取点与起点的距离应超过10μm(伸长后)。试验软件自动地为起点和终点间的数据拟合最小二乘法线性趋势线，趋势线的斜率以lb/in(N/m)给出。斜率的绝对值记录为SSI。
测定在给定样品的各面上进行两次，但试样不重复使用(即试验是破坏性的)。每次测定后更换两片胶带(样品板和探头上)。对四个试样值取平均得到样品的表面稳定值。
平均流量孔径和泡点按ASTM Designation E 1294-89，“StandardTest Method for Pore Size Characteristics of Membrane Filters UsingAutomated Liquid Porosimeter(用自动液体孔率计测试薄膜过滤器的孔径特性的标准方法)”测定，其用来自ASTM Designation F 316的自动泡点法用毛细管流量孔率计(型号CFP-34RTF8A-3-6-L4，PorousMaterials，Inc.(PMI)，Ithaca，NY)大致测定孔径直径0.05μm到300μm的膜的孔径特性。用低表面张力流体(表面张力为16达因/厘米的1，1，2，3，3，3-六氟丙烯或“Galwick”)润湿各样品(直径8、20或30mm)。将各样品置于支架上并施加空气差压而从样品中除去流体。湿流量等于干流量(无润湿溶剂时的流量)的一半时的差压用来计算平均流量孔径，计算使用所提供的软件进行。泡点指最大孔径。
基重(BW)按ASTM D-3776(其通过引用结合到本文中)测定，单位为g/m2(gsm)。
密实度用样品的基重(g/m2)除以聚合物密度(g/cm3)和样品厚度(微米)再乘以100计算，即密实度＝基重/(密度x厚度)x100％。％孔 隙度＝100％-％密实度。
纤维直径的测定如下。对每一细纤维层样品获取十份扫描电镜(SEM)图像(放大5,000倍)。从照片上测定十一(11)条可清楚分辨的细纤维的直径并记录。不包括缺陷(即细纤维的块、聚合物滴、细纤维的交叉点(intersection)。计算各样品的平均纤维直径。
厚度按ASTM D-645(或ISO 534)(其通过引用结合到本文中)在50kPa的外加载荷和200mm2的砧表面积(anvil surface)下测定。厚度以密耳给出并换算为微米。有机电解质中的离子电阻为隔离物阻抗离子流动的量度，其测定如下。将样品切成小块(直径1.5cm)并浸泡在2M的LiCl/甲醇电解质溶液中。隔离物电阻用Solartron 1287电化学界面测试仪和Solartron 1252频率响应分析仪及Zplot软件测定。试验传感器(cell)的电极面积为0.3165平方厘米，该电极面积与湿隔离物接触。测定在10mV的AC振幅和10Hz-500,000Hz的频率范围下进行。Nyquist曲线中的高频截距为隔离物电阻(单位ohms)。用隔离物电阻(ohms)乘电极面积(0.3165平方厘米)得到离子电阻(单位ohms-cm2)。
MacMullin数(Nm)为无量纲数，其为隔离物的离子电阻的量度，定义为充满电解质的隔离物样品的电阻率与相等体积的电解质的电阻率的比率。其由下式表示：
Nm＝(R隔离物×A电极)/(ρ电解质×t隔离物)，
其中R隔离物为隔离物的电阻(单位ohms)，A电极为电极面积(单位cm2)，ρ电解质为电解质的电阻率(单位ohms-cm)，t隔离物为隔离物的厚度(单位cm)。2M的LiCl/甲醇电解质溶液在25℃下的电阻率为50.5ohms-cm。
拉伸模量在伸长计(MTS QUESTTM 5)上以每分钟伸长2英寸的恒定速率测定。将样品切成1英寸×8英寸的尺寸(负载方向上较长)。样品的标距长度为6英寸，样品的起始宽度为1英寸。拉伸模量(也称弹性模量、杨氏模量)定义为与应力-应变曲线的低应变部分相切的线的斜率。样品在纵向和横向两个方向上测试。
抗张强度在伸长计(MTS QUESTTM 5)上以每分钟伸长2英寸的恒定速率测定。将样品切成1英寸×8英寸的尺寸(负载方向上较长)。样品的标距长度为6英寸，样品的起始宽度为1英寸。抗张强度定义为试样承受的最大载荷除以其横截面积(A＝宽度×厚度)。样品在纵向和横向两个方向上测试。
颈缩描述当在纵向施加拉伸载荷时样品宽度(横向)减小的程度。此试验在伸长计(MTS QUESTTM 5)上进行，为非标准试验。样品的伸长以0.5mm的间隔增加，每次增加时记录载荷和宽度数据。宽度总在试样上最窄点处测定。样品的标距长度为6英寸，样品的起始宽度为2英寸。以％宽度(定义为测得的宽度÷起始宽度×100％)对线张力(定义为载荷÷起始宽度)作图。对该数据拟合出截距＝100％的三次多项式，颈缩值为该多项式在100g/cm下的值。泊松比用相同的测定程序测定。
静态摩擦系数用Testing Machines Incorporated (Amityville，NY)的32-25型摩擦系数测试仪按TAPPI方法T503测定。将样品安装在倾斜面上，配对的样品安装在2.5”正方形金属滑片(sled)的底部。金属滑板上连接有导电性的折翼，所述折翼安装进倾斜面左端的电路中。倾斜面的右端有电机，所述电机以1.5+/-0.5度每秒的速率增大倾斜面相对于水平面的仰角。当金属开始折翼移动时，倾斜面左端的开关断开，电机停止。记录倾斜面所保持的角度。静态摩擦系数即为该角度的正切。
实施例
该实施例所用样品自Torn为约215℃的聚酰胺(尼龙-6，6)纺得。在实施例1-3中，通过自解卷机向两辊压延机辊隙传递纳米纤维片材压延数均纤维直径为约717微米、目标基重为约18gsm的初生纳米纤维片材。使用辊压前铺展片材的设备使片材在进入辊隙时保持平整、无皱纹。硬辊为直径9.76英寸(24.79厘米)的钢辊，软辊为Shore D硬度为约85、直径约10.5英寸(26.67厘米)的尼龙表面辊。
图3a示出了通过本发明的方法获得的典型纤网的实例的显微照片，其中各纤维虽然变平(flattened)了(图3b)但未彼此熔合成非纤维物质而是保留了其纤维性质。
对比例1
对比例1为未经压延的纳米纤网(图1)。其最大孔径为约7微米，平均流量孔径为约3微米。
实施例1
片材的卷绕速度为10ft/min(3.05m/min)，硬辊的温度为80℃。辊隙中的压力通过12.64mm的辊隙足迹记录。压延后片材在辊隙出口处以62.5g/cm的张力拉伸。加工得到的纳米纤网的最大孔径为约2.6微米，平均流量孔径为约1.0微米。
实施例2
片材的卷绕速度为10ft/min(3.05m/min)，硬辊的温度为50℃。辊隙中的压力通过12.64mm的辊隙足迹记录。压延后在辊隙出口处以62.5g/cm的张力拉伸片材。加工得到的纳米纤网的最大孔径为约2.7微米，平均流量孔径为约1.1微米。
实施例3
按实施例2制备和压延纳米纤网，但在辊隙出口处以198g/cm的张力拉伸片材。加工得到的纳米纤网的最大孔径为约2.3微米，平均流量孔径为约0.9微米。
对比例2
自熔体流动速率(MFR)为1200g/10分钟的聚丙烯(Basell，Wilmington，DE)X11292-36-6制备平均纤维直径为0.85μm的17gsm熔喷纤网。
对比例3
自聚丙烯(Basell，Wilmington，DE)PF017(2000MFR，涂布过氧化物)制备平均纤维直径为0.94μm的17gsm熔喷纤网。
结果
表1示出了自实施例1-3和对比例1获得的结果。表1中的数据表明，与对比例1的初生纳米纤网相比，经历本发明的压延方法的纳米纤网在泊松比和耐颈缩性方面有大幅改进。
表1
  样品   基重(gsm)   抗张强度(MPa)   模量(MPa)   100g/cm下的颈缩(％)   PR   密实度(％)
  对比例1   15.81   3.5   32.5   12.35   0.99   17.3
  实施例1   17.05   9.3   155.5   1.05   0.19   34.74
  实施例2   17.21   8.0   205.1   1.65   0.29   34.13
  实施例3   15.08   8.9   151.3   0.65   0.14   31.65
按上面的描述对实施例2和4的样品测定表面稳定性，以对比例1作为对照。也测试对比例2和3。表2表明，通过本发明的方法，表面稳定性取得了改进。
表2
 样品   表面稳定性(N/m)
 对比例1   2140
 实施例1   84629
 实施例3   82267
 对比例2   10021
 对比例3   1993
表3中示出了本发明的产品摩擦系数的改进。
表3
 样品   摩擦系数
 对比例1   1.042
 实施例1   0.881
 实施例2   0.580
 实施例3   0.636
表4中示出了本发明的产品的离子电阻。有意义的是通过如实施例1和2所示的本发明的方法后与对比例1相比电阻未增加或其增加仅可忽略不计的事实。同样有意义的是离子电阻可通过在如实施例3和对比例1中所示压延前或后拉伸纤网而显著改变。如实施例3中所示，与对比例1相比，本发明的纤网更坚固、具有更好的表面稳定性、且仍具有较低的离子电阻。
表4
 样品   离子电阻(Ohm.cm2)
 对比例1   0.855
 实施例1   0.857
 实施例2   1.175
 实施例3   0.774

Claims (31)

1.一种包含聚合物纳米纤维的非织造纳米纤网，所述纤网的泊松比小于约0.8，密实度至少为约20％，基重至少为约1gsm，厚度至少为约1μm。
2.权利要求1的非织造纳米纤网，所述纤网任选具有离散的不连续粘结或未粘结区域，所述纤网在纤网平面中包含熔化区域的面积小于约15％，且所述纤网不是粘性粘结的。
3.权利要求2的非织造纳米纤网，所述纤网在纤网平面中包含熔化区域的面积小于约1％。
4.权利要求1的非织造纳米纤网，所述纤网的基重小于约50gsm。
5.权利要求1的非织造纳米纤网，其中所述泊松比在纤网纵向上施加的张应力下测得。
6.权利要求1的非织造纳米纤网，所述纤网为经压延的纤网。
7.权利要求1的非织造纳米纤网，所述纤网的最大孔径为约0.1μm到约15μm，平均流量孔径为约0.01μm到约5μm。
8.权利要求1的非织造纳米纤网，所述纤网在2M的氯化锂/甲醇电解质中的电阻小于或等于约2ohms-cm2，MacMulin数为2-15。
9.权利要求1的非织造纳米纤网，当在纤网的纵向上施加100g/cm的张力时，所述纤网在横向上的颈缩小于约20％。
10.权利要求1的非织造纳米纤网，所述纤网的表面稳定指数大于约17.513N/m。
11.权利要求1的非织造纳米纤网，所述纤网的摩擦系数小于约0.9。
12.权利要求1的非织造纳米纤网，所述纤网在纵向上的拉伸模量至少为约69MPa。
13.权利要求1的非织造纳米纤网，所述纤网在纵向上的断裂拉伸强度至少为约4.1MPa。
14.一种非织造纳米纤网，所述纤网通过包括以下步骤的方法形成：经第一辊和第二辊间的辊隙压延聚合物纳米纤网、向纤网的厚度上对纤网施加压力并加热纤网至纳米纤网聚合物的Tg与其Torn间的温度，其中所述第一辊和第二辊中的一个为硬辊，另一个辊为硬度低于Rockwell b 50的软辊，其中所述经压延的纳米纤网在纤网平面中包含熔化区域的面积低于约15％。
15.权利要求14的非织造纳米纤网，所述纤网的泊松比小于约0.8，密实度至少为约20％，基重至少为约1gsm，厚度至少为约1μm。
16.权利要求14的非织造纳米纤网，所述纤网的最大孔径为约0.1μm到约15μm，平均流量孔径为约0.01μm到约5μm。
17.权利要求14的非织造纳米纤网，所述纤网在纵向上的拉伸模量至少为约69MPa，在纵向上的断裂拉伸强度至少为约4.1MPa。
18.一种稳定化聚合物纳米纤网的表面的方法，所述方法包括经第一辊和第二辊间的辊隙压延纳米纤网、在纤网的厚度上施加压力和加热纤网至纳米纤网聚合物的Tg与其Torn间的温度，其中所述第一辊和第二辊中的一个为硬辊，另一个辊为硬度低于Rockwell B 50的软辊。
19.权利要求18的方法，其中所述硬辊包含凸起区域，所述凸起区域在纳米纤网上形成粘结区域的图案。
20.权利要求18的方法，其中所述硬辊是无图案的。
21.权利要求18的方法，所述方法还包括在压延前或后于所述温度下在纵向和/或横向上拉伸所述纳米纤网。
22.一种包含聚合物纳米纤维的非织造纳米纤网，所述纤网的密实度至少为约20％，基重至少为约1gsm，厚度介于约1μm和400μm之间，最大孔径为约15微米，其中所述纳米纤网在纤网平面中包含熔化区域的面积小于约15％。
23.权利要求22的非织造纳米纤网，其中所述最大孔径介于约0.1微米到约15微米之间，所述纤网的平均流量孔径介于约0.01微米到约5微米之间。
24.权利要求23的非织造纳米纤网，所述纤网的最大孔径/平均流量孔径比率介于约1.1到约6之间。
25.权利要求22的非织造纤网，所述纤网的密实度介于约20％到约80％之间。
26.权利要求25的非织造纤网，其中所述密实度介于约20％到约40％之间。
27.一种包含聚合物纳米纤维的非织造纳米纤网，所述纤网的密实度至少为约20％，基重至少为约1gsm，厚度介于约1μm和400μm之间，纵向上的断裂拉伸强度至少为约4.1MPa，其中所述纳米纤网在纤网平面中包含熔化区域的面积小于约15％。
28.权利要求27的非织造纳米纤网，所述纤网在纵向上的拉伸模量至少为约69MPa。
29.权利要求1、14、22或27中任一项的非织造纳米纤网，所述纤网还包含与所述非织造纤网以面对面的关系结合的第二纤网，其中所述第二纤网选自一种或多种纳米纤网、平纹棉麻织物和层压于一起的前述的任意组合。
30.一种过滤介质，所述过滤介质包含权利要求1、14、22或27中任一项的非织造纳米纤网。
31.一种用于储能设备的隔离物，所述隔离物包含权利要求1、14、22或27中任一项的非织造纳米纤网。
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