CN101821448A - 纤维结构和制备该纤维结构的方法 - Google Patents
纤维结构和制备该纤维结构的方法 Download PDFInfo
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- CN101821448A CN101821448A CN200880104867A CN200880104867A CN101821448A CN 101821448 A CN101821448 A CN 101821448A CN 200880104867 A CN200880104867 A CN 200880104867A CN 200880104867 A CN200880104867 A CN 200880104867A CN 101821448 A CN101821448 A CN 101821448A
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- nanofiber
- oxide
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- fibre
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Abstract
提供了纤维结构和制备该纤维结构的方法。纤维结构包括超细纤维结构,超细纤维结构在其上具有纳米纤维。通过将前体溶液进行电纺丝以形成前体纳米纤维来形成纳米纤维。经电纺丝的前体纳米纤维置于超细纤维结构上并与超细纤维结构熔合。在一个优选实施方式中,硅石纳米纤维形成在玻璃超细纤维上并与该玻璃超细纤维熔合。
Description
相关申请的交叉引用
当前申请要求2007年7月27日递交的第60/952,363号美国临时申请的优先权,该临时申请的全部内容明确地并入本文。
技术领域
本发明涉及包括超细纤维和纳米纤维的纤维结构、以及制备该纤维结构的方法。
背景技术
目前将纤维用作对金属、陶瓷或聚合物成分的加强件。这些纤维实际上可包括任何成分。通常的纤维包括但不限于:由多种成分制成的玻璃纤维,如E玻璃和S玻璃;有机聚合物纤维,如芳纶、聚酯、聚烯烃、尼龙、聚砜、和聚酰亚胺;金属纤维,如不锈钢、钢、铝、硅、和由多种成分制成的合金;陶瓷纤维,如碳化硅、氮化硅、氮化铝、和金属氧化物;以及其它无机纤维,如碳和硼。
用于加强件的典型纤维被制备为具有微米级直径并在本文中称为超细纤维。通常,超细纤维是机织的,尽管其在使用时可以是非机织的。连续超细纤维无论是机织还是非机织的均用于增加强度和模量。然而,当将超细纤维用于增强基体材料时,各向异性、应力集中和局部非均匀性仍是问题。这些问题有时使自身表现为位于其所嵌入的基体中的相对轻微的局部破裂,从而当合成物用作装置的一部分时导致恶劣的装置效率,或者当合成物用于要求承载、气体/液体密封、和电气/热隔绝特性中的一个或组合的应用时导致过早失效。
发明内容
根据本发明的一个实施方式,提供了一种形成纤维结构的方法,该方法包括:获得超细纤维结构;以及在该超细纤维结构上形成纳米纤维。
根据本发明的另一实施方式,提供了一种纤维结构。该纤维机构包括超细纤维结构。该超细纤维结构在其上具有纳米纤维。
通过在以下所提供的详细描述,本发明适用性的其它部分会变得显而易见。应该理解,详细描述和具体示例尽管对本发明的优选实施方式进行了说明,但是仅出于说明且不会限制本发明的范围。
附图说明
通过详细描述和附图可以更加完全地理解本发明,在附图中:
图1是一般地示出加强纤维结构方法的流程图;
图2是示出位于超细纤维结构上的经电纺丝的纳米纤维前体的、放大250倍的扫描式电子显微镜照片;
图3是位于超细纤维结构上的经电纺丝的纳米纤维前体的、放大10,000倍的扫描式电子显微镜照片;
图4是位于超细纤维结构上的经电纺丝的纳米纤维的、放大20,000倍的扫描式电子显微镜照片;
图5是位于超细纤维结构上的经电纺丝的纳米纤维的、放大250倍的扫描式电子显微镜照片;
图6是位于超细纤维结构上的经电纺丝的纳米纤维的、放大1,000倍的扫描式电子显微镜照片;以及
图7是图示对纳米纤维进行电纺丝的一种方法的示意图。
优选实施方式详述
优选实施方式的以下描述本质上仅是示例性的且绝不会对本发明、本发明的应用、或用途进行限制。
根据本发明的一个实施方式,提供了一种纤维结构,该纤维结构包括在超细纤维结构上的纳米纤维。用于制备这种纤维结构的方法的实施方式一般包括获得超细纤维结构、和在纤维结构上形成纳米纤维。如图1所示,该方法一般地由在10处的流程图说明。在12处混合起始材料。接着在14处对起始材料进行加热以形成前体溶液。接着在16处将前体溶液转化为前体纳米纤维。接着在18处将前体纳米纤维形成为纳米纤维。
本发明的一个实施方式可用于将硅石(silica)纳米纤维形成在超细纤维结构上,本文将该实施方式进行具体描述。超细纤维结构可以是主要由具有微米级直径的纤维构成的任何众所周知类型的纤维结构。众所周知,超细纤维结构通常用作很多金属、陶瓷或聚合物合成物的加强件。同样地,超细纤维可以是连续或非连续的。超细纤维结构可以随机取向。可以理解,尽管超细纤维结构中大多数纤维具有微米范围内的直径,但是超细纤维结构中一些个别纤维可能并不处于微米范围内。然而,优选地,纤维的平均直径处于微米范围内。
如上所述,超细纤维结构的纤维可包括主要由平均为微米级尺寸的纤维制成的任何适当机织或非机织纤维结构。作为非限制性示例,适当的纤维可包括:由多种成分制成的玻璃纤维,如E玻璃和S玻璃;有机聚合物纤维,如芳纶、聚酯、聚烯烃、尼龙、聚砜和聚酰亚胺;金属纤维,如不锈钢、钢、铝、硅、和由多种成分制成的合金;陶瓷纤维,如碳化硅、氮化硅、氮化铝、和金属氧化物;以及其它无机纤维,如碳和硼。
根据本发明的一个实施方式,纳米纤维被形成并被置于超细纤维结构上,优选地紧固于该超细纤维结构。纳米纤维可包括可被制备为具有纳米级平均尺寸的纤维的、任何适当材料。作为非限制性示例,纳米纤维可以是:聚合物,例如,聚苯乙烯、PVP、聚酰亚胺、聚酯、聚丙烯腈、聚酰胺、聚倍半硅氧烷、聚硅氧烷、PVC、PVDC、PTFE、聚丙烯酸酯、聚酯、聚砜、聚烯烃、聚氨基甲酸脂、聚倍半硅氧烷、聚硅氧烷、环氧聚合物、氰酸酯、BMI、聚酮、聚醚、聚胺、聚磷腈、聚硫化物、有机\无机杂化聚合物;无机氧化物,如二氧化硅、锌氧化物、铝氧化物、锡氧化物、铅氧化物、二氧化钛、镁氧化物、钙氧化物、钠氧化物、钾氧化物、锂氧化物、铟氧化物、锰氧化物、铜氧化物、钴氧化物、铁氧化物、铈氧化物、锑氧化物、硼氧化物、铍氧化物、锆氧化物、和混合金属氧化物;陶瓷,如碳氧化硅、氮氧化硅;或金属。通过将纳米纤维置于超细纤维上,提供了包括超细纤维和纳米纤维的混合纤维加强结构。
纳米纤维的使用在尺寸、取向、纤维密度和分布方面有利于微米级尺寸的纤维。纳米纤维的使用还允许依据对纤维成分和形态的选择而引入附加功能的自由。因此,可将纳米纤维选择为优化纤维结构的纤维强化特性,包括但不限于机械特性、电气特性、磁特性、和热转变特性。在一个实施方式中,可将纳米纤维置于纤维结构的低纤维目的区域中。
作为非限制性示例,一个适当的纳米纤维包括待置于玻璃超细纤维结构上的硅石纳米纤维。在以下的描述中陈述并在图2-6的扫描式电子显微镜(SEM)照片中示出了制备硅石纳米纤维的示例。
为了根据示例制备硅石纳米纤维,将16.23g甲基三甲氧基硅烷(MTMS)加入三口圆底烧瓶中,该三口圆底烧瓶配备有机械搅拌器、温度计、冷凝器、和Dean Stark分离器。在搅拌的同时加入120g正丁醇和7g去离子水。正丁醇和去离子水是溶剂。接着,加入0.03g三氟甲磺酸。三氟甲磺酸起到催化剂的作用。在不加热或冷却的情况下搅拌混合物30分钟。接着将该混合物的温度升高到70℃并保持在70℃一个小时。将温度进一步升高以在冷凝器的作用下收集挥发成分。到达最终温度120℃。此时,监测到烧瓶中的残留溶液的固体含量。一旦达到约8个重量百分比的固体的浓度,则停止加热。该步骤产生中间预聚物溶液。
接着,将15g预聚物中间溶液与0.5g聚乙烯吡咯烷酮(PVP)混合。在腕摇动器上连续地摇动该混合物,直到PVP完全溶解以形成前体溶液。添加PVP以增加粘度,从而允许纳米纤维前体溶液14的电纺丝。纳米纤维前体溶液的室温粘度约为100厘泊。
接着将该纳米纤维溶液14形成为前体纳米纤维16。以如下方式制备前体纳米纤维16。在图7中示意性地示出了用于对前体纳米纤维进行电纺丝的一个实施方式。将前体溶液置于包括塑料注射器的容器20中,塑料注射器安装在注射器泵22上。注射器泵22与具有钝的端部的吸液不锈钢针24接合。针具有0.05in.的末端外径、0.033in.的内径、和2in.的长度。平坦的不锈钢电极26置于在注射器针下方离针末端9cm的位置。电极26呈矩形并且尺寸为3in.×4in.。电极26是水平的,针与扁平的电极表面垂直。
将购自BGF工业的Style 106玻璃织物28用作超细纤维结构。将玻璃纤维28切割为矩形以及比平坦的不锈钢电极26略大的尺寸(未示出)。超细纤维结构是由具有约为6微米直径的玻璃纤维机织而成的机织结构。玻璃织物28片置于平坦的电极26上。横跨针和平坦的电极施加13.3kV的直流电压,并且针为负极,电极26为正极。只要一施加电压,注射器泵22就启动。泵送速度为5ml/hr。前体纳米纤维30从针末端被纺丝而出并被收集在紧接在正极上方的玻璃织物28上。将具有玻璃织物28的正极36移动到针的下方以均匀地分布前体纳米纤维30。使用总计50秒的纺丝时间。接着使具有前体纳米纤维30的玻璃织物28干燥。图2和3示出了不同放大倍数的位于玻璃织物28上的干燥的前体纳米纤维30的SEM照片。图2具有250倍的放大水平,图3具有10,000倍的放大水平。前体纳米纤维直径的范围从190nm到1200nm,平均直径为610nm。
接着在步骤18(图1)将前体纳米纤维30转换为硅石纳米纤维32并熔合到玻璃织物28。更具体地,将其上具有前体纳米纤维30的玻璃织物28(如图2和3所示)置于空气循环炉中并加热。将温度以每分钟5℃升高到575℃。接着,将温度保持在575℃5个小时。关闭热源,允许炉冷却。图4示出了经热处理的纤维的SEM照片。如图4所示,微米级尺寸的玻璃纤维28和经转换的纳米级尺寸的硅石纤维32均保持其形状。在加热后,经转换的硅石纳米纤维32的平均直径为490nm。这表示从前体纤维的610nm的平均值起的下降。该典型的纳米纤维能够具有0.5nm到10,000nm的典型直径。经转换的硅石纳米纤维32熔合为机织的玻璃织物28。
可以理解,本文提供了形成可根据本发明使用的一个具体类型的纳米纤维的一个具体示例。本领域技术人员容易理解,本文所描述的起始材料可以包括可用于制备纳米纤维的任何起始材料。作为非限制性示例,其它的起始材料可以包括:醋酸锌或AlCl、辛酸锌、钛酸丁酯、及其在浓缩的不同阶段的水解产物。
同样地,可以在本发明的情况下使用任何适当的溶剂、催化剂或流变性改变剂。因而,可以使用任何其他适当的溶剂来替代正丁醇或添加到正丁醇。其它的溶剂可以包括但不限于乙醇、甲醇、异丙醇、甲基异丁基酮、丙酮、甲苯、二甲苯、正己烷、庚烷、乳酸乙酯、乙酸乙酯、二乙醚等。使用其它溶剂可能影响溶液的挥发性,并且可能影响纤维的形态和尺寸。
此外,可以使用任何其它适当的流变性修改剂来替代PVP或添加到PVP。例如,还可以使用PVA。另外,可以在浓缩中调整流动改性剂以改变前体溶液的流变性。对流变性进行控制以提供可被进行电纺丝的前体溶液。
还可以对纳米纤维前体的加工参数进行调整。作为非限制性示例,可以调整泵送速度和纺丝时间。同样地,可以调整针(负极)与正极之间的距离。还可以调整跨过正极和负极的电压。可以理解,可以改变任何加工参数以对纳米纤维的尺寸、取向或特性进行优化。
以下的示例对改变加工参数的一个示例进行说明。以如上所述方式对前体溶液进行制备。加工与上述的相同,除了用于对前体纳米纤维进行纺丝的全部时间从50秒减少到25秒,意图降低纳米纤维的密度。图5和6示出了在575℃保持5个小时期间将前体纳米纤维转换为硅石纳米纤维32’之后、混合纤维网的不同放大水平的SEM照片。可以看到,与以上图4所示的示例相比,纳米纤维的密度降低了。经转换的硅石纳米纤维还可以良好地熔合在玻璃超细纤维上并跨过玻璃纤维之间的间隙。
如上所述,将超细纤维结构置于负极上并将纳米纤维纺丝在纤维结构上。优选地,正极可在电纺丝加工过程中移动到至少两个平面中(沿图7所示的装置的方向)。这样,可使正极移动并因此使超细纤维结构移动以对位于超细纤维结构上的纳米纤维选择性地进行取向和/或分布。这样允许对纳米纤维的放置进行控制。可以通过使用适当的控制器(未示出)实现正极的移动。因而,可对所提供的、包括超细纤维和纳米纤维的最终纤维结构进行设计以对最终纤维网的机械特性和其它特性进行优化。作为非限制性示例,可将纳米纤维至于纤维结构的低纤维密度区域中。
在如上所述的示例中,通过电纺丝产生纳米纤维。在示例中,纳米纤维是连续的。然而可以理解,在本发明的范围内可以预期制备纳米纤维的任何适当方法。此外,纳米纤维无需是连续的。此外,尽管在示例中将纳米纤维放置在超细纤维结构上,但是可以理解,可以在本权利要求书的范围内,将纳米纤维替换地或附加地放置在超细纤维下方或与超细纤维交叠。
本发明的描述本质上仅是示例性的,因此不偏离本发明要点的变体落入本发明的范围。不应将这些变体认为是本发明的精神和范围的偏离。
Claims (27)
1.一种形成纤维结构的方法,包括:
获得纤维结构;以及
在所述纤维结构上形成纳米纤维。
2.如权利要求1所述的方法,其中,形成纳米纤维的步骤包括:
制备纳米前体溶液、形成前体纳米纤维以及加热所述前体纳米纤维以形成所述纳米纤维。
3.如权利要求2所述的方法,其中,形成前体纳米纤维的步骤包括:
将所述纳米前体溶液电纺丝在所述纤维结构上。
4.如权利要求2所述的方法,其中,制备纳米纤维前体的步骤包括:
将甲基三甲氧基硅烷与溶剂和催化剂混合、以及加热该混合物以形成预聚物中间溶液。
5.如权利要求4所述的方法,其中,所述溶剂包括正丁醇。
6.如权利要求4所述的方法,其中,所述催化剂包括三氟甲磺酸。
7.如权利要求4所述的方法,其中,将所述混合物阶段性地加热到在环境温度以上的第一温度和在所述第一温度以上的第二温度。
8.如权利要求4所述的方法,其中,将所述前体中间溶液与聚乙烯吡咯烷酮混合,从而形成所述纳米纤维前体溶液。
9.如权利要求3所述的方法,其中,电纺丝的步骤包括:
将电极定位在注射器针的末端下方并与所述末端间隔开;
将所述纤维结构放置在所述电极上;
跨过所述针和所述电极施加电压;以及
泵送所述前体溶液穿过针的所述末端,从而在所述纤维结构上形成前体纳米纤维。
10.如权利要求9所述的方法,还包括:
在形成所述前体纳米纤维同时使所述电极移动,以对将所述前体纳米纤维应用在所述纤维结构上进行控制。
11.如权利要求9所述的方法,还包括:
对其上具有所述前体纳米纤维的超细纤维进行加热,以形成所述纳米纤维并将所述纳米纤维与所述纤维结构熔合。
12.如权利要求1所述的方法,其中,所述纤维结构包括实质上的超细纤维结构。
13.如权利要求1所述的方法,其中,所述纤维结构是机织纤维。
14.如权利要求1所述的方法,其中,所述纳米纤维是连续的。
15.如权利要求1所述的方法,其中,所述纳米纤维是随机取向的。
16.如权利要求1所述的方法,其中,所述纳米纤维置于所述纤维结构的低纤维密度区域中。
17.一种纤维结构,包括:
超细纤维结构;以及
纳米纤维,布置在所述超细纤维结构上。
18.如权利要求17所述的纤维结构,其中,所述纳米纤维基本上包括聚合物、无机氧化物、陶瓷、金属或其组合。
19.如权利要求18所述的纤维结构,其中,所述聚合物纳米纤维包括聚苯乙烯、PVP、聚酰胺、聚丙烯腈、聚酰亚胺、PVA、PVC、PVDC、PTFE、聚丙烯酸酯、聚酯、聚砜、聚烯烃、聚氨基甲酸脂、聚倍半硅氧烷、聚硅氧烷、环氧聚合物、氰酸酯、BMI、聚酮、聚醚、聚胺、聚磷腈、聚硫化物、有机\无机杂化聚合物、或其组合。
20.如权利要求18所述的纤维结构,其中,所述无机氧化物纳米纤维包括硅氧化物、锌氧化物、铝氧化物、锡氧化物、铅氧化物、钛氧化物、镁氧化物、钙氧化物、钠氧化物、钾氧化物、锂氧化物、铟氧化物、锰氧化物、铜氧化物、钴氧化物、铁氧化物、铈氧化物、锑氧化物、硼氧化物、铍氧化物、锆氧化物、或其组合。
21.如权利要求18所述的纤维结构,其中,所述超细纤维结构包括无机超细纤维。
22.如权利要求17所述的纤维结构,其中,所述纳米纤维与所述超细纤维结构熔合。
23.如权利要求22所述的纤维结构,其中,所述纳米纤维被电纺丝在所述超细纤维上。
24.如权利要求17所述的纤维结构,其中,所述超细纤维是机织纤维。
25.如权利要求17所述的纤维结构,其中,所述纳米纤维是连续的。
26.如权利要求17所述的纤维结构,其中,所述纳米纤维是随机取向的。
27.如权利要求17所述的纤维结构,其中,所述纳米纤维置于所述纤维结构的低纤维密度区域。
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US95236307P | 2007-07-27 | 2007-07-27 | |
US60/952,363 | 2007-07-27 | ||
PCT/US2008/071064 WO2009018104A2 (en) | 2007-07-27 | 2008-07-24 | Fiber structure and method of making same |
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EP (1) | EP2173943A4 (zh) |
JP (1) | JP2010534579A (zh) |
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- 2008-07-24 EP EP08782331A patent/EP2173943A4/en not_active Withdrawn
- 2008-07-24 WO PCT/US2008/071064 patent/WO2009018104A2/en active Application Filing
- 2008-07-24 KR KR1020107001874A patent/KR20100050490A/ko not_active Application Discontinuation
- 2008-07-24 JP JP2010518391A patent/JP2010534579A/ja not_active Withdrawn
- 2008-07-24 US US12/670,749 patent/US20100210159A1/en not_active Abandoned
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CN103451774A (zh) * | 2013-09-12 | 2013-12-18 | 上海大学 | 利用静电纺丝工艺制备铟酸钙(CaIn2O4)纳米棒的方法 |
CN109455982A (zh) * | 2018-12-24 | 2019-03-12 | 安徽省淮阜路桥工程建设有限公司 | 路桥施工用沥青混凝土及其制备方法 |
CN109455982B (zh) * | 2018-12-24 | 2021-09-03 | 安徽省淮阜路桥工程建设有限公司 | 路桥施工用沥青混凝土及其制备方法 |
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JP2010534579A (ja) | 2010-11-11 |
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EP2173943A4 (en) | 2012-08-29 |
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