CN1263596C - 形成导电聚合物纳米复合材料的方法和由其生产的材料 - Google Patents

形成导电聚合物纳米复合材料的方法和由其生产的材料 Download PDF

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CN1263596C
CN1263596C CNB028161157A CN02816115A CN1263596C CN 1263596 C CN1263596 C CN 1263596C CN B028161157 A CNB028161157 A CN B028161157A CN 02816115 A CN02816115 A CN 02816115A CN 1263596 C CN1263596 C CN 1263596C
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C-S·王
M·D·亚历山大
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Abstract

提供一种用碳纳米纤维增强聚合物材料的方法，其中碳纳米纤维与聚合物和聚合物用溶剂混合，形成基本上均匀的混合物，接着通过蒸发或凝固除去溶剂。所得导电聚合物纳米复合材料显示出高的导电率和导热率、提高的机械强度、抗磨性和尺寸稳定性。

Description

形成导电聚合物纳米复合材料的 方法和由其生产的材料
本发明针对均匀地掺入分散的蒸气-生长的碳纳米纤维的导电聚合物纳米复合材料，和针对形成这种纳米复合材料的方法。
蒸气-生长的碳纳米纤维是通过蒸气-相催化方法的变通方案生产的独特形式的碳，在该方法中，在小的金属催化剂颗粒存在下，热解含碳的原料。所得纳米纤维典型地具有60-200纳米的外径，30-90纳米的中空核和数量级为50-100微米的长度。
早已提出使用蒸气-生长的碳纳米纤维，用于提供聚合物改进的机械、电子和热传递性能。例如，通过其中机械地剪切开在聚合物母体内的分散剂的聚合物熔融共混方法，将蒸气-生长的碳纳米纤维分散在聚合物母体内。参见，例如美国专利No.5643502。然而，由于大多数聚合物与碳纳米纤维不相容，因此难以实现碳纳米纤维在聚合物母体内的均匀分散。另外，高剪切机械共混可导致碳纳米纤维的断裂。
因此，本领域仍需要用碳纳米纤维增强聚合物材料的改进方法，以生产在各种机械、电学和热性能上具有最大可获得改进的复合材料。
通过提供将蒸气-生长的碳纳米纤维均匀分散在聚合物母体内的方法，本发明满足了该需要，该方法提高了其机械强度、尺寸稳定性、抗磨性和导电与导热性。通过将聚合物溶解在含有纳米纤维的溶剂内，接着蒸发或凝固溶剂，来实现碳纳米纤维在聚合物母体内的均匀分散。
根据本发明的一个方面，提供一种形成掺有碳纳米纤维的导电聚合物纳米复合材料的方法，该方法包括提供蒸气生长的纳米纤维，纳米纤维与溶剂混合，以形成溶液混合物，和将聚合物加入到该溶液混合物中，形成基本上均匀的混合物。然后优选通过蒸发或凝固，从混合物中除去溶剂。
在本发明可供替代的实施方案中，该方法包括将碳纳米纤维、聚合物和溶剂混合，形成基本上均匀的混合物，接着除去溶剂。
本发明所使用的聚合物优选选自聚氨酯、聚酰亚胺、环氧树脂、硅氧烷聚合物或芳族杂环刚性棒状或梯形聚合物。溶剂优选选自二甲亚砜、四氢呋喃、丙酮、甲磺酸、多磷酸或N，N-二甲基乙酰胺。优选地，聚合物和用于该聚合物的溶剂都是极性的。
本发明所使用的碳纳米纤维可包括生成态(as-grown)纤维、热解裸(stripped)纤维或热处理纤维。
本发明方法产生导电聚合物纳米复合材料，其导电率可随所需应用从小于0.001S/cm调节到大于20S/cm。在导电聚合物纳米复合材料掺有热处理的碳纳米纤维的情况下，纳米复合材料可具有大于20S/cm的导电率，而掺有低浓度生成态或热解裸碳纳米纤维的材料可被调节到具有小于约10-6S/cm的导电率。
本发明形成的导电聚合物纳米复合材料优选具有小于1体积％碳纳米纤维的电子导电突增界限值。
可使用本发明方法形成的聚合物纳米复合材料形成导电油漆、涂料、填缝料、密封剂、捏和机、纤维、薄膜、厚片材、管道和大型结构部件。可使用在所得纳米复合材料内的碳纳米纤维给予这些产品机械强度、刚性、尺寸稳定性、导热性和摩擦性能。
可在各种各样的商业应用，包括航天空间、宇宙空间、电子、汽车和化学工业中使用该纳米复合材料。也可在电磁干扰屏蔽、电磁脉冲应用、电子信号传递、仪表板的静电上漆、静电放电和电光器件如光生伏打电池中使用该纳米复合材料。
因此，本发明的特征是提供一种形成导电聚合物纳米复合材料的方法，该方法导致碳纳米纤维在聚合物母体内的均匀分散。根据下述说明和所附的权利要求，本发明的其它特征和优点将变得显而易见。
我们早已发现，当使用相同用量的碳纳米纤维时，通过本发明方法生产的聚合物纳米复合材料的导电率比通过聚合物熔融共混方法生产的材料高2-3次方的数量级。我们也已发现，所得聚合物纳米复合材料具有小于1体积％碳纳米纤维的极低电子导电突增界限值，这是碳纳米纤维长径比极大的象征。这也表明本发明方法更有效地均匀分散碳纳米纤维到聚合物母体内，和与聚合物熔融共混方法相比，保持纳米纤维大的长度对直径的长径比。重要的是维持碳纳米纤维大的长径比，以给予最大可获得的增强，特别地对于诸如使用形成垫圈或密封结构用的弹性体聚合物之类的应用。
通过将聚合物溶解在含碳纳米纤维的溶剂内，本发明方法实现了蒸气-生长的碳纳米纤维在聚合物母体内的均匀分散。尽管碳纳米纤维单独不会很好地分散在有机溶剂内，但我们已发现，在聚合物存在下它们非常好地分散。因此，将碳纳米纤维与聚合物和溶剂混合，接着蒸发或凝固溶剂，形成导电聚合物纳米复合材料。在除去溶剂之后，可通过常规的挤出和模塑技术，在没有丧失其导电率的情况下，将聚合物纳米复合材料进一步加工成各种形状。
与已有的熔融共混方法相比，本发明方法提供的优点在于使用低温溶液方法来分散碳纳米纤维。该方法不要求聚合物熔体在升高的温度下高剪切混合，而高剪切混合典型地降低碳纳米纤维的长径比并导致劣化的增强作用。
另外，可通过使用不同类型和用量的碳纳米纤维来调节所得聚合物纳米复合材料的机械和热传递性能。例如，在EMI屏蔽应用中，所得导电率应当大于1S/cm。对于仪表板的静电上漆来说，所需的导电率为约10-4-10-6S/cm，和对于静电放电应用来说，为约10-8-10-10S/cm。
本发明中使用的优选聚合物包括极性聚合物，然而，应当理解，可在本发明中使用任何极性聚合物，只要它可溶于溶剂中。优选的聚合物包括聚氨酯、聚酰亚胺、环氧树脂、硅氧烷聚合物和芳族-杂环刚性-棒状和梯形聚合物。优选的聚氨酯包括热塑性聚氨酯。本发明中使用的优选梯形聚合物是聚(苯并咪唑基苯并菲咯啉)(BBL)。聚合物的存在浓度优选为至少10wt％，然而，应当理解，聚合物的浓度可随所得复合材料的所需性能和应用(如涂料)而变化。
本发明中使用的溶剂是极性溶剂，和包括二甲亚砜、丙酮、四氢呋喃、N，N-二甲基乙酰胺、甲磺酸和多磷酸。
优选根据美国专利No.6156256制备本发明所使用的碳纳米纤维，在此引入其参考。可在本发明中使用数类碳纳米纤维，其中包括生成态纤维、热解裸纤维和热处理纤维。热处理纤维是指通过缓慢加热纤维到3000℃，然后缓慢冷却纤维而充分石墨化的纳米纤维。已发现，当热处理碳纳米纤维时，表面化学-蒸气-沉积的碳的数量级高度增加，从而导致显著地改进的机械、电子和热传递性能。热处理的碳纳米纤维的导电率接近于高度有序的热解石墨，和导热率是铜的5倍。在希望高导电率和低碳纳米纤维负载的应用中优选热处理纤维。
优选在密闭容器内，优选通过在溶剂内混合碳纳米纤维和所需的聚合物，来进行本发明的方法。尽管优选在添加聚合物之前将碳纳米纤维分散在溶剂内，但也可同时混合纳米纤维、聚合物和溶剂。可根据所需应用进一步加工所得纳米复合材料。例如，可将材料形成为薄膜，其中所述薄膜是在低于溶剂沸点的温度下，通过蒸发溶剂，从溶液混合物中流延而得。或者，可通过在形成为膜或纤维的溶液混合物中凝固，接着浸渍在非溶剂如水中，以凝固膜，从而除去溶剂。也可通过旋涂和浸涂方法，将溶液混合物形成为薄膜。也可通过喷涂或沉积或通过挤出或模塑干燥的复合材料，将溶液混合物形成为大型部件如厚的片材或仪表板。
为了更容易地理解本发明，参考下述实施例，这些实施例打算描述本发明，而不是限制其范围。
实施例1
通过在密闭容器内，在10g二甲亚砜内混合0.2g生成态碳纳米纤维和1g热塑性聚氨酯，从而制备溶液混合物。采用磁搅拌棒搅拌混合物。通过在约80℃的温度下，在热板上蒸发溶剂，从溶液混合物中流延薄膜。进一步在80℃的真空烘箱内，在减压下干燥所得聚合物纳米复合膜。该膜具有16.7wt％和11.7体积％的碳纳米纤维并显示出0.25S/cm的导电率。
实施例2
通过在密闭容器内，在10g二甲亚砜内混合0.2g热处理碳纳米纤维和1g热塑性聚氨酯，从而制备溶液混合物。采用磁搅拌棒搅拌混合物。通过在约80℃的温度下，在热板上蒸发溶剂，从溶液混合物中流延薄膜。进一步在80℃的真空烘箱内，在减压下干燥所得聚合物纳米复合膜。该膜具有16.7wt％和10.2体积％的碳纳米纤维并显示出5.5S/cm的导电率。在100％伸长率下(拉伸到其起始长度的2倍)，该膜保留了1.3S/cm的导电率。
实施例3
使用实施例1和2所述的方法，在四氢呋喃(THF)中制备热塑性聚氨酯和热处理的碳纳米纤维的一系列溶液混合物。在室温下，通过蒸发溶剂，从溶液混合物中流延薄膜。下表1示出了所得膜的导电率值。
表1与热处理的碳纳米纤维浓度有关的聚氨酯纳米复合膜的导电率
 纳米纤维(g)  聚氨酯(g)   THF(g)   Wt％   Vol.％   导电率(S/cm)
 0.020  1.00   10.0   1.96％   1.12％   0.0038
 0.040  1.00   10.0   3.85％   2.22％   0.10
 0.080  1.00   10.0   7.41％   4.34％   0.54
 0.120  1.00   10.0   10.7％   6.37％   1.14
 0.160  1.00   10.0   13.8％   8.31％   3.93
 0.200  1.00   10.0   16.7％   10.2％   4.69
 0.240  1.00   10.0   19.4％   12.0％   8.70
 0.280  1.00   10.0   21.9％   13.7％   16.6
 0.320  1.00   10.0   24.2％   15.4％   20.8
对比例4
通过熔融共混方法制备纳米复合材料，其中在Haake Rheomixer中，在150℃下，混合20g热处理的碳纳米纤维和100g热塑性聚氨酯2小时。利用热将所得复合材料压成薄膜。膜具有16.7wt％的浓度和10.2体积％的碳纳米纤维，并显示出0.0052-0.0098S/cm的导电率。可看出，这些导电率值比实施例1-3制备的含相同浓度的碳纳米纤维的纳米复合膜低2-3次方的数量级。
实施例5
由在N，N-二甲基乙酰胺(DMAC)中的溶液混合物制备聚酰亚胺/酰氨酸和热处理的碳纳米纤维的纳米复合材料。在密闭的玻璃容器中，通过在10.0g DMAC中混合0.202g热处理的碳纳米纤维和1g聚酰亚胺/酰氨酸来制备溶液混合物。通过在60℃下蒸发溶剂，由溶液混合物制备薄膜。进一步在200℃的真空烘箱中干燥膜2小时。该膜具有16.8wt％的碳纳米纤维浓度和显示出1.7-2.8S/cm的导电率。
实施例6
使用实施例5中所述的方法，在10g DMAC中制备0.302g热处理的碳纳米纤维和1.0g聚酰亚胺/酰氨酸的溶液混合物。通过在60℃下蒸发溶剂，将溶液混合物流延成膜。进一步在200℃的真空烘箱中干燥膜2小时。该膜具有23.2wt％的碳纳米纤维浓度和显示出5.1-7.7S/cm的导电率。
实施例7
在密闭的玻璃容器中，通过在20g甲磺酸中混合0.02g热处理的碳纳米纤维和0.1g聚(苯并咪唑基苯并菲咯啉)(BBL)，来制备溶液混合物。用磁搅拌棒搅拌溶液混合物，然后在玻璃载片上将其刮涂成膜，并浸渍在水中，使纳米复合膜凝固。然后在室温下空气干燥该膜。该膜具有16.7wt％的碳纳米纤维浓度和1.0S/cm的导电率。
实施例8
将11g环氧树脂与1g早已预浸渍在46g四氢呋喃(THF)内的热处理的碳纳米纤维混合，通过机械搅拌形成均匀混合物。然后将2.86g固化剂加入到该混合物中。通过蒸发除去THF，和在150°F下固化复合材料1小时并在250°F下固化又一小时。所得热固性复合材料含有6.77wt％的碳纳米纤维和0.5S/cm的导电率。
已详细地并参考其优选实施方案描述了本发明，但显而易见的是，可在没有脱离本发明的范围情况下，作出改性和改变，而本发明的范围由所附的权利要求来定义。

Claims (11)

1.一种形成掺有碳纳米纤维的导电极性聚合物碳纳米复合材料的方法，该方法包括：
提供蒸气生长的碳纳米纤维；
将所述碳纳米纤维与极性溶剂混合，形成溶液混合物；
将极性聚合物加入到所述溶液混合物中，形成基本上均匀的混合物；和
从所述混合物中除去所述极性溶剂。
2.权利要求1的方法，其中通过蒸发除去所述极性溶剂。
3.权利要求1的方法，其中通过凝固除去所述极性溶剂。
4.权利要求1的方法，其中所述极性聚合物选自聚氨酯、聚酰亚胺、环氧树脂、硅氧烷极性聚合物或芳族杂环刚性棒状或梯形极性聚合物。
5.权利要求1的方法，其中所述极性溶剂选自二甲亚砜、四氢呋喃、丙酮、甲磺酸、多磷酸或N，N-二甲基乙酰胺。
6.权利要求1的方法，其中所述碳纳米纤维选自生成态纤维、热解裸纤维或热处理纤维。
7.权利要求1的方法，该方法包括将所述混合物流延成膜。
8.权利要求1的方法形成的其中掺有碳纳米纤维的导电极性聚合物碳纳米复合材料。
9.一种形成掺有碳纳米纤维的导电极性聚合物碳纳米复合材料的方法，该方法包括：
提供蒸气生长的碳纳米纤维；
提供极性聚合物；
将所述碳纳米纤维和所述极性聚合物与极性溶剂混合，形成基本上均匀的混合物；和
从所述混合物中除去所述极性溶剂。
10.一种形成掺有碳纳米纤维的导电极性聚合物碳纳米复合材料的方法，该方法包括：
提供蒸气生长的碳纳米纤维；
将所述碳纳米纤维与极性溶剂混合，形成溶液混合物；
将极性聚合物加入到所述溶液混合物中，形成基本上均匀的混合物；和
从所述混合物中除去所述极性溶剂；其中所述碳纳米复合材料具有小于1体积％所述碳纳米纤维的电子导电突增界限值。
11.一种形成掺有碳纳米纤维的导电极性聚合物碳纳米复合材料的方法，该方法包括：
提供蒸气生长的碳纳米纤维；
将所述碳纳米纤维与极性溶剂混合，形成溶液混合物；
将极性聚合物加入到所述溶液混合物中，形成基本上均匀的混合物；和
从所述混合物中除去所述极性溶剂；其中所述碳纳米复合材料具有在1.96wt％碳纳米纤维下，0.0038S/cm的导电率，到在24.2wt％的碳纳米纤维下，大于20S/cm的导电率。
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