CN102990999A - 具有改进的弯曲特性和表面特性的大丝束碳纤维复合物 - Google Patents

具有改进的弯曲特性和表面特性的大丝束碳纤维复合物 Download PDF

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CN102990999A
CN102990999A CN2011103841537A CN201110384153A CN102990999A CN 102990999 A CN102990999 A CN 102990999A CN 2011103841537 A CN2011103841537 A CN 2011103841537A CN 201110384153 A CN201110384153 A CN 201110384153A CN 102990999 A CN102990999 A CN 102990999A
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China
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carbon fiber
carbon
fiber composite
weight
resin
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姜铉旻
李相武
崔致勋
崔铁
朴相鲜
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Hyundai Motor Co
Kia Corp
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Hyundai Motor Co
Kia Motors Corp
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Abstract

本发明公开了一种碳纤维复合物，其包括30～80重量％的碳纤维织物，其中碳纤维丝束的尺寸是24K～100K；0.1～20重量％的碳无纺织物，其单位面积重量为10～500g/m2；和10～70重量％的聚合物树脂，其传送时的粘度为0.01～10Pa·s。有利地，可以通过选择性地将碳无纺织物应用到使用碳纤维复合物的材料表面上，以得到具有良好表面特性和弯曲特性的碳纤维复合物的成型产品。

Description

具有改进的弯曲特性和表面特性的大丝束碳纤维复合物
技术领域
本发明涉及一种碳纤维复合物，其中应用大丝束碳纤维来改进生产率和降低通过树脂传递成型法的碳纤维复合物成型工艺的成本，而且可以在改进与其应用引起的表面特性相关的问题的同时赋予复合物以良好的弯曲特性。
背景技术
与钢和轻金属相比具有极佳强度系数的碳纤维复合物通常仅被应用于需要特别坚固的轻质材料的军用设备和航空航天设备上。此外，其也因为其令人却步的昂贵成本而被应用于赛车或贵重车的底盘和车身部件上。然而，其应用的结果是燃料消耗的降低、耐腐蚀、冲击稳定性和由碳纤维轻质带来的灵活性。此外，由于其可塑性，其应用增加设计自由度。但是，对于汽车工业大规模生产的全面应用还没有实现，因为碳纤维复合物的低生产率和高成本。
最近，因为加强的环境规制和持续性的高油价，对于将碳纤维复合物应用到混合动力车和电动车的兴趣增加。在这些车辆上的使用将会降低车辆的总重量并降低所需的电池容量以及发动机尺寸，并同时增加驾驶性能和行驶范围。其应用也可以降低电池和发动机的价格。
因此，已经做出各种努力来解决生产率问题，而该问题是与其在大规模生产工业中的应用相关的最大问题之一，因为需要成型技术的发展来改进具有高强度/硬度和高品质的复合成型产品的生产率。对于可用作结构性材料的碳纤维复合物的一个成型方法是层压预浸料法。更具体地，树脂在高温/高压成型前进行预浸。
然而，该方法也因为其低生产率和高成本而逐渐被树脂传递成型(Resin Transfer Molding，RTM)法所替代。具体来说，是将具有一定形状的碳纤维织物放入模具中，并将热固性树脂传递到模槽中，之后将其在织物中浸透并同时硬化以得到成型产品。用于传递树脂的模具通常是具有高硬度的模具，但在大型成型产品的情况下，将柔性材料用于模具的一部分。
通常来说，也使用VaRTM(真空辅助树脂传递成型)法来减少树脂的传递时间。VaRTM对该方法中树脂进口的相对位置施加真空。然而，如果将柔性材料用于模具的一部分，树脂不能扩散至织物，因为树脂流因为模具与模塑材料的紧密接触而被阻断。
为了解决这些问题，通常使用作为树脂扩散媒介的网状薄片使树脂扩散变得容易。然而，该树脂扩散媒介通常从复合的成型产品中除去并处理掉。该树脂扩散媒介是有效扩散树脂所需要的，但是因为该媒介在模塑后去除会使生产成本增加并造成环境问题。
作为解决这些问题的一个方法，已经使用如下方法，即在例如聚氨酯成型剂的核心材料的表面形成用于树脂扩散的槽(日本专利第2000-501659号和日本专利第2001-510748号)。此外，作为相似技术，也已经在考虑如下方法，即在成型模具中形成用于树脂扩散的槽(日本专利申请公开第2001-62932号)。然而，这些方法并不解决应用大丝束碳纤维时引起的表面质量下降的问题。
通常来说，已经被应用到航空航天工业的碳纤维复合物是1～12K的小丝束[K是指1,000，12K是指组成12,000根具有7～10μm直径的纤维的一束碳纤维]，但是24K～50K的大丝束碳纤维在包括机动车的工业材料中的应用正日益成为需求。当使用大丝束碳纤维时，可以改进生产率，因为单位时间的生产容积增加，而成本也因大丝束碳纤维比小丝束碳纤维便宜而降低。因此，需要能提供良好表面特性的树脂传递成型法的方案，即使在需要大丝束碳纤维时。也需要该方法还具有增加的生产率和降低成本的能力。
发明内容
本发明提供一种复合物，其防止或显著降低当使用大丝束碳纤维的复合物时产生的表面质量下降，并在通过树脂传递成型法制备时改进生产率和降低成本。
一方面，本发明提供一种碳纤维复合物，由30～80重量％的碳纤维织物、0.1～20重量％的碳无纺织物、和10～70重量％的聚合物树脂构成，其中碳纤维的丝束大小是24K～100K。
本发明的以上和其他特征在下文中讨论。
附图说明
本发明的以上和其他特征将参考在附图中举例说明的其某些示例性实施方式来详细描述，该实施方式仅为说明的目的，并不意在限制本发明，其中：
图1是根据本发明的一个示例性实施方式的树脂传递成型法的示意图；
图2A、B是表示在应用根据本发明的一个示例性实施方式的组合物之前(A)或之后(B)的大丝束碳纤维复合物的平表面的图片；且
图3A、B是表示在应用根据本发明的一个示例性实施方式的组合物之前(A)或之后(B)的大丝束碳纤维复合物的弯曲部分的表面的图片。
列于附图中的参照数字包括对以下元件的参考，且这些元件在后面做进一步讨论：
应该理解的是，附图不必要成比例，而是呈现出阐明本发明基本原理的各种优选特征的略微简化的表示。本文中公开的本发明的具体设计特征包括，例如具体尺寸、取向、位置和形状，将部分地由特定的既定应用和使用环境来决定。
在附图中，所有附图的几个图中的参照数字是指本发明的相同的或等同的部件。
具体实施方式
在下文中详细参考本发明的各个实施方式，其实例在附图中示例并在下文中说明。尽管本发明将结合示例性实施方式进行说明，需要理解的是当前的描述并不意在将本发明限制于那些示例性实施方式。相反，本发明旨在不仅包括示例性实施方式，还包括各种替换方式、修改方式、同等方式和其他实施方式，其可以包括在所附权利要求所限定的本发明的精神和范围内。
应该理解的是，本文用到的术语“车辆”或者“车辆的”或其他类似术语一般包括机动车辆，例如载客汽车，包括运动型多功能车(SUV)、公共汽车、卡车、各种商用车；包括各种船和艇在内的水运工具；飞行器等，而且包括混合动力车、电动车、插电式混合电动车、氢动力车和其他替代燃料车(例如，从非石油类资源得来的燃料)。本文中提到的混合动力车是具有两种或更多种动力来源的车，例如同时为汽油动力和电动力的车。
本发明涉及一种碳纤维复合物，其是一种热固性碳纤维复合物，使用通过树脂传递成型法制备的大丝束碳纤维，具有良好的表面和弯曲特性。
根据本发明的一个特征的碳纤维复合物包括30～80重量％的碳纤维丝束尺寸为24K～100K的碳纤维织物、0.1～20重量％的单位面积重量为10～500g/m2的碳无纺织物、和10～70重量％的注射粘度为0.01～10Pa·s的树脂。该复合物的特征为良好的表面特征和弯曲特性，当通过树脂传递成型法制备复合物时选择性地将碳无纺织物应用到材料表面。
碳纤维可以是任何纤维，包括由聚丙烯腈(PAN)纤维、沥青纤维、人造丝纤维或木质素纤维制成的纤维。碳纤维可以通过将纤维与其他类型的纤维混合而制成，当两种或更多种纤维混合在一起时，除碳纤维以外的纤维例如玻璃纤维或聚芳基酰胺纤维可以一起使用。优选地，此碳纤维可以是具有良好物理特性例如强度和弹性模数以及与成本相平衡的PAN类碳纤维。总的来说，碳纤维用一种或更多种表面处理方法或材料进行操作。合适的表面处理方法是如下方法，其中碳纤维表面用合适的方法进行氧化，并用例如聚酰胺、氨基甲酸酯、和环氧树脂之类的材料涂布。通过合适方法进行的碳纤维表面的氧化可以通过引入能在之后表现出与涂布材料的良好粘合力的官能团来实现。这有助于改善纤维在组合物中的分散性。用于表面处理的涂布材料的量可以是碳纤维总重量的大约0.1～大约10重量％。
通过广角X射线散射(WAXS)测定的用于本发明的碳纤维的晶体尺寸优选在1～6nm的范围内。如果尺寸小于1nm，碳纤维本身的强度系数会因为碳纤维的碳化或石墨化不充分而降低。因此，在一些情况下，得到的成型产品的机械强度下降。然而，如果尺寸超过6nm，碳纤维本身的导电性因为碳纤维的充分碳化和石墨化而极佳，但是纤维脆弱且易损坏，因此并不优选具有良好的物理特性补偿效应，因为容易缩短成型产品中的纤维长度。尺寸可以在1.3～4.5nm的范围内，更优选1.6～3.5nm，最优选且具体为1.8～2.8nm。碳纤维的平均单根纤维直径在1～20μm的范围内，优选4～15μm，更优选5～11μm，最优选6～8μm。如果直径小于1μm，可能得不到所需的机械特性，如果超过20μm，强度系数补偿作用可能增加。
碳纤维的量可以优选为组合物总重量的大约30～大约80重量％，更优选为大约40～60重量％，甚至更优选为大约40～大约50重量％。如果量少于30重量％，可能得不到所需的机械强度，如果其超过80重量％，可能遭受到降低的成型性，因为模塑树脂不能完全浸渍硬化剂。因此难以制备足够轻的产品。
从生产率和降低成本的角度出发，碳纤维丝束的尺寸优选为24K～100K，更优选为30～70K，最优选为40～60K。如果尺寸小于24K，碳纤维在成本和生产率的方面可能没有竞争力，如果超过100K，因为低浸渍特性引起的大量起泡可能会破坏特性。
在本发明中，有三种碳纤维织物，例如平纹组织、斜纹组织和类似普通织物的缎纹组织，被称为三种基础编织法、或变成修饰或催生编织的基础的原始编织法。该原始编织可以通过其调整来修饰和应用到最终成型产品的详细说明中。
可被选择性地应用到复合物表面的碳无纺织物的单位面积的重量可以优选为10～500g/cm2，更优选为100～300g/cm2，最优选为150～200g/cm2。如果单位面积的重量小于10g/cm2，织物强度会因为其厚度变得太薄且其孔隙率变得太大而变低，从而在应用过程中不容易操作，而如果其超过500g/cm2，复合物本身的物理特性会因为产品过厚而严重降低。
碳无纺织物可以优选以复合物总重量的大约0.1～大约20重量％的量使用，更优选1～15重量％，最优选5～10重量％。如果量少于0.1重量％，很难实现表面和弯曲特性的强化。同时，如果其超过20重量％，不能得到所需的机械特性。
在本发明中，热固性树脂在其传送中的粘度可以优选0.01～10Pa·s，更优选约0.01～5Pa·s，最优选大约0.01～1Pa·s。如果传送中的树脂粘度小于0.01Pa·s，物理特性会降低，并在硬化过程中通过低分子成分的蒸发而产生气泡。相反，如果其超过10Pa·s，会产生气泡，因为在成型过程中树脂没有通过柔性的降低而完全浸渍，所以物理特性会变差。
在本发明中，树脂的量可以优选为10～70重量％，更优选为20～60重量％，最优选为25～50重量％。如果树脂量少于20重量％，特性会由于低浸渍特性而降低。相反，如果其超过70重量％，无法得到作为结构材料所需的机械特性。
以耐化学性、机械、热和电学特性、和耐环境性作为标准来选择适用的树脂。作为一个例子，当需要高度的和中度的耐化学性时，可以使用异邻苯二甲酸聚酯；当还需要高耐腐蚀性时，可以使用乙烯酯类的树脂；并且当需要高机械和热特性时，可以使用低粘度环氧树脂。除该组分外，本发明的组合物还可以包括阻燃剂、抗氧化剂、热稳定剂、润滑剂、染料、颜料和无机填充剂。
将组合物用于树脂传递成型法以提供成型的产品。该方法可以制备具有纤维增强复合物的各向异性的复杂三维结构，并具有显著的产品可靠性和再生产性特征，从而适合于复合部件的成型。此外，在大规模生产中，可以以低成本制备复杂的形状，且可以实现高度精密的产品。树脂传递成型法的进行是通过将增强纤维预成型体(pre-form)放入所需形状的模具中并通过进口将树脂传送到模具中，然后进行加热以成型。树脂传递成型(RTM)法具有模具制备、仪器和装置例如传送机等的低起始费用，因为它在比其他树脂传递成型更低的压力(例如，20～50psi)下运行。此外，简化了对于内部硬化剂和安装(例如用于其与其他部件连接的插入)的用量和方向的控制。
图1示出用于本发明的树脂传递成型法的示意图，从图示中可以看出，设置有一个孔口，用于在低压成型中将压力施加到树脂放入位点的相对侧以改善传递速率和质量。如图1所示，如上所述的碳无纺织物置于表面上以通过平顺树脂的流动来加强表面特性。根据产品的目的，在放置织物后可以将形状更改成覆盖上侧、下侧或整个碳纤维织物的形状。因此，当选择性地将碳无纺织物应用到部件的表面时，部件表现出良好的表面特性和极佳的抗弯强度/刚度。
如上所述制备的成型产品可以应用在具有显著降低的重量的电动汽车部件和结构/半结构材料上。优选的项目可以包括需要良好的表面质量和弯曲特性的备用轮胎底座、后挡板、和/或座架。
[实施例]
在下文中，提供以下实施例来进一步说明本发明，但是他们不应该被认为是对本发明的限制。以下实施例说明本发明，而并不意在限制本发明。
应用到本发明的实施例的方法在以下进行说明。
(1)弯曲特性的测定
抗弯强度和刚度是根据ASTM D790使用制备的测试片通过三点弯曲测试法测定，加载速度(cross-head rate)为2mm/min，结果列在表1中。在放置测试片时，其中碳无纺织物应用在测试片的一侧，将碳无纺织物侧朝上，并测定弯曲特性。
(2)拉伸性能的测定
根据ASTM D30309，通过使用制备的测试片来测试拉伸强度和刚度，加载速度为5mm/min，结果列在表1中。
(3)比重的测定
根据ASTM D792，通过使用制备的测试片来测定比重，结果列在表2中。
[比较例1]
本发明已经参考其示例性实施方式进行了详细说明。然而，本领域的技术人员应该意识到可以在这些实施方式中进行各种变化而不脱离本发明的原理和精神，其中本发明的范围由所附权利要求及其等效形式限定。
用于制备测试片的热固性树脂的制备是通过将低粘度环氧树脂(KFR-320(Kukdo Chemical Co.，Ltd.))与硬化剂(KFH-350(KukdoChemical Co.，Ltd.))混合，之后将脂肪族缩水甘油醚双功能稀释液以30重量％的量混合于其中以降低粘度。将单位面积重量为300g/m2的三层碳无纺织物放入制备模具中，然后如图1所示，在例如1～10torr的低压下进行树脂传递成型。硬化于60℃进行5小时，之后进一步于室温硬化24小时。结果，树脂含量为81重量％，碳无纺织物的含量是19重量％。测定测试片的比重、弯曲性能和拉伸性能并列在表1中。
[比较例2]
将两层的50K斜纹织物(2/2斜纹织物，Zoltek Corporation)放入制备模具中，然后如图1所示，于低压用树脂进行树脂传递成型，其中树脂和比较例1中制备的树脂相同。硬化于60℃进行5小时，之后进一步于室温硬化24小时。结果，树脂含量为31重量％，碳无纺织物的含量是69重量％。测定测试片的比重、弯曲性能和拉伸性能并列在表1中。
[实施例1]
将单位面积重量为300g/m2的一层碳无纺织物和一层的50K斜纹织物(2/2斜纹织物，Zoltek Corporation)如图1所示分层，然后如图1所示，于低压用树脂进行树脂传递成型，其中树脂和比较例1中制备的树脂相同。硬化于60℃进行5小时，之后进一步于室温硬化24小时。结果，树脂含量为54重量％，碳无纺织物的含量是46重量％。测定测试片的比重、弯曲性能和拉伸性能并列在表1中。
【表1】
Figure BDA0000113182320000081
如表1所示，根据本发明的用碳纤维复合物制备的实施例1具有增强的特性，例如相比于仅用碳无纺织物制备的测试片(比较例1)和仅用50K碳纤维斜纹织物制备的测试片(比较例2)，具有2倍或更多倍的抗弯强度以及3倍或更多倍的抗弯刚度。该效果可能是因为由本发明碳纤维复合物制备的测试片在其上部具有耐压缩力的结构以及在其下部具有耐拉伸力的结构，而当一定量或更大的力以垂直于测试片的方向产生作用以使其弯曲时，压缩力作用于测试片的上部，而拉伸力作用于测试片的下部。此外，如表1所示，根据本发明的复合物具有相对于仅由大丝束(50K)的碳纤维织物制备而来的测试片更低的比重，从而可以将其应用于需要极佳弯曲特性的超轻结构。
如图2所示，当使用大丝束碳纤维织物制备平坦测试片时，由碳纤维间隙处的树脂非浸渍或树脂收缩而产生压纹现象。通过使用根据本发明的碳纤维复合物没有导致相同的现象。此外，如图3所示，当具有弯曲的产品通过使用大丝束碳纤维进行成型时，树脂非浸渍发生在弯曲部分，但是当本发明的复合物应用于其上时，没有出现相同的现象。
根据本发明的碳纤维复合物有利地防止或降低表面特性的恶化以改进生产率和减少成本，其中所述恶化在用大丝束碳纤维复合物进行成型时发生，同时该复合物通过比重降低而具有弯曲特性的增强和变轻的作用。因此，根据本发明的碳纤维复合物可以为具有复杂形状的车辆结构或半结构的成型产品提供良好的弯曲和表面特性。

Claims (20)

1.一种碳纤维复合物，包括
30～80重量％的碳纤维织物，其中碳纤维丝束的尺寸是24K～100K；
0.1～20重量％的碳无纺织物；和
10～70重量％的聚合物树脂。
2.如权利要求1所述的碳纤维复合物，其中所述碳无纺织物位于所述碳纤维织物的表面。
3.如权利要求1所述的碳纤维复合物，其中所述碳无纺织物的单位面积重量在10～500g/m2的范围内。
4.如权利要求1所述的碳纤维复合物，其中所述聚合物树脂在其传送过程中的粘度在0.01～10Pa·s的范围内。
5.如权利要求1所述的碳纤维复合物，其中所述碳纤维织物具有平纹组织、斜纹组织或缎纹组织。
6.如权利要求1所述的碳纤维复合物，其中通过广角X射线散射法测定的所述碳纤维的晶体尺寸为1～6nm，平均单根纤维的直径在1～20μm的范围内。
7.如权利要求1所述的碳纤维复合物，其中还将玻璃纤维或聚芳基酰胺纤维混入所述碳纤维中。
8.如权利要求1所述的碳纤维复合物，其中将玻璃棉或不连续纤维无纺织物混合并应用到所述碳无纺织物中。
9.如权利要求3所述的碳纤维复合物，其中所述聚合物树脂包括异邻苯二甲酸聚酯、乙烯酯类树脂和低粘度环氧树脂。
10.如权利要求1所述的碳纤维复合物，所述碳纤维复合物还包括阻燃剂、抗氧化剂、热稳定剂、润滑剂、染料、颜料和无机填充剂。
11.一种车辆部件，由碳纤维复合物构成，其中所述碳纤维复合物包括：
30～80重量％的碳纤维织物，其中碳纤维丝束的尺寸是24K～100K；
0.1～20重量％的碳无纺织物；和
10～70重量％的聚合物树脂。
12.如权利要求11所述的车辆部件，其中所述碳无纺织物位于所述碳纤维织物的表面。
13.如权利要求11所述的车辆部件，其中所述碳无纺织物的单位面积重量在10～500g/m2的范围内。
14.如权利要求11所述的车辆部件，其中所述聚合物树脂在其传送过程中的粘度在0.01～10Pa·s的范围内。
15.如权利要求11所述的车辆部件，其中所述碳纤维织物具有平纹组织、斜纹组织或缎纹组织。
16.如权利要求11所述的车辆部件，其中通过广角X射线散射法测定的所述碳纤维的晶体尺寸为1～6nm，平均单根纤维的直径在1～20μm的范围内。
17.如权利要求11所述的车辆部件，其中还将玻璃纤维或聚芳基酰胺纤维混入所述碳纤维中。
18.如权利要求11所述的车辆部件，其中将玻璃棉或不连续纤维无纺织物混合并应用到所述碳无纺织物中。
19.如权利要求13所述的车辆部件，其中所述聚合物树脂包括异邻苯二甲酸聚酯、乙烯酯类树脂和低粘度环氧树脂。
20.如权利要求11所述的车辆部件，其中所述碳纤维复合物还包括阻燃剂、抗氧化剂、热稳定剂、润滑剂、染料、颜料和无机填充剂。
CN2011103841537A 2011-09-09 2011-11-28 具有改进的弯曲特性和表面特性的大丝束碳纤维复合物 Pending CN102990999A (zh)

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