CN110997268A - 复合材料的制造方法及复合材料 - Google Patents

复合材料的制造方法及复合材料 Download PDF

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CN110997268A
CN110997268A CN201980003682.2A CN201980003682A CN110997268A CN 110997268 A CN110997268 A CN 110997268A CN 201980003682 A CN201980003682 A CN 201980003682A CN 110997268 A CN110997268 A CN 110997268A
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resin
composite material
fiber
prepreg
producing
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武内幸生
秋山胜德
森岛骏一
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Mitsubishi Heavy Industries Ltd
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Abstract

本发明的目的在于提供使层间强度提高的复合材料的制造方法。本发明是将使未固化的基质树脂含浸于纤维增强基材而得到的多个预成型料(10)层叠、并进行加热成型的复合材料的制造方法，该方法包括：使用预成型料(10)，所述预成型料(10)具备不包含基质树脂且沿面内方向连续的空隙层(12)、及配置于空隙层的两面的树脂层(11a、11b)，在相邻的预成型料(10)与预成型料(10)的对置面配置多个短纤维(13)，将层叠后的预成型料(10)抽真空，使空隙层(12)脱气后，进行加热成型。

Description

复合材料的制造方法及复合材料
技术领域
本发明涉及复合材料的制造方法及复合材料。
背景技术
在飞机、船舶、车辆等领域中，广泛使用了纤维增强塑料(FRP:Fiber ReinforcedPlastics)制的复合材料作为结构体(专利文献1)。与金属相比，复合材料聚有“轻且坚固”的优点。FRP是由增强纤维和基质树脂构成的材料。
作为使用了FRP的复合材料的制造方法，已知有如下方法：将干燥增强纤维配置于成型模具中，注入基质树脂，使该基质树脂含浸于增强纤维并进行成型的方法；以及，将预成型料层叠并进行成型的方法。
在专利文献1中，使用将多张由增强纤维丝条形成的增强布帛层叠而形成的层叠体，利用前者的方法制造了复合材料。
后者中使用的“预成型料”是使未固化的树脂含浸于增强纤维中、并在中途停止树脂的固化反应而变得易于操作的片状的中间材料。在任意方向上层叠该预成型料，并在高压釜中进行加压固化成型的方法是可靠性最高且获得高品质的方式。
在使用了复合材料的结构部件的强度设计中，针对不同载荷的输入状态另行进行了静态强度评价及准静态强度评价。准静态强度评价中重要的评价指标是断裂韧性(以下简称为韧性)。在后者的情况下，韧性通过在任意方向上粘贴朝向任意方向的纤维增强预成型料并使其固化而得到的试验片来进行评价。
现有技术文献
专利文献
专利文献1：日本特开2003-80607号公报
发明内容
发明所要解决的课题
如上所述，复合材料包含层叠的纤维增强层(增强布帛或预成型料)。在将纤维增强层层叠而成的成型品中，纤维增强层与纤维增强层之间(层间)的韧性低。因此，成型品在层间产生裂纹而破坏的情况较多。裂纹的发展方向多数情况下为纤维增强层的面内方向S。
作为提高层间的韧性的方法，可列举出以下(1)～(3)。
(1)使弹性体粒子分散于树脂本身。
(2)将热塑性树脂导入层间。
(3)应用将纤维沿板厚方向取向的三维织物。
图3示出了在基质树脂中分散有弹性体粒子(橡胶粒子)21的复合材料20的厚度方向的剖面示意图。在分散有如弹性体粒子21那样的柔软材料的复合材料20中，在施加负载时，弹性体粒子21裂开，由于所产生的空隙而出现树脂能够发生变形的空间。由此，图3的复合材料20能够剪切变形并吸收破坏能量。另一方面，在分散弹性体粒子21的情况下，由于对弹性体粒子21的粒度及分散状态进行管理及后续需要韧性提高剂的添加工序，因此成本增高。另外，在基质树脂中添加弹性体粒子21时，基质树脂量相对减少，因此复合材料的强度降低。
图4示出了在纤维增强层31与纤维增强层31的层间导入了热塑性树脂32而得到的复合材料30的厚度方向的剖面示意图。被***的热塑性树脂32具有伸长率大且对热稳定的性质。层间的热塑性树脂32有助于提高复合材料的韧性。与图3的弹性体粒子21相比，热塑性树脂32使韧性提高的效果更高。另一方面，在导入热塑性树脂32的情况下，由于需要对热塑性树脂32的粒度及分散状态进行管理，因此成本增高。另外，存在因热塑性树脂32和基质树脂的热稳定状态而使升温速度等的限制严格等的问题。
图5示出了将增强纤维沿厚度方向T取向而成的三维织物的复合材料40的厚度方向的剖面示意图。由于将增强纤维沿厚度方向取向，因此层间韧性的加强效果高。另一方面，三维织物不仅比现有的织物在制造上成本更高，而且面内方向S的纤维取向减少，因此，作为复合材料40的强度降低。在三维织物中，沿厚度方向取向的纤维避开沿面内方向S取向的纤维束而配置。此时产生的纤维束的曲折及偏移可能成为使复合材料40的强度降低的因素。另外，三维织物通常在将纤维增强层调整为希望的形状后含浸树脂，难以采用使用了预成型料的方法。
本发明是鉴于这样的情况而完成的，其目的在于提供使层间强度提高的复合材料的制造方法。本发明的目的在于提供使层间强度提高且更廉价的复合材料。
用于解决课题的方法
为了解决上述课题，本发明的复合材料的制造方法及复合材料采用以下的方式。
本发明提供一种复合材料的制造方法，其是将使未固化的基质树脂含浸于纤维增强基材而得到的多个预成型料层叠、并进行加热成型的复合材料的制造方法，该方法包括：使用预成型料，所述预成型料具备不包含基质树脂且沿面内方向连续的空隙层、及配置于上述空隙层的两面的树脂层，在相邻的预成型料与预成型料的对置面配置多个短纤维，将层叠后的上述预成型料抽真空，使上述空隙层脱气后，进行加热成型。
本发明提供一种复合材料，其具备：多个纤维增强基材层叠而成的层叠体；上述层叠体中填充的固化后的基质树脂；以及朝向与上述纤维增强基材的面内方向不同的方向、且跨越邻接的上述纤维增强基材之间而存在的多个短纤维。
根据上述公开，配置于预成型料和预成型料之间的短纤维与基质树脂相接。短纤维随着被加热而能够流动的基质树脂流入空隙层而改变取向，朝向与纤维增强基材的面内方向不同的方向。由此，使短纤维跨越邻接的纤维增强基材之间。跨越邻接的纤维增强基材之间而存在的短纤维对邻接的纤维增强基材之间(层间)的接合进行加强。根据上述发明，可以获得与三维织物相同程度的层间加强效果。
与仅在一面设有树脂层的预成型料相比，在空隙层的两面设有树脂层的预成型料在层叠时的预成型料的定位性更好。
在上述发明的一个方式中，多个上述预成型料优选以将相同侧的面朝向相同方向进行层叠。由此，可以使多个层间的韧性为相同程度。
在上述发明的一个方式中，在配置于上述空隙层的两面的树脂层的厚度不同的情况下，优选将薄的树脂层朝向层叠方向来层叠多个上述预成型料。由此，容易使短纤维的取向朝向预成型料的厚度方向。
在上述发明的一个方式中，上述树脂层中含有的基质树脂优选包含热固性树脂，或者包含热固化树脂及其固化剂。
这里，“包含”除了“仅包含”这样的含义之外，还包括“不包含热塑性树脂、弹性体及韧性提高剂，而包含除此以外的添加物”的含义。“韧性提高剂”是：以丁腈橡胶为代表的橡胶类、与基质树脂具有相容性的热塑性树脂(例如，在基质树脂为环氧树脂时为聚醚砜)、与使交联点之间变长的长链状基质树脂或与基质树脂的相容性高的树脂、以层状存在氢键使剪切变形能力得到增强的苯并
Figure BDA0002375976180000041
嗪树脂类等。“除此以外的添加物”是指紫外线吸收剂、阻燃剂、增稠剂及粘度调节剂、内部脱模剂、润滑剂等。
不包含热塑性树脂、弹性体及韧性提高剂的热固性树脂比包含这些的热固性树脂更廉价。不包含韧性提高剂的热固性树脂由于交联密度高，因此固化温度接近玻璃化转变温度。不包含热塑性树脂、弹性体及韧性提高剂的热固性树脂由于未加入多余的添加物而固化反应简单，因此容易对具备空隙层的预成型料的制造及复合材料制造时的温度等进行管理。由此，用户可以根据用途选择基质树脂及增强纤维。
在上述发明的一个方式中，上述短纤维的长度为上述空隙层的厚度以上。由此，即使在基质树脂移动了空隙层厚度的量的情况下，只要短纤维沿预成型料的厚度方向取向，就能够跨越邻接的纤维增强基材之间而存在。
发明的效果
根据本发明，可以在不使用韧性提高类型的昂贵的预成型料的情况下，以低成本制造能够获得与三维织物相同程度的韧性提高效果的复合材料。
附图说明
图1是对本实施方式的复合材料的制造方法进行说明的图。
图2是本实施方式中使用的预成型料的厚度方向的剖面图。
图3是现有的复合材料的厚度方向的剖面示意图。
图4是现有的复合材料的厚度方向的剖面示意图。
图5是现有的复合材料的厚度方向的剖面示意图。
符号说明
10 预成型料(有空隙层)
10’ 预成型料(空隙层中已含浸有基质树脂)
11a、11b 树脂层
12 空隙层
13 短纤维
20、30、40 复合材料
21 弹性体粒子
31 纤维增强层
32 热塑性树脂
具体实施方式
本发明的复合材料的制造方法可适用于碳纤维增强塑料(CFRP)制的飞机的结构部件。具体而言，本发明的复合材料的制造方法适合用于要求施加冲击后残余强度的飞机的一次结构构件。另外，本发明的复合材料的制造方法也适用于虽然耐冲击的要求比一次结构构件低、但要求简便廉价地制造且进一步轻质化的飞机的二次结构构件(整流罩、动机舱罩等)。此外，本发明的复合材料的制造方法还可以适用于通常工业设备中要求冲击性的部件(例如，叉车、设置于火车站月台的站台门)。
首先，参照图1对本实施方式的复合材料的制造方法进行说明。在本实施方式中，将使未固化的基质树脂含浸于纤维增强基材而得到的多个预成型料10层叠，进行加热成型，制造复合材料。需要说明的是，图1中示例出将2个预成型料层叠的方法，但预成型料的层叠张数并不限定于此。
(预成型料层叠)
预成型料10使用在树脂层(11a、11b)之间具有空隙层12的半含浸预成型料。对于半含浸预成型料，在后面进行详细说明。在将预成型料10层叠时，在相邻的预成型料10与预成型料10的对置面配置多个短纤维13。在层叠后，多个短纤维13处于与预成型料10的基质树脂接触的状态。
短纤维例如是纳米纤维素纤维，厚度为10微米至100微米。短纤维例如是丙烯酸纤维、尼龙纤维、玻璃纤维等短纤维垫材料，以每单位面积的重量计为10g/m2至100g/m2。
例如，将短纤维13无规地撒在一个预成型料10的表面后，以夹住短纤维13的方式将另一个预成型料10层叠于一个预成型料10。在将2个以上的预成型料10层叠的情况下，只要按照以上所述将短纤维13的配置和预成型料10的层叠重复给定次数即可。
预成型料10具备具有树脂层11a的表侧面及具有树脂层11b的背侧面。多个预成型料10可以将全部相同侧的面朝向相同方向进行层叠。特别是在配置于空隙层12的两面的树脂层(11a、11b)的厚度不同的情况(在预成型料的厚度方向T上，空隙层12偏向于任一个预成型料10的情况)下，优选将薄的树脂层11b朝向层叠方向来层叠多个预成型料10。其中，仅在层叠的预成型料10为2个的情况下，使薄的树脂层11b对置进行层叠。“厚度不同”是指与树脂厚度相比时存在100μm以上的差异的情况。
在本实施方式中，预成型料的“厚度方向T”是与预成型料的面成基本以直角相交的方向，大致相当于与预成型料的层叠方向相同的方向。
(加热成型)
将层叠有多个预成型料10的层叠体包裹在真空袋膜(bagging film)(未图示)中并将内部抽真空，使空隙层12充分地脱气后，进行加热成型。
脱气在200mmHg以下、优选在150mmHg以下的真空度下进行。优选成型中始终进行抽真空，以使已脱气的气体不会返回至层叠体中。“充分地”是指10分钟以上。空隙层12本身作为脱气回路发挥作用。在脱气不充分的情况下，有时会堵塞脱气回路，因此不优选。
在将空隙层12充分脱气后开始进行加热。加热方式除了高压釜以外，还可使用烘箱或加热垫等。加热通过至少如下3个阶段来实施：第1加热，从常温升温至给定温度；第2加热，从给定温度升温至成型温度；第3加热，将成型温度保持给定时间而使基质树脂固化。
第1加热中的升温速度优选为10℃/分以下。第2加热中的升温速度优选为10℃/分以下。给定温度为100℃以上。成型温度是能够使基质树脂固化的温度。由于本实施方式中使用的预成型料不包含热塑性树脂及弹性体等添加物，因此上述成型温度及上述给定时间只要单纯基于基质树脂的特性即可。成型温度及给定时间可以是使用的基质树脂的制造商所推荐的条件。
基质树脂升温至给定温度时，基质树脂的粘度暂时降低而能够流动。粘度降低了的基质树脂流入空隙层12中，填埋纤维增强基材的空隙。与基质树脂相接的短纤维13伴随着基质树脂的流动而被带入邻近的纤维增强基材。由于基质树脂沿厚度方向流动，因此短纤维13也沿与预成型料10’的面内方向S不同的方向(主要为预成型料10’的厚度方向T)取向。
可以在基质树脂的粘度降低的时刻对预成型料10(例如，以2～3气压)进行加压。在进行加压时，调整加热温度使第2加热的升温速度不超过希望范围。通过加压，可以促进基质树脂流入空隙层12。
根据上述实施方式的方法，可以得到如下复合材料，所述复合材料具备：多个纤维增强基材层叠而成的层叠体、填充于层叠体中的固化后的基质树脂、以及朝向与纤维增强基材的面内方向不同的方向、且跨越多个纤维增强基材之间而存在的多个短纤维13。
沿与纤维增强基材的面内方向S不同的方向取向的短纤维13可以跨越多个纤维增强基材之间而存在。对于这样的复合材料而言，纤维增强基材与纤维增强基材之间(层间)的接合得到加强，结果是韧性提高。
接下来，对本实施方式的制造方法中使用的材料更详细地进行说明。
(纤维增强基材)
纤维增强基材为将纤维束沿一个方向(长度方向)对齐的单向材料、无纺布、织物等。纤维增强基材中使用的纤维为碳纤维、玻璃纤维、有机纤维、除玻璃以外的无机纤维等。纤维增强基材的厚度优选为0.05mm以上且0.5mm以下。
(基质树脂)
基质树脂使用高耐热的热固性树脂。高耐热的热固性树脂可以选自通常作为模具材料或夹具使用的树脂材料。具体而言，热固性树脂为环氧树脂、聚酯树脂、乙烯基酯树脂、氰酸酯树脂、聚酰亚胺树脂等。“高耐热”可以根据复合材料的应用来定义。例如，在飞机的结构构件的情况下，是指可耐受150℃以上的热。
在使用双组分混合型的热固性树脂时，基质树脂可以包含热固性树脂及其固化剂。基质树脂不包含热塑性树脂、弹性体、长链状树脂等。基质树脂可以包含内部脱模剂、阻燃剂、紫外线吸收剂、润滑剂等添加物。添加物的添加率低于基质树脂总量的20重量％，优选低于10重量％，进一步优选为0重量％。
采用耐热性高且硬的树脂时，在制造预成型料时容易残留空隙层12。通过采用耐热性高的树脂，使空隙层12在预成型料的保管中及复合材料的成型操作中也不易被压溃。与混入了弹性体及热塑性树脂的韧性提高类型的树脂相比，不包含热塑性树脂及弹性体的高耐热的热固性树脂更加廉价。
(预成型料)
预成型料是在纤维增强基材中含浸未固化的基质树脂而成的中间材料。图2示例出了本实施方式中使用的预成型料的厚度方向的剖面图。本实施方式中使用的预成型料10是半含浸预成型料。
半含浸预成型料具备空隙层12和配置于空隙层12两面的树脂层(11a、11b)。
空隙层12是由不包含基质树脂的纤维增强基材(未图示)构成的层。空隙层12在面内方向S上是连续的。空隙层12的厚度优选为0.1mm至1层厚度的一半。图2中的空隙层12的厚度为0.1mm。
树脂层(11a、11b)覆盖了纤维增强基材(空隙层12)的两面。树脂层(11a、11b)是由纤维增强基材及含浸于纤维增强基材的基质树脂构成的层。图2中的树脂层11a的厚度等于或大于空隙层的厚度。
半含浸预成型料可通过如下方式制造：将预先制作的基质树脂的膜粘贴于纤维增强基材的两面，抽真空并施加热，使基质树脂含浸于纤维增强基材，在基质树脂含浸于纤维增强基材整体之前，在基质树脂的凝胶点附近停止反应。
通过调节温度、抽真空的力、压力，可以在纤维增强基材的厚度方向上保留空隙(未含浸基质树脂的区域)。
在通过上述方法制造的半含浸预成型料中，如图2所示，空隙层12有时偏向于纤维增强基材的垂直下面侧而形成。这是由于，在预成型料的制造中，沿一个方向使纤维对齐时，将纤维位置固定，树脂仅快速含浸一面，因此一面的树脂含浸加深，结果是发生偏置。
通过使基质树脂中不包含热塑性树脂及弹性体等多余的添加物，能够使固化反应单纯地依赖于热固性树脂的性质。由此，使固化反应的管理变得容易，因此可以形成希望厚度的空隙层12。
(短纤维)
短纤维13只要是刚度柔软、且容易被带入基质树脂的流动中的纤维即可。具体而言，短纤维13为聚酰胺纤维(例如尼龙)、纤维素纤维、玻璃纤维、聚酯纤维等。
短纤维13的长度为空隙层的厚度以上。具体而言，短纤维13的长度为0.1mm以上。
短纤维13过粗时，难以被带入纤维增强基材内。短纤维13过细时，操作性降低。短纤维13过细时，加强效果降低。在常温下，预成型料表面有少许发粘。因此，只要是满足上述直径范围的短纤维13，就可以仅通过撒在预成型料表面而利用该粘性保持在预成型料表面。

Claims (6)

1.一种复合材料的制造方法，其是将使未固化的基质树脂含浸于纤维增强基材而得到的多个预成型料层叠、并进行加热成型的复合材料的制造方法，该方法包括：
使用预成型料，所述预成型料具备不包含树脂且沿面内方向连续的空隙层、及配置于所述空隙层的两面的树脂层，
在相邻的所述预成型料与所述预成型料的对置面配置多个短纤维，
将层叠后的所述预成型料抽真空，使所述空隙层脱气后，进行加热成型。
2.根据权利要求1所述的复合材料的制造方法，其中，将多个所述预成型料以相同侧的面朝向相同方向进行层叠。
3.根据权利要求1或2所述的复合材料的制造方法，其中，在配置于所述空隙层的两面的树脂层的厚度不同的情况下，将薄的树脂层朝向层叠方向来层叠多个所述预成型料。
4.根据权利要求1～3中任一项所述的复合材料的制造方法，其中，所述树脂层中含有的基质树脂包含热固性树脂，或者包含热固化树脂及其固化剂。
5.根据权利要求1～4中任一项所述的复合材料的制造方法，其中，所述短纤维的长度为所述空隙层的厚度以上。
6.一种复合材料，其具备：
多个纤维增强基材层叠而成的层叠体；
所述层叠体中填充的固化后的基质树脂；以及
朝向与所述纤维增强基材的面内方向不同的方向、且跨越邻接的所述纤维增强基材之间而存在的多个短纤维。
CN201980003682.2A 2018-05-18 2019-04-25 复合材料的制造方法及复合材料 Pending CN110997268A (zh)

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