CN102027051B - 预浸料的改进 - Google Patents
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Abstract
本发明提供一种预浸料,制备这种预浸料的方法,固化多个这种预浸料的层合体的方法,以及通过这种方法生产的固化的层合体,其中所述预浸料包括基质和纤维,其具有沉积在其上的多个区域,所述区域相对于所述基质的表面凸起至少5微米。
Description
技术领域
本发明涉及预浸料和多个这种预浸料的固化的层合体的改进,所述改进尤其是在减少这些层合体的孔隙率方面。
背景技术
大量文献记载了复合材料相对于传统结构材料的优点,尤其是在以非常低的材料密度提供优良的机械性质方面的优点。结果,这些材料的使用变得越来越广泛,它们的应用涉及到从“工业”和“运动和休闲”到高性能航天组件。
包括用树脂例如环氧树脂浸渍的纤维布置的预浸料宽泛地用于产生这些复合材料。通常,将许多层这些预浸料根据需要“层叠”,并使得到的层合体固化(通常通过暴露于升高的温度进行),得到固化的复合层合体。
这一工艺涉及到的一个危险是气体滞留在预浸料的各个层之间,这导致在所述固化的复合层合体中有不期望的孔隙率。孔隙率对所述固化的复合层合体的机械性质有负面影响,因此希望对孔隙率进行最小化或者消除。
已知,在固化过程中施加压力能够减小固化的层合体的最终孔隙率。如果期望低孔隙率的复合材料(例如对于要求苛刻的应用例如航空应用),那么长时间暴露于高温和高压,例如通过在高压釜中固化层合体,是唯一的实践选择。但是,用于长时间的高压和高温的应用是昂贵的和缓慢的。
涉及到较低压力的固化方法,例如已知的真空袋方法(vacuum bagprocess),是较便宜的和较快的选择,但是常常导致在固化的层合体中有较高的孔隙率。
因此,已经进行努力通过在固化之前调整层合体的结构来减少孔隙率。
US 5,104,718披露了预浸料的层合体,其中所述预浸料在所述预浸料内具有平行于所述单向纤维的纵向凹槽。
发明内容
一方面,本发明涉及预浸料,其包括树脂基质和纤维,所述预浸料具有沉积在其上的多个区域,所述区域相对于所述基质的表面凸起至少5微米。
在所述凸起区域沉积在所述基质的表面上时,不扰乱所述预浸料在沉积之前的结构,由此防止损害含在其中的纤维。因此,本发明的预浸料包括在表面上的树脂基质,在其上沉积了多个区域。与纤维表面相反,树脂表面提供了较光滑的、较平的表面,使得凸起区域(其本身可能是非常薄的)能够在层合的预浸料之间提供有效的间隔。
因此,第二方面,本发明提供处理包括基质和纤维的预浸料的方法,所述方法包括沉积多个相对于所述基质的表面凸起的区域。
当将根据本发明的预浸料“层叠”为预浸料的层合体时,所述凸起区域在接下来的固化过程中给任何滞留的气体提供从所述层合体流出的通道,在所述固化的层合体中得到较低的孔隙率。
此外,根据本发明的预浸料具有各种级别的悬垂性,柔性和粘性,使得它们能够以通常的方式使用,并且能够方便地和有效地用于形成结构体。
所述树脂通常包括热固性树脂,并且可选自本领域通常已知的那些,例如酚醛树脂,脲醛树脂,1,3,5-三嗪-2,4,6-三胺(三聚氰胺)树脂,双马来酰亚胺树脂,环氧树脂,乙烯基酯树脂,苯并噁嗪树脂,聚酯,不饱和的聚酯,氰酸酯树脂,或其混合物。环氧树脂是特别优选的。可根据需要添加固化剂和任选的促进剂。
所述纤维可具有宽泛的各种形式,并且可由宽泛的合适的材料制成。根据目标应用的要求的需要,所述纤维可以是单向的或者是多向排列编织的,或者是无纺的。优选的排列是使用单向的纤维,并且排列所述结构层,从而使得它们的纤维方向交替,从而形成半各向同性的组件。也可根据具体的应用,采用其它层堆叠排列。
所述纤维可由碳纤维、玻璃纤维或者有机纤维例如芳族聚酰胺制成。
在优选的实施方式中,所述凸起区域通过将它们印刷到基质的表面上而沉积。在本发明中合适的印刷类型是涉及到不直接与预浸料接触的类型。这些包括喷墨印刷,电子录印(electrographic printing),静电复印(xerographicprinting)和任何其它非接触式印刷技术。喷墨印刷是特别理想的,这是因为它不会涉及到任何与预浸料的接触,防止损害它的结构,以及最小化打印头的劣化。对于小规模的方法,Xenjet 4000喷墨打印机得到良好的结果。
为了获得足够高的凸起区域,可能需要使预浸料通过打印机几次。对于工业规模的方法,可使用与小规模上使用的那些类似的喷墨打印头,将打印头根据需要集结成组(ganging),从而容许快速和有效地印刷预浸料的整个宽度。
使用印刷方法来沉积所述凸起区域具有另外的优点:无论它们可能会有多么复杂,都容许实际地任意排列要沉积的凸起区域。
优选所述凸起区域通过沉积可通过除热之外的方法固化的物质例如可紫外线(UV)固化的物质而形成,从而它们可在沉积之后固化,而不会固化预浸料的基质。当通过印刷沉积所述凸起区域时,可固化的物质是尤其有利的,这是因为它们可以以液体形式沉积接着通过除热之外的方法固化,在未固化的预浸料上留下硬化的凸起区域。
通常,将会使沉积的液体在使预浸料再次通过打印机下面之前固化,从而将另外的可固化液体沉积到凸起区中。可根据需要重复这一步骤,直到获得足够高度的凸起区域为止。为了保持所述印刷的凸起区域的精确尺寸,所述区域的快速固化是重要的。如果固化不快速,那么该液态可固化的墨水可能从沉积的点向侧面或者向下迁移,导致凸起区的清晰度较差。
因此,在优选的实施方式中,所述凸起区域通过印刷(优选通过喷墨印刷)可通过除热之外的方法(优选可通过UV光或者可见光)固化的液体而沉积。
用于沉积的优选物质是可UV固化的喷墨墨水(inkjet inks),其中可固化的物质为例如丙烯酸类物质或者乙烯基醚。
可将所述凸起区域沉积为形成任何所需的图案,例如直线,折线(zig-zagline),波浪线,圆,方形等。但是,已经发现,简单的直线排列,尤其是平行的直线性能良好。
认为,不连续的凸起区域的图案,例如不连续的直线,在降低孔隙率方面比连续贯串所述预浸料的图案好。
因为本发明涉及到沉积到预浸料的表面上,所以它适合用于单向的预浸料,织物形式预浸料和多轴预浸料。但是,在使凸起区域的线平行于单向的预浸料中的纤维方向的情况下,获得较好的性能。
为了在层叠本发明的预浸料时形成尺寸适当的通道,凸起区域的高度必需大于5微米。典型的最大高度为200微米,优选为10至100微米,更优选为20至100微米。
所述凸起区域优选是不传导的,这是因为它们是不连续的,或者是因为它们由不传导的物质制成,或者同时存在这两个原因。
如上所讨论的,意图将根据本发明的预浸料层叠形成层合体,通常与模具接触。一旦形成层合体,就将它暴露于升高的温度,以及任选的升高的压力,从而使基质固化,得到具有模具形状的固化的复合层合体。
因此,另一方面,本发明提供固化多个根据本发明的预浸料的层合体的方法,所述方法包括将所述层合体暴露于升高的温度和任选的升高的压力,得到固化的复合层合体。
在固化过程中,滞留气体沿着层叠的根据本发明的预浸料所形成的通道流动,并离开层合体。在固化的过程中,基质随着温度的升高而软化,并且它开始流动,关闭所述通道并导致预浸料的融合,从而它们不再是单独可分辨的。进一步的温度增加导致基质固化,其给所产生的固化复合材料赋予它的固体特征。因此,凸起区域在固化的复合材料中通常不再是可分辨的。
因此,另一方面,本发明提供可通过固化根据本发明的层合体获得的多个预浸料的固化层合体。
合适的固化方法对于本领域技术人员将是已知的。如上所述,通常使用所谓的高压釜方法,这是因为它能够产生较低孔隙率的复合材料,但是需要消耗加热高压釜和将容器内的压力增加至通常为至多10巴的水平所需的花费和时间。
可供选择的方法包括将袋子置于预浸料的层合体上,并抽真空,从而迫使该袋子以大气压附着在层合体周围。通常将该层合体在炉中固化较短的时间,并且花费比高压釜方法少得多。但是这种方法的缺点是所产生的固化的复合层合体的孔隙率往往比高压釜中的高。
因为根据本发明的预浸料有助于任何滞留气体在固化过程中流出层合体,通过使用本发明,在以上的两种固化方法中都可获得改进。例如,已知的真空袋方法会产生具有降低的孔隙率的固化层合体,这将它的可能应用扩展到了需要较低孔隙率和较好的机械性质的领域。或者,可保持高压釜方法的非常低的孔隙率,但是可能使用较低的压力或者循环时间,减少对于给定的具体孔隙率的花费。
下面将以示例的方式并且参考以下附图说明本发明,在附图中:
图1至6示出了对于根据本发明的预浸料的印刷图案的选择。
图7是没有通过施加凸起区域进行改进的Hexply 8552预浸料的固化层合体的横截面图。
图8是已经根据图3中所示的图案在其上施加了凸起区域的Hexply8552预浸料的固化层合体的横截面图。
图9是已经根据图4中所示的图案在其上施加了凸起区域的Hexply8552预浸料的固化层合体的横截面图。
图10是在其上已经施加了凸起区域的Hexply 8552预浸料的平面图。
Hexply 8552,M56和M72是环氧树脂预浸料材料,可得自HexcelComposites,Duxford,Cambridge,United Kingdom。
对比例1
将面重量为134gm-2的单向的碳纤维8552预浸料层叠,其中交替的层为0和90°方向(200mm x 200mm)。在该层叠中所用的层数为12。然后将该组件在室温在真空下压实15分钟。将该预浸料置于真空台(vacuum table)上并在以下条件下固化:-加热至110℃,升温速率为1℃/min,并保持1小时,然后加热至180℃,升温速率为1℃/min,并保持2小时。使该组件冷却至室温并从真空台取出。
通过如下步骤测定样品的孔隙率:从该层合体的中心切下三个样品(30mm x 30mm),然后用细砂纸抛光各个边。将白色修正液涂到样品的一个切边上,并使其在室温干燥。通过用刀片的背面刮,除去白色修正液。留下的白色修正液为实测的层合体的孔面积。使用图像分析软件,孔隙率的百分比可从白色修正液的面积与该边的总面积比较而计算得到。
通过这个方法计算层合体的三个样品的平均孔隙率。表1总结了未改进的8552预浸料的孔隙率结果。图7至9示出了8552在用修正液处理之后的横截面,表明孔隙存在的地方,这能够通过图像分析来测定。
实施例2
将8552预浸料切成一定的尺寸(300mm x 300mm),并将各个层置于Xenjet 4000的Omnidot 760GS8打印头下。施加的墨水由多官能丙烯酸酯、专用的光敏引发剂混合物和品红染料的混合物(Magenta Vivide X8022Ink,得自Xennia)制成。使用UV灯(融合H灯泡(fusion H bulb))以159mJ/cm2的最小剂量来固化所述墨水。然后以100m/min的速度将所需的图案印刷到所述预浸料上。通过在相同的预浸料上印刷不止一次来获得不同的线高度。然后将印刷的预浸料层叠,交替的层为0和90°方向(200mm x 200mm)。在该层叠中所用的层数为12。然后将该组件在室温在真空下压实15分钟。
将该预浸料置于真空台上并在以下条件下固化:-加热至110℃,升温速率为1℃/min,并保持1小时,然后加热至180℃,升温速率为1℃/min,并保持2小时。使该组件冷却至室温并从真空台取出。与前面的实施例一样测定样品的孔隙率。
表1总结了不同图案和不同的线高度的孔隙率结果,并将其与未改进的预浸料进行比较。
表1
实施例3
将M56预浸料切成一定的尺寸(300mm x 300mm),并将各个层置于Xenjet 4000的Omnidot 760GS8打印头下。墨水和打印条件如前面的实施例所述。在该层叠中所用的层数为10。然后将该组件在室温在真空下压实15分钟。将该预浸料如前面的实施例一样进行固化。如实施例1和2中所述测定层合体的孔隙率。平均值基于来自相同层合体的三个样品的孔隙率测量值。
表2总结了M56和改进的M56复合材料的孔隙率结果。
表2
实施例4
将M72预浸料如前面的实施例所述进行切割和印刷。在该层叠中所用的层数为10。如前面所述进行压实和固化。如实施例1和2中所述测定层合体的孔隙率。平均值基于三个样品的孔隙率测量值。
表3总结了M72和改进的M72复合材料的孔隙率结果。
表3
Claims (19)
1.一种预浸料,其包括基质和纤维,所述预浸料具有沉积在其上的多个区域,所述区域相对于所述基质的表面凸起至少5微米。
2.根据权利要求1的预浸料,其中凸起区域通过印刷来沉积。
3.根据权利要求2的预浸料,其中所述印刷方法是喷墨印刷。
4.根据权利要求1的预浸料,其中凸起区域通过沉积可通过除热之外的方法固化的物质来形成。
5.根据权利要求4的预浸料,其中所述物质可通过暴露于紫外光或者可见光而固化。
6.根据权利要求1的预浸料,其中所述凸起区域是直线。
7.根据权利要求6的预浸料,其中所述预浸料中的纤维是单向的,而所述凸起区域的线与所述纤维平行。
8.根据权利要求1的预浸料,其中所述区域从所述基质的表面凸起5至200微米。
9.根据权利要求1的预浸料,其中所述凸起区域是不传导的。
10.固化多个根据权利要求1的预浸料的层合体的方法,所述方法包括将层合体暴露于升高的温度,得到固化的复合层合体。
11.通过根据权利要求10的方法获得的多个预浸料的固化的层合体。
12.从多个预浸料层制备层合体的方法,所述预浸料层各自包括纤维和具有表面的基质,其中改进包括在所述基质的表面上提供足够数目的凸起区域,该凸起区域的图案使得减少所述层合体的孔隙率。
13.根据权利要求12的方法,其中所述凸起区域形成平行线的图案。
14.根据权利要求13的方法,其中所述平行线是分段的,并且其中所述分段的平行线中的线段是对齐的,从而提供横向通过所述平行线图案延伸的通道。
15.根据权利要求14的方法,其中所述分段的平行线的线段具有基本上相等的长度,并且其中每条线中所述线段之间的距离显著短于所述线段的长度。
16.一种用于制备层合体的预浸料,所述预浸料包括纤维和具有表面的基质,其中改进包括在所述基质的表面上提供气体流出通道,所述气体流出通道由凸起区域形成,所述凸起区域置于所述基质的表面上,该凸起区域的图案使得减少所述层合体的孔隙率。
17.根据权利要求16的预浸料,其中所述凸起区域形成平行线图案。
18.根据权利要求17的预浸料,其中所述平行线是分段的,并且其中所述分段的平行线中的线段是对齐的,从而提供横向通过所述平行线图案延伸的通道。
19.根据权利要求18的预浸料,其中所述分段的平行线的线段具有基本上相等的长度,并且其中每条线中所述线段之间的距离显著短于所述线段的长度。
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US20110014419A1 (en) | 2011-01-20 |
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CN102027051A (zh) | 2011-04-20 |
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RU2491167C2 (ru) | 2013-08-27 |
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