CN114829468A - 预浸材料、该预浸材料的制备方法和由该预浸材料制备的纤维增强复合材料 - Google Patents
预浸材料、该预浸材料的制备方法和由该预浸材料制备的纤维增强复合材料 Download PDFInfo
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- CN114829468A CN114829468A CN202080087382.XA CN202080087382A CN114829468A CN 114829468 A CN114829468 A CN 114829468A CN 202080087382 A CN202080087382 A CN 202080087382A CN 114829468 A CN114829468 A CN 114829468A
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- Prior art keywords
- prepreg
- epoxy resin
- resin
- type epoxy
- producing
- Prior art date
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Classifications
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Abstract
本公开涉及一种预浸材料、该预浸材料的制备方法和由该预浸材料制备的纤维增强复合材料。该预浸材料的制备方法可以包括对树脂具有改善的润湿性能的芳纶纤维基材,在预浸材料成型过程中能够提高厚度降低率,具有合适的树脂含量,并且能够提供一种适合通过非高压釜工艺而成型的预浸材料。此外,所述预浸材料可以提供一种即使通过非高压釜工艺也表现出薄厚度和高树脂含量、并且表现出高强度和低水分吸收率的纤维增强复合材料。
Description
技术领域
本公开涉及一种预浸材料、该预浸材料的制备方法和由该预浸材料制备的纤维增强复合材料。
背景技术
通过将基质树脂浸渍在用于增强的纤维材料中、然后固化所制备的纤维增强复合材料已经广泛用于诸如电子部件、汽车部件等的各种领域。
玻璃纤维或碳纤维已经主要用作用于增强的纤维材料。然而,玻璃纤维具有高比重,因此难以减轻重量,并且玻璃纤维对人体也有害,而碳纤维具有高比刚度,因此机械加工性和抗冲击性差。
作为解决这些问题的替代物,已经引入了一种使用芳纶纤维的技术。然而,与玻璃纤维或碳纤维相比,芳纶纤维的润湿性能差,并且与基质树脂的相容性差,因此导致例如在固化成纤维增强复合材料之后产生空隙的另外的问题。
发明内容
技术问题
在本公开中,提供一种预浸材料的制备方法。
还提供一种由所述预浸材料的制备方法制备的预浸材料和由所述预浸材料制备的纤维增强复合材料。
技术方案
下文,将描述根据本公开的具体实施方案的预浸材料的制备方法、由该制备方法制备的预浸材料和由该预浸材料制备的纤维增强复合材料。
根据一个实施方案,提供一种预浸材料的制备方法,包括:
第一层压步骤,将树脂薄膜层压在芳纶纤维基材上并施加压力;和第二层压步骤,对由所述第一层压步骤得到的层压体施加压力,
其中,相比于在所述第一层压步骤中,在所述第二层压步骤中在更低的温度下施加更低的压力。
作为研究提高纤维增强复合材料的芳纶纤维对树脂的润湿性能的结果,本发明人已经证实,当通过在高温和高压条件下进行的第一层压步骤和在低温和中压条件下进行的第二层压步骤,制备预浸材料(该预浸材料是一种用于制备纤维增强复合材料的中间材料)时,通过改善在预浸材料成型过程中芳纶纤维基材对树脂的润湿性能,能够获得高品质的纤维增强复合材料。
具体地,本发明人考虑到在制备和成型预浸材料的条件下芳纶纤维基材的弹性回复性能、树脂薄膜的粘度性能和固化性能等,已经开发了一种具有合适的树脂含量的预浸材料的制备方法,同时在预浸材料成型过程中提高厚度降低率。
根据一个实施方案的制备方法的第一层压步骤可以使树脂的渗透性最大化,使得树脂薄膜可以深入渗透到芳纶纤维基材中,并且该第一层压步骤可以在高温和高压下进行,使得合适含量的树脂可以浸渍到芳纶纤维基材中。
具体地,第一层压步骤可以在80℃至90℃、82℃至88℃或者84℃至86℃的温度下进行。在上述温度范围内,树脂的渗透性可以最大化,同时树脂薄膜不硬化,并且在芳纶纤维基材的内部可以不出现未浸渍部分,从而阻止如下问题发生,例如强度降低,以及由未浸渍区域或者在后续成型过程中出现的干燥区域所造成的高水分吸收率。
此外,第一层压步骤可以在2.6巴至5巴、2.8巴至4.5巴或者3巴至4巴的压力下进行。像这样,当在高温下对层压在芳纶纤维基材的两面上的树脂薄膜施加高压时,树脂的粘度可能会降低,并且树脂可以容易地在芳纶纤维基材的纤维之间渗透,因此在芳纶纤维基材的内部可能不会出现未浸渍部分,从而阻止了诸如强度降低和高水分吸收率的问题的发生。另外,当对芳纶纤维基材施加高压之后除去压力时,由于芳纶纤维基材的弹性回复,可能在预浸材料的内部形成相对大的空隙。由于该大的空隙,预浸材料在成型过程中可以具有提高的厚度降低率。
根据上述一个实施方案的制备方法的第二层压步骤可以在低温和中压下进行,以提高芳纶纤维基材的表面附近的树脂粘合性、浸渍性能等,并且提供合适水平的树脂含量。
具体地,第二层压步骤可以在70℃至79℃、70℃至75℃或者70℃至73℃的温度下进行。此外,第二层压步骤可以在1.5至2.5巴、1.7至2.3巴或者1.8至2.2巴的压力下进行。像这样,当在低温下对层压体施加中压时,芳纶纤维基材的弹性回复程度和树脂的粘度可以控制在合适的水平,以改善芳纶纤维基材的表面附近的与树脂的粘合性和树脂的浸渍,并且改善表面质量,同时提高预浸材料中的树脂含量。
根据一个实施方案的制备方法可以以连续工艺来进行。具体地,可以连续地供应芳纶纤维基材和树脂薄膜,使树脂薄膜层压在芳纶纤维基材的两面上。更具体地,芳纶纤维基材和树脂薄膜可以通过辊连续地供应,并且可以通过具有加热表面的压力辊来进行层压。作为一个实例,第一层压步骤和第二层压步骤可以通过至少两个辊来进行,其中至少一个辊可以在表面温度被加热至高温(例如,80℃至90℃、82℃至88℃或者84℃至86℃)的状态下在高压(例如,2.6巴至5巴、2.8巴至4.5巴或者3巴至4巴)下对层压在芳纶纤维基材的两面上的树脂薄膜加压,并且至少另一个辊可以在表面温度被加热至低温(例如,70℃至79℃、70℃至75℃或者70℃至73℃)的状态下在中压(例如,1.5巴至2.5巴、1.7巴至2.3巴或者1.8巴至2.2巴)下对层压体加压。
此时,可以通过将第一层压步骤中的进料速度调整为0.1m/min至1.5m/min、0.1m/min至1.0m/min或者0.1m/min至0.8m/min将树脂薄膜充分浸渍直至芳纶纤维基材的中心。
在第二层压步骤中,可以将层压体的进料速度调整为与第一层压步骤中相同,这在于第二层压步骤可以以与第一层压步骤连续的工艺来进行。
可以用于根据一个实施方案的制备方法中的芳纶纤维基材可以是用芳纶纤维编织成的织物。在这种情况下,可以通过使用1500旦尼尔至3500旦尼尔的纤维作为芳纶纤维使树脂的浸渍性能最大化来制备具有优异的机械性能的预浸材料。
在根据一个实施方案的制备方法中,通过使用在约90℃至130℃的温度下固化的树脂薄膜,可以防止树脂薄膜在第一层压步骤和第二层压步骤中固化。
另外,通过使用在约70℃下的绝对粘度为约5Pa·s至10Pa·s的树脂薄膜,可以改善树脂薄膜对芳纶纤维基材的浸渍性能。
绝对粘度可以是在制备直径为约300mm且厚度为约300μm的试样之后通过使用旋转流变仪在约70℃下测量的粘度值。
这种树脂薄膜可以包括热塑性树脂、热固性树脂或它们的混合物。
例如,所述树脂薄膜可以由热固性树脂组合物形成。热固性树脂组合物的主要树脂可以是选自环氧树脂、酚树脂、不饱和聚酯树脂和氰酸酯树脂等中的至少一种。
其中,所述树脂薄膜可以由包含环氧树脂的热固性树脂组合物形成。
在热固性树脂组合物中包含的环氧树脂可以是指分子中具有两个或更多个环氧基团的材料或者通过该材料的聚合而制得的树脂。作为环氧树脂,例如,可以使用选自以下中的至少一种:双酚型环氧树脂,例如双酚A型环氧树脂、双酚F型环氧树脂、双酚AD型环氧树脂和双酚S型环氧树脂;溴化环氧树脂,例如四溴双酚A二缩水甘油醚;具有联苯骨架的环氧树脂;具有萘骨架的环氧树脂;具有双环戊二烯骨架的环氧树脂;酚醛清漆型环氧树脂,例如苯酚酚醛清漆型环氧树脂和甲酚酚醛清漆型环氧树脂;和缩水甘油胺型环氧树脂,例如二氨基二苯甲烷型环氧树脂、二氨基二苯砜型环氧树脂、氨基苯酚型环氧树脂、间二甲苯二胺型环氧树脂、1,3-双(氨基甲基)环己烷型环氧树脂(1,3-bisaminomethylcyclohexane type epoxy resin)和异氰脲酸酯型环氧树脂。
此外,所述热固性树脂组合物可以包含用于使环氧树脂固化的固化剂。具有能够与环氧基团交联的活性基团的化合物可以用作固化剂。该固化剂的实例可以包括双氰胺、二氨基二苯甲烷、二氨基二苯砜、氨基苯甲酸酯、各种酸酐、苯酚酚醛清漆树脂、甲酚酚醛清漆树脂、多酚化合物、咪唑衍生物、脂肪胺、四甲基胍、硫脲-胺(thiourea-amine)、甲基六氢邻苯二甲酸酐、其它羧酸酸酐、羧酸酰肼(carboxylic acid hydrazide)、羧酸酰胺(carboxylic acid amide)、多硫醇、三氟化硼乙胺配合物、其它路易斯酸配合物等。
基于100重量份的环氧树脂,固化剂可以以约3重量份至10重量份的量使用,从而在没有残留固化剂的情况下适当地使环氧树脂固化。
如果需要,所述热固性树脂组合物可以进一步包含热塑性树脂。例如,该热塑性树脂可以是选自聚酰胺、聚碳酸酯、聚缩醛、聚苯醚、聚苯硫醚、聚芳酯、聚酯、聚酰胺酰亚胺、聚酰亚胺、聚醚酰亚胺、具有苯基三甲基二氢化茚结构的聚酰亚胺、聚砜、聚醚砜、聚醚酮、聚醚醚酮、聚芳酰胺、聚醚腈和聚苯并咪唑中的至少一种。
所述热塑性树脂可以以颗粒或纤维的形式加入。当以颗粒的形式加入时,其形状可以是球形、非球形、多孔、晶须或薄片形状,当以纤维的形式加入时,热塑性树脂可以以短纤维或长纤维的状态加入。
除了上述构成之外,所述热固性树脂组合物可以进一步包含本发明所属领域中已知的各种添加剂,例如,固化助剂等。
同时,根据本公开的另一实施方案,提供一种根据所述制备方法制备的预浸材料。根据所述制备方法制备的预浸材料可以包括芳纶纤维基材和浸渍在芳纶纤维基材中的树脂。由于上文已经详细地描述了芳纶纤维基材和树脂,因此将省略它们的详细描述。
具体地,所述预浸材料通过在特定条件下的两步层压工艺制备得到,并且被树脂浸渍直至该预浸材料的中心,因此可以以最小化的未浸渍区域来提供。此外,它还可以具有相对大的空隙,从而表现出合适的树脂含量,同时在成型为纤维增强复合材料的过程中表现出大的厚度降低率。
具体地,所述预浸材料可以具有35重量%至45重量%、37重量%至43重量%或者39重量%至41重量%的高树脂含量。
此外,所述预浸材料可以在不使用高压釜(其是昂贵的加压设备)的情况下,通过仅使用真空泵和烘箱的非高压釜工艺提供纤维增强复合材料。
虽然现有的非高压釜工艺具有不使用昂贵的加压设备的优点,但是该方法的缺点是由于通过树脂薄膜的挥发性成分形成空隙而导致缺陷率高。
然而,根据一个实施方案的制备方法制备的预浸材料即使通过非高压釜工艺也可以提供高质量的纤维增强复合材料。
同时,根据本公开的另一实施方案,提供一种由所述预浸材料制备的纤维增强复合材料。该纤维增强复合材料可以包括芳纶纤维基材和在浸渍在所述芳纶纤维基材中的状态下被固化的树脂。由于上面已经详细描述了芳纶纤维基材和树脂,因此将省略它们的详细描述。
纤维增强复合材料可以由一种或更多种预浸材料制备而成,或者由两种或更多种预浸材料层合的层压体制备而成。
纤维增强复合材料由通过上述特定条件下的两步层压工艺制备的预浸材料制备而成,以使未浸渍区域或干燥区域最小化,从而表现出优异的强度、低水分吸收率等。
具体地,所述纤维增强复合材料根据ASTM D790测量的弯曲强度可以为250MPa至400MPa、270MPa至350MPa或者300MPa至330MPa。
另外,所述纤维增强复合材料通过以下公式1计算的水分吸收率可以为0重量%以上,且3重量%以下、2重量%以下或者1.7重量%以下。
[公式1]
水分吸收率=(浸渍之后样品的重量-浸渍之前样品的重量)/浸渍之前样品的重量*100
在公式1中,所述浸渍之前样品的重量是将样品浸渍在蒸馏水中之前的重量;所述浸渍之后样品的重量是完全浸渍在蒸馏水中并取出之后测量的样品的重量,其中该重量是首先用毛巾从样品的上下部分和边缘除去水分并用干毛巾二次从上下部分除去水分之后测量的值。
对于测量弯曲强度和水分吸收率的方法的细节,参照后文描述的试验例中描述的内容。
即使当通过非高压釜工艺成型时,所述纤维增强复合材料也可以表现出上述优异的弯曲强度和低水分吸收率。
此外,所述纤维增强复合材料可以表现出35重量%至45重量%、35重量%至40重量%、36重量%至38重量%或者37重量%至38重量%的高树脂含量。
有益效果
根据本公开的一个实施方案的预浸材料的制备方法可以包括对树脂具有改善的润湿性能的芳纶纤维基材,在预浸材料成型过程中能够提高厚度降低率,具有合适的树脂含量,并且能够提供一种适合通过非高压釜工艺而成型的预浸材料。此外,所述预浸材料可以提供一种即使通过非高压釜工艺也表现出薄厚度和高树脂含量的纤维增强复合材料,并且该纤维增强复合材料表现出高强度和低水分吸收率。
具体实施方式
下文中,将通过具体实施例更详细地描述本发明的功能和效果。然而,这些实施例仅用于说明的目的,并且本发明不旨在局限于这些实施例。
实施例1:预浸材料的制备
使用具有约3000旦尼尔的芳纶纱作为经纱和纬纱编织成平纹芳纶织物。
同时,通过将来自EZ Composite的以SCP-510供应的环氧树脂组合物以约80±10g/m2的涂覆量涂覆到离型纸上、然后进行干燥而制备的环氧树脂薄膜用作树脂薄膜。
在连续供应芳纶织物的同时,连续供应环氧树脂薄膜以与芳纶织物的两面接触。芳纶织物和树脂薄膜的进料速度控制在约0.5m/min。
然后,通过用加热至85℃的压力辊对层压在芳纶织物的两面上的树脂薄膜施加3巴的压力进行第一层压步骤。之后,通过用再次加热至70℃的压力辊对在第一层压步骤中得到的层压体施加2巴的压力的第二层压步骤,通过将树脂薄膜浸渍在芳纶织物的两面上而制备预浸材料。
比较例1:预浸材料的制备
除了进行用加热至85℃的压力辊对层压在芳纶织物的两面上的树脂薄膜施加压力的第一层压步骤;用加热至70℃的压力辊对层压在芳纶织物的两面上的树脂薄膜施加压力的第二层压步骤;和用加热至100℃的压力辊对层压在芳纶织物的两面上的树脂薄膜施加压力的第三层压步骤,来代替第一层压步骤和第二层压步骤之外,通过与实施例1相同的方法制备预浸材料。
试验例:预浸材料的物理性能的评价
在实施例和比较例中制备的预浸材料的物理性能通过下述方法进行评价,并且其结果示于表1中。
1)成型之前的树脂含量
测量每单位树脂薄膜的质量与每单位预浸材料的质量的百分率((每单位预浸材料的质量-每单位芳纶织物的质量)/每单位预浸材料的质量*100),并将其定义为树脂含量(单位:重量%)。
2)成型之后的厚度、厚度变化率和树脂含量
将四个预浸材料层压成四层,然后用辊充分压制。然后,将层压体放置在经过防粘处理的平坦模具上,并且将一离型膜层压上。并且,在具有与厚度为2mm的预浸材料相同尺寸的垫板(钢)层压和不层压的情况下,将用作真空袋内部空气流路的通气孔层压在离型膜上,最后用真空袋包裹上,然后用密封胶密封。然后,通过在28inchHg的真空压力下在125℃下保持30分钟,同时使预浸材料固化,而制备纤维增强复合材料。
对于使用垫板制备的纤维增强复合材料和不使用垫板制备的纤维增强复合材料,分别测量厚度、厚度变化率和树脂含量。
通过对于样品的每个角两个点,测量总共四个角的八个点处的厚度来测量厚度,然后获得其平均值,厚度变化率由成型之前与之后的厚度差与成型之前的厚度的百分率(成型之前与之后的厚度差/成型之前的厚度×100)来计算得出,并且树脂含量通过上述方法来测量。
3)弯曲强度
根据ASTM D790,在23±2℃的温度下,使用万能拉伸试验机测量通过使用垫板制备的纤维增强复合材料和在不使用垫板的情况下制备的纤维增强复合材料的弯曲强度。
4)水分吸收率
通过将样品完全浸入蒸馏水中来测量使用垫板制备的纤维增强复合材料和在不使用垫板的情况下制备的纤维增强复合材料的水分吸收率。然后,通过将浸渍之前的重量和浸渍之后的重量代入以下公式1来计算水分吸收率。
[公式1]
水分吸收率(重量%)=(浸渍之后样品的重量-浸渍之前样品的重量)/浸渍之前样品的重量*100
此时,首先用毛巾(五张金佰利纸巾、干织物等)从样品的上下部分和边缘除去水分,再次用干毛巾二次从上下部分除去水分以目视完全除去水分之后,测量浸渍之前和之后的重量。
[表1]
Claims (15)
1.一种预浸材料的制备方法,包括:
第一层压步骤,将树脂薄膜层压在芳纶纤维基材上并施加压力;和第二层压步骤,对由所述第一层压步骤得到的层压体施加压力,
其中,相比于在所述第一层压步骤中,在所述第二层压步骤中在更低的温度下施加更低的压力。
2.根据权利要求1所述的预浸材料的制备方法,其中,所述第一层压步骤在80℃至90℃的温度下进行。
3.根据权利要求1所述的预浸材料的制备方法,其中,所述第一层压步骤是将树脂薄膜层压在芳纶纤维基材上并施加2.6巴至5巴的压力。
4.根据权利要求1所述的预浸材料的制备方法,其中,所述第二层压步骤在70℃至79℃的温度下进行。
5.根据权利要求1所述的预浸材料的制备方法,其中,所述第二层压步骤是对由所述第一层压步骤得到的层压体施加1.5巴至2.5巴的压力。
6.根据权利要求1所述的预浸材料的制备方法,其中,所述第一层压步骤是以0.1m/min至1.5m/min的进料速度连续供应所述芳纶纤维基材和所述树脂薄膜,使得所述树脂薄膜层压在所述芳纶纤维基材的两面上。
7.根据权利要求1所述的预浸材料的制备方法,其中,所述芳纶纤维基材用1500旦尼尔至3500旦尼尔的芳纶纤维编织而成。
8.根据权利要求1所述的预浸材料的制备方法,其中,所述树脂薄膜在90℃至130℃下固化。
9.根据权利要求1所述的预浸材料的制备方法,其中,所述树脂薄膜在70℃下的绝对粘度为5Pa·s至10Pa·s。
10.根据权利要求1所述的预浸材料的制备方法,其中,所述树脂薄膜由包含环氧树脂和固化剂的热固性树脂组合物形成。
11.根据权利要求10所述的预浸材料的制备方法,其中,所述环氧树脂包括选自双酚A型环氧树脂、双酚F型环氧树脂、双酚AD型环氧树脂、双酚S型环氧树脂、四溴双酚A二缩水甘油醚、具有联苯骨架的环氧树脂、具有萘骨架的环氧树脂、具有双环戊二烯骨架的环氧树脂、苯酚酚醛清漆型环氧树脂、甲酚酚醛清漆型环氧树脂、二氨基二苯甲烷型环氧树脂、二氨基二苯砜型环氧树脂、氨基苯酚型环氧树脂、间二甲苯二胺型环氧树脂、1,3-双(氨基甲基)环己烷型环氧树脂和异氰脲酸酯型环氧树脂中的至少一种。
12.一种由权利要求1所述的预浸材料的制备方法制备的预浸材料。
13.根据权利要求12所述的预浸材料,该预浸材料的树脂含量为35重量%至45重量%。
14.一种纤维增强复合材料,包括芳纶纤维基材和在浸渍在所述芳纶纤维基材中的状态下被固化的树脂,其中,根据ASTM D790测量的弯曲强度为250MPa至400MPa。
15.根据权利要求14所述的纤维增强复合材料,其中,由以下公式1计算的水分吸收率为0至3重量%:
[公式1]
水分吸收率=(浸渍之后样品的重量-浸渍之前样品的重量)/浸渍之前样品的重量*100
在所述公式1中,所述浸渍之前样品的重量是将样品浸渍在蒸馏水中之前的重量;所述浸渍之后样品的重量是完全浸渍在蒸馏水中并取出之后测量的样品的重量,其中该重量是首先用毛巾从样品的上下部分和边缘除去水分、并用干毛巾从上下部分二次除去水分之后测量的值。
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