CN108045015A - 一种增强型碳纤维预浸料、制备方法及应用 - Google Patents

一种增强型碳纤维预浸料、制备方法及应用 Download PDF

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CN108045015A
CN108045015A CN201711343390.2A CN201711343390A CN108045015A CN 108045015 A CN108045015 A CN 108045015A CN 201711343390 A CN201711343390 A CN 201711343390A CN 108045015 A CN108045015 A CN 108045015A
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fiber
carbon
aramid fiber
aramid
film
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孙直
郭旭
陈红杰
石姗姗
陈秉智
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Dalian University of Technology
Dalian Jiaotong University
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Dalian University of Technology
Dalian Jiaotong University
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Abstract

本发明提供了一种增强型碳纤维预浸料、制备方法及应用。一种增强型碳纤维预浸料，由树脂、芳纶短纤维薄膜和碳纤维织物组成；所述的芳纶短纤维薄膜由干法或湿法制备，面密度为0.1‑500g/m2，由长度2‑50mm，直径5nm‑50μm的芳纶短切纤维构成；所述的树脂完全浸渍碳纤维织物，同时在碳纤维织物表面形成富脂层，使至少一半芳纶短纤维薄膜没入富脂层中。本发明开发了一种轻质、绝缘、不限制气泡排除、材料利用率高且增韧效果优异的增强性碳纤维预浸料，该预浸料应用于复合材料金属芯体夹芯结构时，在不对结构引入损伤的情况下，仍能表现出优异的界面增韧效果。

Description

一种增强型碳纤维预浸料、制备方法及应用
技术领域
本发明涉及一种增强型碳纤维预浸料，尤其是能够显著提高金属芯体夹芯结构面芯界面韧性，及合适地获得该预浸料的制备方法。
背景技术
碳纤维夹芯结构以其轻质，比强度高，比模量高，隔热，隔声，耐腐蚀等优点被广泛应用于航空航天，船舶工业，汽车制造，文体休闲器材等众多领域，伴随着碳纤维复合材料的广泛应用，碳纤维预浸料的需求也日益增加。然而碳纤维增强复合材料的推广受到抗冲击性能差、易分层、面芯界面易脱粘等缺点的制约，为提高复合材料界面韧性，提出了多种改进技术。
一种技术是使用CF网片或短切碳纤维对碳纤维预浸料进行增强(参考专利文献CN102294846A和专利文献CN 103987764A)，然而该技术用于增强金属芯体夹芯结构界面韧性时，面芯界面会发生电化学腐蚀，影响结构安全。
一种技术是使用热塑性树脂薄膜(参考非专利文献J.Eng.Mater.Technol 118(3),302-309)提高复合材料界面韧性，然而热塑性树脂薄膜在复合材料成型时会限制气泡的排除及层间树脂再分配。
一种技术是使用热塑性粒子或纤维，导电粒子或纤维增强碳纤维预浸料(参考专利文献CN 102838766A和专利文献CN 103552331A)，该类增强型预浸料在使用时被发现热塑性树脂纤维与热固性树脂基体结合强度低，且粒子增强碳纤维预浸料不适用于增强多孔芯体的夹芯结构，导电粒子或纤维增强碳纤维预浸料不适用于增强碳纤维-金属界面韧性。
还有人提出了一种使用热塑性尼龙无纺布增韧碳纤维-金属层合板的技术(参考专利文献CN 102991009B)，然而该增韧碳纤维-金属层合板在热压固化过程中，热塑性尼龙无纺布会发生熔融或软化，从而造成成型品物性不稳定。
以上所提及的增强型预浸料坯或增韧技术，多用于层合板界面增韧，而不适用与夹芯结构面芯界面增韧。目前常用Z-pin法和缝纫法提高夹芯结构面芯界面韧性，然而这两种方法不适用于金属芯体或内部结构规则的芯体，且会引入蒙皮和芯体损伤，降低芯体的刚度和剪切强度。
为提高层合板界面韧性，且在不引入蒙皮和芯体缺陷的情况下实现夹芯结构界面增韧，方便工业化生产制造，要求开发一种满足绝缘、轻质、不限制气泡排除、材料利用率高并且具有优异的界面增韧性能的碳纤维预浸料及相应的生产工艺。
发明内容
本发明的目的是针对现有技术存在的问题，提供一种具有芳纶短纤维增强的碳纤维预浸料及相应的生产工艺。
一种增强型碳纤维预浸料、制备方法及应用，所述增强型预浸料表面覆盖一层由芳纶短纤维组成的薄膜，这种薄膜在金属芯体的夹芯结构中，能够预防蒙皮与芯体之间发生电化学腐蚀，提高结构的可靠性。
芳纶短纤维薄膜结构质地疏松，通透性能好，在复合材料固化过程中不影响树脂中小气泡的排除，同时对碳纤维层间树脂的重新分配影响较小，能够确保复合材料结构层间树脂分配均匀，提高结构整体性能。
所述的增强型碳纤维预浸料适应范围广，增强效果明显，当预浸料用于制备复合材料夹芯结构或层合板时，面芯或层间界面会由芳纶短纤维形成桥连结构，提供额外连接。裂纹尖端区域中的桥连作用，能够有效提高结构的临界断裂强度。当芯体为蜂窝芯体时，芳纶短纤维和富余的树脂在蜂窝端部形成圆角增韧区，能够有效提高芯体与蒙皮的结合强度。
增强型预浸料采用表面覆盖芳纶短纤维薄膜以达到界面增韧目的，与碳短纤维不同，芳纶短纤维具有更好的柔韧性，这种柔韧性使其在树脂基体中具有弯曲交联的特征。
由增强型预浸料制造的复合材料在界面开裂时，形成“桥”结构的芳纶短纤维会出现两种形式的破坏，即拉断和拔出，拉断和拔出存在竞争关系。芳纶短纤维的弯曲交联特征，使短纤维不容易从基体中拔出，确保了短纤维能够充分发挥增强性能。而碳短纤维柔韧性较差，单根短纤维在基体中不易弯曲，由其增强的复合材料在界面开裂时，短纤维容易从基体中拔出，不能充分发挥碳短纤维的增强性能。
本发明的技术方案：
一种增强型碳纤维预浸料，由树脂、芳纶短纤维薄膜和碳纤维织物组成；
所述的芳纶短纤维薄膜由干法或湿法制备，面密度为0.1-500g/m2，由长度2-50mm，直径5nm-50μm的芳纶短切纤维构成；
所述的树脂完全浸渍碳纤维织物，同时在碳纤维织物表面形成富脂层，使至少一半芳纶短纤维薄膜没入富脂层中；
所述的碳纤维织物中碳纤维为T300级碳纤维、T700级碳纤维、T800级碳纤维、T1000级碳纤维或MJ系列碳纤维。
干法制备芳纶短纤维薄膜，步骤如下：
(1)将芳纶纤维织物切割成包含所需尺寸短纤维的芳纶纤维块；
(2)将芳纶纤维块置于搅拌器中，搅拌，将芳纶纤维块打散，使其在搅拌器上方形成交联的短纤维絮状薄膜；
(3)在保证短纤维絮状薄膜松散的情况下，收集薄膜，铺设成均匀的具有一定面密度的芳纶短纤维薄膜；
(4)将芳纶短纤维薄膜夹在离型纸中间储存。
为保证芳纶纤维不被搅拌器刀片破坏，同时避免纤维缠绕刀片，搅拌器刀片使用钝刀片。
为保证短纤维被充分打散，并得到均匀的絮状纤维薄膜，所述搅拌器转速为2000-30000转/分，每次搅拌短纤维质量与搅拌器容积之比为0.05-1g/L，搅拌时间为1-20分钟。
湿法制备芳纶短纤维薄膜，步骤如下：
(1)将芳纶纤维织物切割成包含所需尺寸短纤维的芳纶纤维块；
(2)将芳纶纤维块和水共同置于搅拌器中搅拌，将芳纶纤维块在水中打散，使其充分均匀分布在水中，继续超声震荡10-30分钟；
(3)震荡结束，用预埋置于超声分散器底部的丝网将芳纶纤维丝捞起，送至干燥箱干燥形成芳纶短纤维薄膜。
为减轻搅拌器负荷，保证水在搅拌器中形成足够的涡流，要求被注入搅拌器的水为搅拌器容器的1/5-1/2，每次搅拌短纤维质量与所注入水的容积之比为0.05-0.5g/L，搅拌器转速为2000-20000转/分，搅拌时间为1-20分钟；干燥箱温度为30℃-90℃，干燥时间为1-10分钟。
一种溶液法制备增强型碳纤维预浸料的方法，
步骤如下：
(1)浸胶挤胶：将碳纤维织物通过浸胶槽，对充分浸润树脂的碳纤维织物进行挤胶处理；
(2)压合：在经过挤胶处理的碳纤维织物上层覆盖离型纸包覆层，然后将碳纤维织物和芳纶短纤维薄膜共同通过压合装置，使芳纶短纤维薄膜粘覆于碳纤维织物表层；
(3)收卷储存：将制作好的具有芳纶短纤维增强的碳纤维预浸料通过收卷装置收卷储存。
该增强型碳纤维预浸料用于夹芯结构或碳纤维-金属组合结构界面增韧。
本发明的有益效果：
1.本发明开发了一种轻质、绝缘、不限制气泡排除、材料利用率高且增韧效果优异的增强性碳纤维预浸料，该预浸料应用于复合材料金属芯体夹芯结构时，在不对结构引入损伤的情况下，仍能表现出优异的界面增韧效果。
2.本发明试用范围较广，不仅适用于各种夹芯结构面芯增韧，还可用于层合板界面增韧。根据所制造夹芯结构或层合板尺寸，承载方式和载荷水平，可对芳纶短纤维面密度进行适应性调整，使结构刚度，强度和功能性满足要求。
3.本发明还开发了一种用于制备该增强型预浸料的生产工艺，尤其是专门设计了制备芳纶短纤维薄膜的方法，使该增强型预浸料得以能够批量生产。
4.本发明所使用树脂材料为相同树脂，在制造相应复合材料时可以共固化成型。
5.本发明所设计的生产工艺与现有预浸料生产工艺相比，增加了芳纶短纤维薄膜制备与铺设环节，方便在现有设计基础上改进，节省设备更新开支。
附图说明
图1为经搅拌器搅拌形成的絮状芳纶短纤维。
图2为面密度为6g/m2的芳纶短纤维薄膜。
图3为湿法制备芳纶短纤维薄膜配合溶液法制备增强型碳纤维预浸料的工艺示意图。
图4为溶液法制备的增强型碳纤维预浸料的示意图。
图中：1搅拌器；2超声分散器；3碳纤维织物；4打捞网；5传送带；6干燥箱；7浸胶槽；8挤胶装置；9离型纸；10压合装置；11收卷装置；12芳纶短纤维薄膜；13环氧树脂。
具体实施方式
本发明涉及一种增强型碳纤维预浸料及生产工艺，其特征是：预浸料由碳纤维织物、树脂和芳纶短纤维薄膜组成；所述的树脂完全浸渍碳纤维织物，并在碳纤维织物表形成富脂层，所述的芳纶短纤维薄膜覆于碳纤维织物一个表面，且至少一半芳纶短纤维薄膜没入碳纤维表面的富脂层内。
本发明设计了干法和湿法制备芳纶短纤维薄膜的方法。
干法制备芳纶短纤维薄膜：将芳纶纤维织物切割成剪切成一定边长的方块；将纤维块放置进搅拌器中搅拌1-3分钟，使短纤维在搅拌器上方形成交联的絮状薄膜；在保证短纤维絮状薄膜松散的情况下，收集薄膜，手工铺设成均匀的具有一定面密度的芳纶短纤维薄膜。
其中搅拌器刀片使用钝刀片，搅拌器转速为2000-30000转/分，每次搅拌短纤维质量与搅拌器容积之比为0.05-1g/L。
湿法制备芳纶短纤维薄膜：将芳纶纤维织物剪切成一定边长的方块，将适量剪切好的芳纶纤维块放入搅拌器中，并注入一定量的水，搅拌1-20分钟使芳纶纤维在水中分布均匀，继续震荡10-30分钟，震荡结束，用预置在分散器中的丝网将芳纶短纤维打捞起来送入干燥箱干燥，得到一定面密度的芳纶短纤维薄膜。
其中搅拌器刀片使用钝刀片，搅拌器转速为2000-20000转/分，所注入水占搅拌器容积的1/5-1/2，每次搅拌短纤维质量与所注入水的容积之比为0.05-0.5g/L，干燥箱温度为30℃-90℃，干燥时间为1-10分钟。
将制备芳纶短纤维薄膜覆于经树脂浸渍的碳纤维织物表面，共同缓慢通过压合装置，使至少一半芳纶短纤维没入碳纤维织物表面富脂层内，得到具有芳纶短纤维增韧的碳纤维预浸料。
实施例1
干法制备Kevlar短纤维薄膜，所述Kevlar方块边长8mm，搅拌器转速20000转/分钟，每次搅拌Kevlar短纤维质量与搅拌器容积之比为0.15g/L，搅拌时间2分钟，Kevlar短纤维薄膜面密度6g/m2。
实施例2
干法制备Kevlar短纤维薄膜，所述Kevlar方块边长8mm，搅拌器转速20000转/分钟，每次搅拌Kevlar短纤维质量与搅拌器容积之比为0.2g/L，搅拌时间2分钟，Kevlar短纤维薄膜面密度12g/m2。
实施例3
湿法制备Kevlar短纤维薄膜，所述Kevlar方块边长12mm，搅拌器转速15000转/分钟，搅拌时间3分钟，超声震荡时间10分钟，干燥箱温度90℃，干燥2分钟，Kevlar短纤维薄膜面密度12g/m2。
实施例4
湿法制备Kevlar短纤维薄膜，所述Kevlar方块边长12mm，搅拌器转速15000转/分钟，搅拌时间3分钟，超声震荡时间15分钟，干燥箱温度50℃，干燥5分钟，Kevlar薄膜面密度50g/m2。
将实施例1所制备的预浸料用于碳纤维/泡沫铝夹芯结构面芯增韧。铝泡沫厚度为15mm，上下蒙皮均由两层普通碳纤维预浸料和一层实施例1所制备增强型预浸料组成，其中增强型预浸料有Kevlar薄膜的一面置于蒙皮与芯体交界面上。层合材料组装/装配后共固化成型。
根据实验结果，在面内压缩条件下，相比于未增韧的泡沫铝夹芯试件，增韧试件的极限载荷和能量吸收平均值分别上升22.23％和47.13％。
将实施例3所制备的预浸料用于夹芯结构面芯增韧。夹芯结构芯体采用蜂窝芯体，其中蜂窝孔径为6.35mm，壁厚为0.06mm，高度为12mm；上下蒙皮均由四层普通斜纹编织碳纤维预浸料和一层实施例3所制备增强型预浸料组成，其中增强型预浸料有Kevlar薄膜的一面置于蒙皮与芯体交界面上。层合材料组装/装配后共固化成型。
根据实验结果，在三点弯曲条件下，相比于未增韧的蜂窝铝夹芯试件，增韧试件的极限载荷和能量吸收平均值分别上升14.06％和61.53％，而标准差分别下降37.14％和52.65％。在面内压缩条件下，相比于未增韧的蜂窝铝夹芯试件，增韧试件的极限载荷和能量吸收平均值分别上升55.80％和99.47％，而标准差分别下降0.97％和65.10％。

Claims (6)

1.一种增强型碳纤维预浸料，其特征在于，所述的增强型碳纤维预浸料由树脂、芳纶短纤维薄膜和碳纤维织物组成；
所述的芳纶短纤维薄膜由干法或湿法制备，面密度为0.1-500g/m2，由长度2-50mm，直径5nm-50μm的芳纶短切纤维构成；
所述的树脂完全浸渍碳纤维织物，同时在碳纤维织物表面形成富脂层，使至少一半芳纶短纤维薄膜没入富脂层中。
2.根据权利要求1所述的增强型碳纤维预浸料，其特征在于，所述的碳纤维织物中碳纤维为T300级碳纤维、T700级碳纤维、T800级碳纤维、T1000级碳纤维或MJ系列碳纤维。
3.根据权利要求1或2所述的增强型碳纤维预浸料，其特征在于，干法制备芳纶短纤维薄膜，步骤如下：
(1)将芳纶纤维织物切割成包含所需尺寸短纤维的芳纶纤维块；
(2)将芳纶纤维块置于搅拌器中，搅拌，将芳纶纤维块打散，使其在搅拌器上方形成交联的短纤维絮状薄膜；
(3)在保证短纤维絮状薄膜松散的情况下，收集薄膜，铺设成均匀的具有一定面密度的芳纶短纤维薄膜；
(4)将芳纶短纤维薄膜夹在离型纸中间储存；
所述搅拌器转速为2000-30000转/分，每次搅拌短纤维质量与搅拌器容积之比为0.05-1g/L，搅拌时间为1-20分钟；
所述的搅拌器刀片使用钝刀片。
4.根据权利要求1或2所述的增强型碳纤维预浸料，其特征在于，湿法制备芳纶短纤维薄膜，步骤如下：
(1)将芳纶纤维织物切割成包含所需尺寸短纤维的芳纶纤维块；
(2)将芳纶纤维块和水共同置于搅拌器中搅拌，将芳纶纤维块在水中打散，使其充分均匀分布在水中，继续超声震荡10-30分钟；
(3)震荡结束，用预埋置于超声分散器底部的丝网将芳纶纤维丝捞起，送至干燥箱干燥形成芳纶短纤维薄膜；
注入搅拌器的水为搅拌器容器的1/5-1/2，每次搅拌短纤维质量与所注入水的容积之比为0.05-0.5g/L，搅拌器转速为2000-20000转/分，搅拌时间为1-20分钟；干燥箱温度为30℃-90℃，干燥时间为1-10分钟；
所述的搅拌器刀片使用钝刀片。
5.一种溶液法制备增强型碳纤维预浸料的方法，其特征在于，步骤如下：
(1)浸胶挤胶：将碳纤维织物通过浸胶槽，对充分浸润树脂的碳纤维织物进行挤胶处理；
(2)压合：在经过挤胶处理的碳纤维织物上层覆盖离型纸包覆层，然后将碳纤维织物和芳纶短纤维薄膜共同通过压合装置，使芳纶短纤维薄膜粘覆于碳纤维织物表层；
(3)收卷储存：将制作好的具有芳纶短纤维增强的碳纤维预浸料通过收卷装置收卷储存。
6.一种增强型碳纤维预浸料用于夹芯结构或碳纤维-金属组合结构界面增韧。
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