CN103946012A - 剥离层、使用其的表面制备和结合复合结构的方法 - Google Patents

剥离层、使用其的表面制备和结合复合结构的方法 Download PDF

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Publication number
CN103946012A
CN103946012A CN201280055806.XA CN201280055806A CN103946012A CN 103946012 A CN103946012 A CN 103946012A CN 201280055806 A CN201280055806 A CN 201280055806A CN 103946012 A CN103946012 A CN 103946012A
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Prior art keywords
peel ply
resin
compound substrate
epoxy
denier
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CN103946012B (zh
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赵艺强
达利普·库马尔·科利
库纳尔·高兰格·沙阿
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Cytec Technology Corp
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Cytec Technology Corp
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    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28—Shaping operations therefor
    • B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
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Abstract

本发明提供一种富树脂剥离层(11)，其在剥离后不会留下残余纤维且可与不同的基于树脂的复合衬底(10)一起良好地工作。所述富树脂剥离层(11)是由经不同于所述复合衬底(10)的树脂基质的树脂基质(11a)浸渍的编织织物(lib)构成。所述剥离层(11)经设计以使在从所述复合衬底(10)的表面人工去除所述剥离层(11)时，所述剥离层树脂的薄膜留在所述复合衬底的表面上以产生能够与另一个复合衬底(12)结合的可结合表面，但来自所述编织织物的纤维材料不留在所述表面上。

Description

剥离层、使用其的表面制备和结合复合结构的方法
背景技术
本发明大体来说涉及用于在结合之前复合衬底、更具体来说基于树脂的复合衬底的表面制备的剥离层。
手动磨砂、粗砂喷射和剥离层去除是制备在航天工业中用于粘着剂结合的基于树脂的复合衬底的表面的常规方法。通过剥离层去除的粘着剂结合是所述三种技术中的最常见者，这是因为其节省大量人力且产生更加均匀处理的表面。剥离层去除通常涉及将干燥的有纹理织物材料施加到基于树脂的复合衬底的结合表面上，之后固化。固化后，去除(即剥离)剥离层以显露粗糙化或有纹理结合表面。然而，干燥剥离层在剥离后往往在结合表面上留下残余断裂纤维。此导致差的粘着剂结合性质，这是因为残余纤维可存在以下缺陷：防止粘着剂完全润湿复合衬底的结合表面，借此导致粘着失效。一般工业经验为剥离层工艺关于结合性能无可靠性和预测性。
发明内容
本发明提供在剥离后不留下残余纤维且可与不同基于树脂的复合衬底良好地工作的富树脂剥离层。富树脂剥离层是由经不同于复合衬底的树脂基质的树脂基质浸渍的编织织物构成。所述剥离层经设计以使在从复合衬底表面人工去除剥离层时，剥离层树脂的薄膜保留在复合衬底表面上以产生可结合表面，但在同一表面上未留下来自编织织物的纤维材料。此富树脂剥离层能够改质不同复合物的表面用于与多种粘着剂可靠结合。因此，可将其视为“通用”剥离层。
本发明还提供使用上文论述的剥离层制备用于复合物结合的表面的方法。还揭示形成结合复合结构的方法，其包括：将剥离层施加到由纤维强化树脂构成的第一复合衬底表面上；共固化剥离层和第一复合衬底；从第一复合衬底去除剥离层，从而在复合衬底表面上留下剥离层树脂的薄层；将粘着剂膜施加到第一复合衬底的经改质表面和第二复合衬底表面中的至少一者上；使第一复合衬底的经改质表面与第二复合衬底表面接触，其间具有粘着剂膜；和固化以结合衬底。
附图说明
图1示意性显示本发明的富树脂剥离层的工作机制。
图2显示在从复合衬底去除剥离层时出现的断裂线。
图3为可用于富树脂剥离层的例示性聚酯织物的扫描电子显微镜(SEM)图像。
图4为可用于富树脂剥离层的例示性玻璃织物的扫描电子显微镜(SEM)图像。
图5为去除富树脂剥离层后经处理表面的扫描电子显微镜(SEM)图像。
图6显示实例中用于各种粘着性结合预浸材的断裂韧性(G1c)数据。
图7A和7B为显示一个实例的断裂韧性(G1c)测试后共结合预浸材的粘结失效条件的光学显微镜图像。
具体实施方式
已发现可在以下方面实现优势：用富树脂剥离层处理纤维强化树脂复合衬底以改质经处理复合衬底表面，以便有利于并促进表面处理的复合结构与第二复合衬底之间更强且更长持续时间结合。在剥离富树脂剥离层(11)后，复合衬底(10)表面由其上剩余的薄树脂膜(12)改质(图1)。图1图解说明剥离层的工作机制。去除剥离层后剩余树脂的厚度为剥离之前剥离层的初始厚度的约2％-15％。此剩余剥离层树脂层为粘着剂结合(包括共结合和二级结合)提供一致表面层。复合结合工业中的共结合意指使用粘着剂结合固化预浸材与未固化预浸材。二级结合意指使用粘着剂结合固化预浸材与另一固化预浸材。控制剥离层树脂的流变性和固化动力学以使固化期间剥离层树脂与复合衬底的树脂之间的掺和最小化，借此剥离层树脂调配物具有实质上比复合衬底的树脂调配物快的固化动力学。由于富树脂剥离层可与各种纤维强化树脂复合衬底一起使用，因此可将其视为“通用”剥离层。
本文论述的纤维强化树脂复合衬底包括通常用于制造航天结构零件的预浸材或预浸材叠层。本文所用术语“预浸材”是指经基质树脂浸渍的纤维的片或薄板。基质树脂可以未固化或部分固化状态存在。本文所用术语“预浸材叠层”是指多个彼此堆叠放置的预浸材层。叠层内的预浸材层可相对于彼此以所选定向定位。举例来说，预浸材叠层可包含具有单向纤维架构的预浸材层，其中纤维相对于叠层的最大尺寸(例如长度)以0°、90°、所选角度θ和其组合定向。应进一步理解，在某些实施例中，预浸材可具有纤维架构的任一组合，例如单向和多维。
本发明的富树脂剥离层(11)是由用树脂基质(11b)浸渍的编织织物(11a)构成，如图1中所图解说明，且根据所浸渍编织织物的特定类型，以剥离层的总重量计具有至少20重量％的树脂含量。在某些实施例中，树脂含量在20％-50％范围内。树脂调配物和织物构筑经选择以使在去除剥离层后复合衬底表面上未留下断裂纤维。剥离期间的断裂线(13)是在树脂基质(11b)内或纤维-树脂界面处，但不在织物(11a)内，如由图2所图解说明。固化后易于从复合衬底表面去除富树脂剥离层。为此，其呈现根据滚筒剥离测试ASTMD1781不大于10in-lb/英寸宽度的剥离强度。
富树脂剥离层的织物是由多根编织成编织图案的纱线构成。每一纱线是由多个加捻在一起的连续纤维丝线(单一纤维)构成。编织织物的织物重量在50-250gsm(克/m2)、优选70-220gsm范围内，且厚度在50-250μm、优选100-200μm范围内。厚度主要随重量和纤维类型变化，但还取决于编织。编织织物的纤维类型可选自各种合成材料，包括聚酯(聚对苯二甲酸乙二酯、聚对苯二甲酸丁二酯、聚对苯二甲酸三亚甲基酯、聚乳酸和其共聚物)、聚乙烯、聚丙烯、尼龙(nylon)、弹性材料，例如莱卡和高性能纤维，例如聚芳酰胺(例如克维拉(Kevlar))、聚酰亚胺、聚乙烯亚胺(PEI)、聚恶唑(例如柴隆(Zylon))、聚苯并咪唑(PBI)、聚醚醚酮(PEEK)和玻璃。纤维材料的主要要求为：材料不易碎且具有所需抗张强度。此外，织物可具有热定型饰面或其它常规饰面。
纱线支数可以线性质量密度单位丹尼尔(denier)表示。丹尼尔等于以克表示的9000米纱线的重量。数目越低，则纱线越精细。对于一卷织物，在辊方向上运行且对于辊的全长连续的纱线为经向纱线。横跨辊方向运行的短纱线称为纬向纱线。对于富树脂剥离层，基于以下特征选择织物：经向纱线的线性质量密度在50-250丹尼尔、优选70-230丹尼尔范围内，且纬向纱线的线性质量密度在50-250、优选70-230丹尼尔范围内，经向抗张强度为至少70lbf/in(1.23×104N/m)，优选≥80lbf/in(1.40×104N/m)；纬向抗张强度为至少40lbf/in(7.00×103N/m)，优选≥50lbf/in(8.76×103N/m)。编织图案不受限且可为平纹编织、斜纹编织、方平编织、锦缎编织和诸如此类。对于基于聚合物的织物，编织密度不应过高(即，紧密编织)，以便可产生纱线的低树脂浸渍和不完全浸渍。
图3为可用于富树脂剥离层的例示性聚酯织物的扫描电子显微镜(SEM)图像。此特定织物的重量为110gsm且纱线的线性质量密度为125丹尼尔。如从图3可见，此类型的聚酯织物并不紧密织造且在编织中含有微小开口。在从复合表面剥离含有此类型的聚酯织物的剥离层时，产生具有粗糙化表面且无断裂纤维的树脂膜。所述粗糙化表面为结合所需。紧密编织织物(例如玻璃织物)还可用于形成富树脂剥离层以产生为复合结合所需的表面粗糙度。图4显示可用于富树脂剥离层的例示性玻璃织物。此玻璃织物比图3中所示聚酯织物更紧密织造且更厚；其重量为205gsm且厚度为175μm。
剥离层的树脂基质是从包括以下的可固化树脂组合物形成：至少一种具有至少2的环氧官能度的环氧酚醛树脂；选自多元酚的二缩水甘油醚的二官能基环氧树脂；选自氨基苯酚的三缩水甘油醚的三官能基环氧树脂；无机填料粒子(例如发烟二氧化硅)；和固化剂。以组合物的总重量计，环氧酚醛树脂占至少40重量％、优选50-70重量％。以树脂组合物的总重量计，二官能基环氧树脂是以10-35重量％、优选15-25重量％的量存在，三官能基环氧树脂是以10-30重量％、优选10-20重量％的量存在。
环氧酚醛树脂的实例包括那些通过使酚(例如苯酚、邻甲酚、间甲酚、对甲酚、对叔丁基苯酚、对壬基苯酚、2,6-二甲苯酚、间苯二酚、双酚-A、α和β-萘酚和萘二醇)与醛(例如乙醛、甲醛、糠醛、乙二醛和对羟基苯甲醛)在酸催化剂存在下反应获得者。
适宜环氧酚醛树脂包括由以下结构I代表的环氧苯酚酚醛树脂和环氧甲酚酚醛树脂：
(I)
其中n为0到8的整数，R＝H或CH3。在R＝H时，树脂为苯酚酚醛树脂。在R＝CH3时，树脂为甲酚酚醛树脂。环氧苯酚酚醛树脂是以DEN428、DEN431、DEN438、DEN439和DEN485从多维化学公司(Dow Chemical Co)购得。环氧甲酚酚醛树脂是以ECN1235、ECN1273和ECN1299从汽巴-嘉基公司(Ciba-Geigy Corp)购得。
另一适宜环氧酚醛树脂是具有由以下结构II代表的二环戊二烯主链的烃环氧酚醛树脂：
(II)
其中n为0到7的整数。所述烃环氧酚醛树脂的市售实例包括来自泛达公司(VanticoInc)的拓为71756、拓为和拓为在一个实施例中，结构I的酚醛树脂与结构II的含有二环戊二烯的酚醛树脂结合使用。
适宜二官能基环氧树脂包括双酚A或双酚F的二缩水甘油醚，例如由多维化学公司供应的易普恩TM(EponTM)828(液体环氧树脂)、D.E.R.331、D.E.R.661(固体环氧树脂)。
氨基苯酚的三缩水甘油醚是以爱牢达MY0510、MY0500、MY0600、MY0610从亨斯迈先进材料公司(Huntsman Advanced Materials)购得。
适于剥离层树脂组合物中的环氧树脂的固化剂包括一类称作路易斯酸(Lewis Acid)的固化剂：三氟化硼(BF3)、三氯化硼(BCl3)和其复合物，例如BF3-胺复合物和BCl3-胺复合物。BF3-胺复合物的实例包括来自阿托科技(Ato-Tech)的BF3-MEA、来自空气产品公司(Air Products)的安佳(Anchor)1040(与苄胺和异丙胺复合的BF3)、来自空气产品公司的安佳1115(与异丙胺加合物复合的BF3)和也来自空气产品公司的安佳1170(与氯苄胺复合的BF3)。BCl3-胺复合物的实例包括OmincureTMBC-120。制备复合物以在正常使用条件下提供液体或固体形式。许多市售的基于环氧树脂的预浸材包括基于胺的固化剂，例如3,3’-二氨基二苯砜(DDS)和二氰基二酰胺(DICY)，其显示实质上比含有上述固化剂(例如BF3液体)的剥离层树脂调配物缓慢的固化动力学。因此，剥离层树脂调配物可足够快速地固化以使共固化工艺期间与预浸材树脂的掺和最少。
将呈颗粒形式(例如粉末)的无机填料作为流变性改良组份添加到剥离层树脂组合物中以控制树脂组合物的流动并防止其中的聚结。可用于表面膜组合物中的适宜无机填料包括发烟二氧化硅、滑石粉、云母、碳酸钙、氧化铝。以表面膜组合物的总重量计，无机填料的量可在1-10重量％、优选地1-5重量％范围内。
在一个实施例中，以树脂组合物的总重量计，剥离层的树脂组合物可包括：约45-55％苯酚酚醛环氧树脂；约5-15％含有二环戊二烯的酚醛环氧树脂、约20-30％双酚A的二缩水甘油醚；约15-25％氨基苯酚的三缩水甘油醚；约5-15％BF3固化剂和约1-5％无机填料。
此外，如果需要，还可向上述树脂组合物中添加一种或一种以上有机溶剂以有利于组份的混合。此类溶剂的实例可包括(但不限于)甲基乙基酮(MEK)、丙酮、二甲基乙酰胺和N-甲基吡咯烷酮。
富树脂剥离层可通过以下方式形成：使用常规溶剂或热熔融涂布工艺将上述树脂组合物涂布于编织织物上，以便完全浸渍织物中的纱线。如果需要，随后使湿剥离层干燥以将挥发物含量减少到优选地小于2重量％。干燥可通过在室温下风干过夜、之后在140℉-170℉下烘炉干燥或(视需要)在高温下烘炉干燥以缩短干燥时间来完成。随后，可通过将可去除的剥离型纸或合成膜(例如聚酯膜)施加于相对侧上保护干燥富树脂剥离层。此类剥离型纸或合成膜将在使用剥离层进行表面结合之前去除。将干燥剥离层施加到未固化(或部分固化)的基于树脂的复合衬底(例如基于环氧树脂的预浸材)的表面上。接下来，使剥离层与复合衬底一起经受共固化。随后去除剥离层以在复合衬底上留下树脂薄膜，借此形成准备用于与另一个复合衬底用粘着剂结合的经改质表面。
对于两个复合衬底的共结合和二级结合，将可固化粘着剂膜施加到已经固化的第一复合衬底的经改质表面与第二复合衬底表面中的至少一者上。使第一固化复合衬底的经改质表面与第二复合衬底表面接触，以使粘着剂介于衬底之间。随后实施固化以形成结合复合结构。本文所用术语“固化”(“curing”和“cure”)是指可通过加热、暴露于紫外光或辐射执行的聚合和/或交联过程。
富树脂剥离层和基于树脂的复合衬底(例如基于环氧的预浸材)的共固化可于高于230℉(110℃)、更特定来说在250℉-375℉(121℃-190℃)范围内的温度下实施。已发现本文所述富树脂剥离层的优势在于剥离层可在上述固化范围内与大多数市售预浸材共固化。所述预浸材包括以CYCOM997、CYCOM977-2、CYCOM934、CYCOM970、CYCOM5317-3、CYCOM5320-1和CYCOM851从氰特工业公司(Cytec Industries Inc.)购得的树脂预浸渍织物和/或胶带；来自赫氏公司(Hexcel Corp.)的赫普利(Hexply)8552；和来自东丽工业公司(Toray Industries Inc)的东丽(Toray)3900-2。在共固化后，固化富树脂剥离层呈现如由调节示差扫描热量测定(DSC)方法所测量的≥140℃、在一些实施例中140℃-200℃的玻璃转变温度(Tg)。
实例
以下实例阐释本文揭示的富树脂剥离层和其应用的一些实施例，且不应理解为限制本发明的范围。
实例1
富树脂剥离层是通过用树脂调配物浸渍聚酯织物制得，所述树脂调配物包含(以重量％表示)：45％苯酚-甲醛酚醛环氧树脂；11％含有二环戊二烯的酚醛环氧树脂；23％双酚A的二缩水甘油醚；14％氨基苯酚的三缩水甘油醚；5％液体BF3和2％发烟二氧化硅。聚酯织物具有以下性质：
先后使用热熔融工艺和溶剂添加工艺混合树脂调配物。在进行热熔融混合后，向树脂组合物中添加甲基乙基酮(MEK)溶剂以形成82％固体悬浮液。使用溶剂涂布工艺将湿树脂组合物涂布于织物上且于室温下干燥过夜，之后进行炉干燥过程，以将挥发物含量减少到小于2％。干燥剥离层的树脂含量为约43重量％且厚度为约140μm。
或者，还可于室温下在溶剂辅助工艺中混合树脂调配物与MEK。以与上述相同的方式将82％固体含量下的所得湿树脂混合物涂布到织物上。
如上文所论述干燥剥离层用于制备纤维强化的基于环氧的预浸材CYCOM997胶带(来自氰特工业公司)的表面。于177℃下共固化后，剥离剥离层，留下经改质表面准备用于结合。执行滚筒剥离测试(ASTM D1781)以评价剥离层的剥离强度。测试结果指示11.1牛顿(Newton)(2.5in-lb/英寸宽度)。此显示易于剥离剥离层。执行通过ATR-FTIR(衰减全反射)的表面分析以研究固化并去除剥离层后预浸材的经处理表面。发现在预浸材顶部上留下约3-10μm的剥离层树脂薄层。图5是去除富树脂剥离层后经处理表面的扫描电子显微镜(SEM)图像，其显示未留下来自织物的断裂纤维。
实例2
富树脂剥离层是通过用以下树脂调配物浸渍聚酯织物制作：以重量％表示，45％苯酚-甲醛酚醛环氧树脂；11％含有二环戊二烯的酚醛环氧树脂；22.5％双酚A的二缩水甘油醚；13.5％氨基苯酚的三缩水甘油醚；6％BF3-MEA；和2％发烟二氧化硅。织物具有以下性质：
以与实例1相同的方式将树脂调配物混合，涂布于织物上，干燥并测试。观察到类似结果-在去除富树脂剥离层后在预浸材顶部留下约3-10μm的剥离层树脂薄层，但未留下来自织物的断裂纤维。
实例3
富树脂剥离层是通过用树脂调配物浸渍聚酯织物制得，所述树脂调配物包含(以重量％表示)：44.5％苯酚-甲醛酚醛环氧树脂；9％含有二环戊二烯的酚醛环氧树脂；22％双酚A的二缩水甘油醚；18％氨基苯酚的三缩水甘油醚；4.7％液体BF3和1.8％发烟二氧化硅。聚酯织物具有以下性质：
以与实例1相同的方式将树脂调配物混合，涂布于织物上，干燥并测试。观察到类似结果-在去除富树脂剥离层后在预浸材顶部留下约3-10μm的剥离层树脂薄层，但未留下来自织物的断裂纤维。
实例4
富树脂剥离层是通过用树脂调配物浸渍聚酯织物制得，所述树脂调配物包含(以重量％表示)：44％苯酚-甲醛酚醛环氧树脂；9％含有二环戊二烯的酚醛环氧树脂；22％双酚A的二缩水甘油醚；17％氨基苯酚的三缩水甘油醚；6％BF3-MEA和2％发烟二氧化硅。聚酯织物具有以下性质：
以与实例1相同的方式将树脂调配物混合，涂布于织物上，干燥并测试。观察到类似结果-在去除富树脂剥离层后在预浸材顶部上留下约3-10μm的剥离层树脂薄层，但未留下来自织物的断裂纤维。
实例5
富树脂剥离层是通过用树脂调配物浸渍聚酯织物制得，所述树脂调配物包含(以重量％表示)：45.5％苯酚-甲醛酚醛环氧树脂；11.4％含有二环戊二烯的酚醛环氧树脂；22.8％双酚A的二缩水甘油醚；13.7％氨基苯酚的三缩水甘油醚；4.8％液体BF3和1.8％发烟二氧化硅。聚酯织物具有以下性质：
以与实例1相同的方式将树脂调配物混合，涂布于织物上，干燥并测试。观察到类似结果-在去除富树脂剥离层后在预浸材顶部上留下约3-10μm的剥离层树脂薄层，但未留下来自织物的断裂纤维。
实例6
富树脂剥离层是通过用树脂调配物浸渍玻璃织物制得，所述树脂调配物包含(以重量％表示)：44.5％苯酚-甲醛酚醛环氧树脂；8.9％含有二环戊二烯的酚醛环氧树脂；22.3％双酚A的二缩水甘油醚；17.8％氨基苯酚的三缩水甘油醚；4.7％液体BF3和1.8％发烟二氧化硅。玻璃织物具有以下性质：
以与实例1相同的方式混合树脂调配物，涂布到织物上。干燥后，干燥剥离层的树脂含量为约28重量％且厚度为约195μm。随后以与实例1相同的方式测试富树脂剥离层。观察到类似结果-在去除富树脂剥离层后在预浸材顶部上留下约3-10μm的剥离层树脂薄层，但未留下来自织物的断裂纤维。
实例7
富树脂剥离层是通过用实例6中揭示的树脂调配物浸渍聚酯织物制得。聚酯织物具有以下性质：
以与实例1相同的方式将树脂调配物混合，涂布于织物上，干燥并测试。观察到类似结果-在去除富树脂剥离层后在预浸材顶部上留下约3-10μm的剥离层树脂薄层，但未留下来自织物的断裂纤维。
实例8
双重叠剪切测试
使用市售粘着剂FM318M.05psf(来自氰特工业公司)将CYCOM970预浸材(来自氰特工业公司)彼此结合。于每一测试温度下测试3到4个结合预浸材试样。在结合之前，使用如实例1中论述的富树脂剥离层制备预浸材的结合表面。表2显示基于双重叠剪切测试(ASTM D3528)的23℃、-55℃和72℃测试温度下的平均剪切数据。如表2中可见，剥离层促进各种测试温度下的粘结失效。
表2
测试温度 平均剪切(MPa)
23℃ 35.5
-55℃ 32.9
72℃ 31.7
实例9
双悬臂梁测试
结合预浸材试样是使用各种市售预浸材材料和市售粘着剂FM309-1(来自氰特工业公司)形成。在结合之前，使用如实例1中论述的富树脂剥离层制备预浸材的结合表面。于23℃和-55℃下实施双悬臂梁测试(ASTM D5528)以测量结合预浸材的板间断裂韧性(G1c)且结果示于图6中。
使用结构粘着剂FM309-1M.05psf使CYCOM5317-6预浸材(来自氰特工业公司)共结合。在共结合之前，使用利用图4中所示玻璃织物形成的富树脂剥离层以在一个预浸材上制备结合表面。图7A和7B显示共结合预浸材的G1c测试后的粘结失效条件。
术语“第一”、“第二”和诸如此类在本文中并不表示任何次序、量或重要性，而是用于将元素彼此区分，且术语“一”(“a”和“an”)在本文中并不表示限制量，而是表示存在所提及项目中的至少一者。与量连用的修饰词“约”(“approximately”或“about”)涵盖所述值且具有由上下文指定的含义(例如，包括与特定量测量相关的误差度)。如本文所用后缀“(s)”打算包括单数和多个其修饰的项，借此包括所述项中的一种或一种以上(例如，金属包括一种或一种以上金属)。本文中揭示的范围具涵盖性且可独立组合(例如，“高达约25wt％或更特定来说约5wt％到约20wt％”的范围包括“约5wt％到约25wt％”范围的端点和所有中间值等)。
尽管本文阐述各种实施例，但从说明书应了解，可由所属领域技术人员作出要素的各种组合、其中的改变或改良，且此在本发明范围内。另外，为适应特定情况或材料还可对本发明的教示实施多项改良，此并不背离本发明的基本范围。因此，本文并非打算将本发明限制于所揭示的作为实施本发明的最好设想模式的特定实施例，而是打算使本发明包括所有属于所附权利要求书范围内的实施例。

Claims (21)

1.一种剥离层系统，其用于各种复合衬底的表面制备，所述系统包含：
(a)复合衬底，其包含经固化的第一树脂基质浸渍的强化纤维；和
(b)粘附到所述复合衬底的表面的可去除的富树脂剥离层，所述剥离层包含经不同于所述第一树脂基质的经固化的第二树脂基质浸渍的编织织物，
借此在从所述复合衬底的表面人工去除所述剥离层时，所述第二树脂基质的薄膜留在所述复合衬底的表面上，以提供能够与另一个复合衬底共结合并二级结合的可结合表面，
其中所述第二树脂基质是从包含以下的树脂组合物形成：
至少一种具有至少2的环氧官能度的环氧酚醛树脂；
选自多元酚的二缩水甘油醚的二官能基环氧树脂；
选自氨基苯酚的三缩水甘油醚的三官能基环氧树脂；
固化剂；和
无机填料粒子；
其中所述剥离层具有以所述剥离层的总重量计至少20重量％的树脂含量，且
其中所述编织织物包含多根编织成编织图案的纱线，所述纱线具有≥70lbf/in(1.23×104N/m)的经向抗张强度、≥40lbf/in(7.00×103N/m)的纬向抗张强度、在50丹尼尔到250丹尼尔范围内的经向线性质量密度和在50丹尼尔到250丹尼尔范围内的纬向线性质量密度。
2.根据权利要求1所述的系统，其中所述纱线具有≥80lbf/in(1.40×104N/m)的经向抗张强度、≥50lbf/in(8.76×103N/m)的纬向抗张强度、在70丹尼尔到230丹尼尔范围内的经向线性质量密度和在70丹尼尔到230丹尼尔范围内的纬向线性质量密度。
3.根据权利要求1或2所述的系统，其中留下的所述第二树脂基质的薄膜具有为在去除之前所述剥离层的初始厚度的约2％到15％的厚度。
4.根据权利要求1到3中任一权利要求所述的系统，其中所述树脂组合物包含至少一种选自由以下结构表示的环氧苯酚酚醛树脂和环氧甲酚酚醛树脂的环氧酚醛树脂：
其中n为0到8的整数，R＝H或CH3。
5.根据权利要求1到4中任一权利要求所述的系统，其中所述树脂组合物进一步包含由以下结构表示的含有二环戊二烯的酚醛环氧树脂：
其中n＝0到7的整数。
6.根据权利要求1到5中任一权利要求所述的系统，其中所述编织织物具有在50gsm到250gsm范围内的织物重量。
7.根据权利要求1到6中任一权利要求所述的系统，其中所述编织织物具有在70gsm到220gsm范围内的织物重量。
8.根据权利要求1到7中任一权利要求所述的系统，其中所述编织织物具有在50μm到250μm范围内的织物厚度。
9.根据权利要求1到8中任一权利要求所述的系统，其中所述编织织物具有在100μm到200μm范围内的织物厚度。
10.根据权利要求1到9中任一权利要求所述的系统，其中所述编织织物的所述纱线是由选自由以下组成的群组的材料制造：聚酯、聚乙烯、聚丙烯、尼龙、弹性材料、聚芳酰胺、聚酰亚胺、聚乙烯亚胺PEI、聚噁唑、聚苯并咪唑PBI、聚醚醚酮PEEK和玻璃。
11.根据权利要求1到10中任一权利要求所述的系统，其中所述剥离层具有以所述剥离层的总重量计至少20重量％的树脂含量。
12.根据权利要求1到11中任一权利要求所述的系统，其中所述剥离层具有以所述剥离层的总重量计在20重量％到50重量％范围内的树脂含量。
13.根据权利要求1到12中任一权利要求所述的系统，其中所述剥离层具有≥140℃的玻璃转变温度(Tg)。
14.根据权利要求1到13中任一权利要求所述的系统，其中所述剥离层具有在140℃到200℃范围内的玻璃转变温度(Tg)。
15.根据权利要求1到14中任一权利要求所述的系统，其中所述固化剂选自由BF3、BCl3和其复合物组成的群组。
16.根据权利要求1到15中任一权利要求所述的系统，其中所述第二树脂基质是从包含以下的树脂组合物形成：
具有至少2的环氧官能度的环氧苯酚酚醛树脂；
具有至少2的环氧官能度的含有二环戊二烯的环氧酚醛树脂；
双酚A的二缩水甘油醚；
氨基苯酚的三缩水甘油醚；
选自由BF3、BCl3和其复合物组成的群组的固化剂；和
发烟二氧化硅。
17.根据权利要求1到16中任一权利要求所述的系统，其中以所述组合物的总重量计，所述酚醛树脂占至少20重量％。
18.一种用于各种复合衬底的表面制备的方法，其包含：
(a)提供包含经第一树脂基质浸渍的强化纤维的复合衬底；
(b)放置富树脂剥离层以与所述复合衬底的表面接触，所述剥离层是通过用包含以下的可固化树脂组合物浸渍编织织物形成：
至少一种具有至少2的环氧官能度的环氧酚醛树脂；
选自多元酚的二缩水甘油醚的二官能基环氧树脂；
选自氨基苯酚的三缩水甘油醚的三官能基环氧树脂；
固化剂；和
无机填料粒子，
其中所述编织织物包含多根编织成编织图案的纱线，所述纱线具有≥70lbf/in(1.23×104N/m)的经向抗张强度、≥40lbf/in(7.00×103N/m)的纬向抗张强度、在50丹尼尔到250丹尼尔范围内的经向线性质量密度和在50丹尼尔到250丹尼尔范围内的纬向线性质量密度；
(c)共固化所述剥离层和所述复合衬底；和
(d)从所述复合衬底的所述表面去除所述剥离层，以使来自所述剥离层的树脂的薄膜留在所述复合衬底的表面上，以提供能够与另一个复合衬底共结合并二级结合的可结合表面。
19.根据权利要求18所述的方法，其中所述共固化是在高于230℉(110℃)的温度下进行。
20.根据权利要求18或19所述的方法，其中所述共固化是在250℉到375℉(121℃到190℃)的温度范围内进行。
21.一种形成结合复合结构的方法，其包含：
(a)提供包含经第一树脂基质浸渍的强化纤维的第一复合衬底；
(b)提供包含经第二树脂基质浸渍的强化纤维的第二复合衬底；
(c)放置富树脂剥离层以与所述第一复合衬底的表面接触，所述剥离层是通过用包含以下的可固化树脂组合物浸渍编织织物形成：
至少一种具有至少2的环氧官能度的环氧酚醛树脂；
选自多元酚的二缩水甘油醚的二官能基环氧树脂；
选自氨基苯酚的三缩水甘油醚的三官能基环氧树脂；
固化剂；和
无机填料粒子，
其中所述编织织物包含多根编织成编织图案的纱线，所述纱线具有≥70lbf/in(1.23×104N/m)的经向抗张强度、≥40lbf/in(7.00×103N/m)的纬向抗张强度、在50丹尼尔到250丹尼尔范围内的经向线性质量密度和在50丹尼尔到250丹尼尔范围内的纬向线性质量密度；
(d)在高于230℉(110℃)的温度下共固化所述剥离层和所述第一复合衬底；
(e)从所述复合衬底的所述表面去除所述剥离层，以使来自所述剥离层的树脂的薄膜留在所述复合衬底的表面上以提供可结合表面，但来自所述编织织物的纤维材料不留在所述表面上；
(f)将粘着膜施加于所述第一衬底的所述可结合表面或所述第二衬底的表面上；
(g)放置所述第一复合衬底的所述可结合表面以与所述第二复合衬底的表面接触，其间具有所述粘着膜；和
(h)固化以结合所述第一和第二衬底。
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