CN112646091A - 树脂组合物及使用其制作的低流胶半固化片 - Google Patents
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Abstract
本发明开发了一种树脂组合物,以重量计,包括如下组分:(a)环氧树脂;(b)含马来酰亚胺基的酚醛树脂;(c)环氧树脂固化促进剂;(d)韧性树脂;(e)含有不饱和双键的液体树脂。本发明通过在树脂体系中引入了强极性且帯可反应双键的对羟基苯基马来酰亚胺结构,实验证明:使用该树脂组合物制备的低流胶半固化片和软板聚酰亚胺面结合力优异,同时还备有优异的耐热性能、韧性和掉粉性,非常适用于刚挠结合印制电路板等特殊PCB的制作,具有很强的加工适应性和质量可靠性。
Description
技术领域
本发明涉及电子材料技术领域,具体涉及一种树脂组合物及使用其制作的低流胶半固化片。
背景技术
目前,刚挠结合印制电路板(又称为刚挠结合板)是当下需求及发展正旺的印制电路板。刚挠结合印制电路板是将薄层状的挠性底层和刚性底层结合,再层压入一个单一组件中,形成的电路板,刚挠结合板改变了传统的平面式的设计概念,扩大到立体的3维空间概念,在给产品设计带来巨大的方便的同时,也带来了巨大的挑战。典型的(四层)刚挠结合印刷电路板有一个聚酰亚胺核,它的上下两面都有覆着铜箔。外部刚性层由单面的FR4组成,它们被层压入挠性核的两面,组装成多层的PCB。在制作多层刚挠结合板时,挠性层的加工工艺又与外部FR4层截然不同。由不同材料制作的各个层面必须通过层压聚集在一起,然后再钻孔、电镀。因此,制作一个典型的四层刚挠结合印刷电路板的时间,可能比制作一个标准的四层刚性印刷电路板长5至7倍。目前,刚挠结合板的应用范围主要包括:航空航天,如高端的飞机挂载武器导航系统,先进医疗设备,数码相机,可携式摄相机和高品质MP3播放器。刚挠结合板最常用于制造军用飞机和医疗设备。刚挠结合板为军用飞机的设计带来了巨大的益处,因为它在提高连接可靠度的同时还减轻了重量。
刚挠结合印制电路板在加工制作时需要使用粘结材料将软板和硬板粘结起来,现阶段最常用的粘结材料是低流动度半固化片。相对于常规FR-4半固化片来说,低树脂流动性半固化片需要具备在高温高压下流胶极小或几乎不流胶的特性,同时还需要具备很好的粘结力,优异的韧性及低掉粉性。由于低流动度半固化片在高温高压下流胶极小或几乎不流胶的特性,通常需要提高树脂体系的反应程度,这会导致粘结片的粘结能力下降。特别是低流胶半固化片与软板聚酰亚胺面的结合力,是严重影响软硬结合板可靠性的因素之一。
为了解决低流胶半固化片与软板聚酰亚胺面结合力的问题,中国发明专利申请CN104164087A中使用烯丙基改性的双马来酰亚胺树脂和特殊结构的环氧树脂组成的热固性树脂组合物,该专利中主要是使用特殊结构的环氧树脂来改善低流胶半固化片与软板聚酰亚胺面结合力的问题。然而,该专利中的技术方案存在韧性不足而导致的掉粉性大的问题,会严重的影响印制电路板的加工性能。为了改善低流胶半固化片的韧性问题,加入过多的双酚A型环氧树脂,这又会导致玻璃化转变温度变低的问题。
为了改善低流胶半固化片的韧性及掉粉性,现有技术通常会在树脂体系中加入酚氧树脂、丁腈橡胶、聚丙烯酸酯树脂等大分子聚合物,然而,大分子聚合物会导致树脂体系对玻纤布的浸润性降低,在半固化片的内部形成树脂空洞等缺陷,这会导致低流胶半固化片压合后可靠性的下降。
因此,开发一种新的树脂组合物及使用其制作的低流胶半固化片,在提高低流胶半固化片和软板聚酰亚胺面结合力的同时,还可以保证低流胶半固化片具备优异耐热性能、韧性及低掉粉性,且可以避免树脂体系对玻纤布的浸润性降低的问题,显然具有积极的现实意义。
发明内容
本发明的发明目的是提供一种树脂组合物及使用其制作的低流胶半固化片。
为达到上述发明目的,本发明采用的技术方案是:一种树脂组合物,以重量计,包括如下组分:
(a)环氧树脂,100份;
(b)含马来酰亚胺基的酚醛树脂;
(c)环氧树脂固化促进剂,0.05~5份;
(d)韧性树脂;
(e)含有不饱和双键的液体树脂;
所述组分(b)的添加量如下:所述环氧树脂与含马来酰亚胺基的酚醛树脂的官能当量比为1:0.5~5;
所述组分(d)的添加量如下:所述韧性树脂与其他组分的重量比为1~20:100;
所述组分(b)的结构式如下:
所述组分(e)的添加量如下:含有不饱和双键的液体树脂和含马来酰亚胺基的酚醛树脂双键官能当量比为1:0.5~10。
上文中,所述环氧树脂可以选自含磷环氧树脂、含氮环氧树脂、多官能环氧树脂、双酚A环氧树脂、双酚F环氧树脂、四苯基乙烷环氧树脂、三苯基甲烷环氧树脂、联苯型环氧树脂、萘环型环氧树脂、双环戊二烯型环氧树脂、异氰酸酯型环氧树脂、酚醛环氧树脂、甲基酚醛环氧树脂、双酚型酚醛环氧树脂、聚苯醚改性环氧树脂、脂环族类环氧树脂、烯丙基缩水甘油型环氧树脂、缩水甘油胺型环氧树脂、缩水甘油酯型环氧树脂中的一种或几种。
为了使得到的低流胶半固化片和软板聚酰亚胺面结合力良好,优选的,所述环氧树脂中包含DOPO-HQ型含磷环氧树脂、联苯型环氧树脂、双酚型酚醛环氧树脂中的一种或者几种;更有选的,所述的环氧树脂包含双酚型酚醛环氧树脂,所述双酚型酚醛环氧树脂可以是双酚A型酚醛环氧树脂、双酚F型酚醛环氧树脂、双酚S型酚醛环氧树脂,二羟基二苯醚型酚醛环氧树脂。
为了使得到的低流胶半固化片中树脂体系对玻纤布的浸润性良好,避免在半固化片的内部形成树脂空洞等缺陷,优选的,所述环氧树脂中包含双酚A环氧树脂、双酚F环氧树脂、二羟基二苯醚环氧树脂、烯丙基缩水甘油醚、N,N,N',N'-四环氧丙基-4,4'-二氨基二苯甲烷等小分子环氧树脂中的一种或几种。
优选的,为了使得到的低流胶粘结片具有更好的抗发粘特性和耐热性能,当所述环氧树脂中包含双酚A环氧树脂、双酚F环氧树脂、二羟基二苯醚环氧树脂、烯丙基缩水甘油醚中的一种或几种时,所述的双酚A环氧树脂、双酚F环氧树脂、二羟基二苯醚环氧树脂、烯丙基缩水甘油醚的添加量为总树脂组合物总固体量的1~15%。
上文中,所述组分(b)的添加量如下:所述环氧树脂与含马来酰亚胺基的酚醛树脂的官能当量比为1:0.5~5;优选为1:0.6~4,更优选为1:0.8~3,优选为1:1~2。
所述组分(d)的添加量如下:所述韧性树脂与其他组分的重量比为1~20:100;优选为1~15:100,更优选为2~10:100,更优选为3~8:100,更优选为4~6:100。
所述组分(e)的添加量如下:含有不饱和双键的液体树脂和含马来酰亚胺基的酚醛树脂双键官能当量比为1:0.5~10。优选为100:1~8,更优选为100:2~5,更优选为100:3~4。
本发明的树脂组合物还可以包括阻燃剂,所述阻燃剂可以是磷系阻燃剂、氮系阻燃剂、有机硅阻燃剂和无机系阻燃剂等。其中,磷系阻燃剂可以是含磷环氧树脂、含磷酚醛树脂、无机磷、磷酸酯化合物、膦酸化合物、次膦酸化合物、氧化膦化合物、以及9,10-二氢-9氧杂-10-膦杂菲-10-氧化物、10-(2,5二羟基苯基)-9,10-二氢-9氧杂-10-膦杂菲-10-氧化物、10-苯基-9,10-二氢-9氧杂-10-膦杂菲-10-氧化物、三(2,6二甲基苯基)磷腈等有机含磷化合物。氮系阻燃剂可以是三嗪化合物、氰尿酸化合物、异氰酸化合物、吩噻嗪等。有机硅阻燃剂可以是有机硅油、有机硅橡胶、有机硅树脂等。无机阻燃剂可以是氢氧化铝、氢氧化镁、氧化铝、氧化钡等。
上述技术方案中,所述环氧树脂固化促进剂选自咪唑类促进剂、胺类促进剂、锡类促进剂、改性DBN/DBU中的一种或几种。所述咪唑类促进剂可以是2-甲基咪唑、2-乙基-4-甲基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑等。所述胺类促进剂可以是三乙烯二胺、N-氨基吗啡啉、三氟化硼乙胺等。所述锡类促进剂可以是有二月桂酸二丁基锡、辛酸亚锡等。
优选的,所述Ar*为苯环。
优选的,所述Ar选自如下结构中的一种或几种:
优选的,所述组分(b)的结构式中,x结构单元和y结构单元的摩尔比为1:1~5。
上述技术方案中,所述环氧树脂选自DOPO-HQ改性环氧树脂、联苯型环氧树脂、双酚型酚醛环氧树脂、含双酚A环氧树脂、双酚F环氧树脂、二羟基二苯醚环氧树脂、烯丙基缩水甘油醚中的一种或几种。
上述技术方案中,所述韧性树脂选自酚氧树脂、丁腈橡胶、核壳橡胶、聚丙烯酸酯树脂中的一种或几种。
所述酚氧树脂可以选自烯丙基酚氧树脂、含磷酚氧树脂、含硫酚氧树脂、双酚A缩水甘油醚型、双酚F缩水甘油醚型或联苯型缩水甘油醚型酚氧树脂中的一种或几种;优选的,其重均分子量为5000~70000。
所述丁腈橡胶可以选自羧基丁腈橡胶、氨基丁腈橡胶或者其他改性丁腈橡胶,优选分子量较大的固体橡胶或改性固体橡胶,更优选的,其重均分子量为50000~300000。
所述聚丙烯酸酯树脂可以选自丙烯酸酯型均聚物、其他乙烯基单体和丙烯酸酯的共聚物。优选的,所述聚丙烯酸酯为丙烯酸酯三嵌段共聚物。所述丙烯酸酯三嵌段共聚物是指包含中间柔韧段和两端为硬段的三嵌段共聚物。中间柔韧嵌段可以是聚丙烯酸丁酯、聚甲基丙烯酸丁酯、聚丙烯酸乙酯、聚丙烯酸异辛酯、聚丙烯酸2-乙基己酯、聚甲基丙烯酸2-乙基己酯、或聚丁二烯等柔韧性好的嵌段;两端的硬段可以是聚甲基丙烯酸酯、聚苯乙烯等刚性较好的嵌段。优选的,所述丙烯酸酯三嵌段共聚物为聚苯乙烯-聚丁二烯-聚甲基丙烯酸酯三嵌段共聚物、聚甲基丙烯酸甲酯-聚丙烯酸丁酯-聚甲基丙烯酸甲酯三嵌段共聚物。优选的,所述丙烯酸酯三嵌段共聚物的重均分子量为10000~800000,更优选的,所述丙烯酸酯三嵌段共聚物的重均分子量为10000~300000。当分子量较大时,丙烯酸酯的韧性和耐热性能较好,但是可能会存在其与其他树脂的相容性问题。为了提高丙烯酸酯和其他树脂的相容性,可以对丙烯酸酯嵌段共聚物进行官能化改性,可以羟基官能化、羧基官能化、氨基官能化、环氧基官能化改性。聚丙烯酸酯树脂的添加量,相对于100重量份的环氧树脂,优选为1~10重量份。当丙烯酸酯的分子量较高时,为改善丙烯酸酯和其他树脂的相容性,可以适当降低丙烯酸酯的加入量,优选的添加量为1~5重量份。
上述技术方案中,还包括共固化剂,所述共固化剂的添加量为:按照官能当量计算,在所述含马来酰亚胺基的酚醛树脂和共固化剂总官能当量和所述环氧树脂的官能当量比为0.5~5:1的前提下,含马来酰亚胺基的酚醛树脂占固化剂总官能当量的50~90%。优选为60~80%,更优选为70~77%。
所述共固化剂可以是:脂肪族胺、芳香族胺、脂环族胺、杂环胺、聚酰胺-多胺、改性多胺化合物、双氰胺、芳香族酸酐、脂环族酸酐、脂肪族酸酐、聚酰胺树脂、线型酚醛树脂、苯并恶嗪树脂、聚酚树脂、芳胺甲醛树脂、聚硫化合物、聚酯树脂、潜伏型固化剂、阻燃固化剂、活性酯固化剂中的一种或任意几种的混合物。所述共固化剂优选为胺类固化剂。
为了使得得到的低流胶半固化片和软板聚酰亚胺面结合力良好,优选的,所述共固化剂为双氰胺。
为了使得得到的高耐热性的低流胶半固化片,同时保证低流胶半固化片和软板聚酰亚胺面具有良好的结合力,优选的,所述共固化剂为二氨基二苯砜、二氨基二苯醚。
上述技术方案中,还包括填料,以重量计,填料占树脂组合物的5~80%。所述填料可以选自结晶型二氧化硅、熔融二氧化硅、球形二氧化硅、氧化铝、氢氧化铝、氮化铝、氮化硼、二氧化钛、钛酸锶、钛酸钡、硫酸钡、滑石粉、硅酸钙、碳酸钙、云母、聚四氟乙烯、石墨烯中的一种或几种。所述填料可以经硅烷偶联剂进行表面处理,可以直接投入或预先制备填料分散液或制成膏体投入树脂组合物中。所述填料的粒径优选为0.5~10微米(粒径D50)。为了使得得到的低流胶半固化片具有优异的掉分率,填料含量优选为:填料占树脂组合物的5~10%。为了使得得到的低流胶半固化片具有优异的刚性和导热性,填料含量占比优选为50~70%。为了得到的低流胶半固化片具有优异导热性同时还具有优异的层间粘结力、铜箔粘结力,优选的填料为氧化铝。
此外,本发明的树脂组合物还可以包含分散剂、偶联剂、消泡剂、流平剂、染色剂、相容剂、UV阻挡剂等特殊功能助剂。
优选的,当所述环氧树脂中含有双酚A环氧树脂、双酚F环氧树脂、二羟基二苯醚环氧树脂、烯丙基缩水甘油醚、N,N,N',N'-四环氧丙基-4,4'-二氨基二苯甲烷中的一种或几种时,所述双酚A环氧树脂、双酚F环氧树脂、二羟基二苯醚环氧树脂、烯丙基缩水甘油醚、N,N,N',N'-四环氧丙基-4,4'-二氨基二苯甲烷的添加量为总树脂组合物总固体量的1~15%。
上述技术方案中,所述含有不饱和双键的液体树脂选自丙烯酸树脂、烯丙基树脂、苯乙烯及取代苯乙烯树脂中的一种或几种。所述不饱和双键的液体树脂的添加量,按照含有不饱和双键的液体树脂和其他总树脂重量比的1~10%添加。
所述丙烯酸树脂可以是丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟丙酯、甲基丙烯酸缩水甘油酯、甲基丙烯酸异冰片酯、丙烯酸苯氧基乙酯、甲基丙烯酸四氢呋喃酯、二乙二醇类丙烯酸酯、三乙二醇类丙烯酸酯、聚乙二醇类丙烯酸酯、二乙丙醇类丙烯酸酯、三乙丙醇类丙烯酸酯、新戊二醇二丙烯酸酯、邻苯二甲酸二乙二醇二丙烯酸酯、三羟甲基丙烷三丙烯酸酯、季戊四醇三丙烯酸酯、季戊四醇四丙烯酸酯、甲基丙烯酸磷酸酯、烷氧基三官能团丙烯酸酯、脂肪族单丙烯酸酯、叔胺基丙烯酸酯、烷氧基化二丙烯酸酯中的一种或任意种。为了得到的低流胶半固化片具有更好的粘结性能,优选的,所述丙烯酸树脂为丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟丙酯、甲基丙烯酸缩水甘油酯、甲基丙烯酸磷酸酯中的一种或任意种。为了得到的低流胶半固化片具有更好的韧性,优选的,所述丙烯酸树脂为聚乙二醇类丙烯酸酯。为了得到的热固性树脂组合物具有更好的填料分散性,优选的,所述丙烯酸酯树脂为烷氧基化二丙烯酸酯。
所述烯丙基树脂可以选自烯丙基双酚A、烯丙基双酚S、二烯丙基二苯醚、烯丙基甲酚、烯丙基缩水甘油醚、烯丙基树脂改性马来酰亚胺预聚物中的一种或几种。为了使得得到的低流胶半固化片和软板聚酰亚胺面具有更好的粘结力,优选的,所述烯丙基树脂为二烯丙基二苯醚、烯丙基甲酚改性马来酰亚胺预聚物。为了使得得到的树脂组合物具有更好玻纤布浸润性,优选的,所述烯丙基树脂为烯丙基甲酚及烯丙基甲酚改性马来酰亚胺预聚物。
优选的,为得到的低流胶半固化片和软板聚酰亚胺面具有更好的粘结力,所述取代苯乙烯优选的为羟基苯乙烯。
本发明同时请求保护一种采用上述树脂组合物制备的低流胶半固化片。
上述低流胶半固化片的制备方法为如下:将所述树脂组合物和溶剂加入到混胶釜中,固体含量为40~70%,搅拌均匀,并熟化4-8小时,制成树脂组合物胶液;继而将增强材料浸渍在上述树脂组合物胶液中,然后将浸渍后的增强材料在100~200℃环境下按照设定的程序反应干燥后,即可得本发明的低流胶半固化片。所述增强材料为天然纤维、有机合成纤维、有机织物或者无机织物。所述稀释剂选自N,N-二甲基甲酰胺、N,N-二甲乙酰胺、丙酮、丁酮、丙二醇甲醚、乙二醇乙醚、甲醇、乙醇、苯、甲苯、对二甲苯、四氢呋喃、N-甲基吡咯烷酮、二甲基亚砜中的一种或几种。
由于上述技术方案运用,本发明与现有技术相比具有下列优点:
1.本发明开发了一种新的用于制备低流胶半固化片的树脂组合物,通过在树脂体系中引入了强极性且帯可反应双键的对羟基苯基马来酰亚胺结构,实验证明:使用该树脂组合物制备的低流胶半固化片和软板聚酰亚胺面结合力优异,同时还备有优异的耐热性能、韧性和掉粉性,非常适用于刚挠结合印制电路板等特殊PCB的制作,具有很强的加工适应性和质量可靠性;
2.本发明采用含马来酰亚胺基的酚醛树脂作为环氧树脂的固化剂,配合环氧树脂固化促进剂,得到了具备优异耐热性能、韧性及低掉粉性的低流胶半固化片,而且避免了树脂体系对玻纤布的浸润性降低的问题,显然具有积极的现实意义;
3.本发明在树脂体系中引入了强极性且帯可反应双键的对羟基苯基马来酰亚胺结构,同时引入了含有不饱和双键的液体树脂,在明显改善了不流胶粘结片浸润性的同时,由于不饱和双键的液体树脂可以和马来酰亚胺的双键反应,进而保证了优异的耐热性能;
4.本发明的低流胶半固化片的制备工艺简单易行,且成本较低,适于推广应用。
具体实施方式
下面结合实施例对本发明作进一步描述:
实施例
含马来酰亚胺基的酚醛树脂的化学结构式如下:
其中,x、y为1-20整数,y为0-20的整数,n为1-10的整数。当x与y量中结构单元的比例为1:1时,得到的含马来酰亚胺基的酚醛树脂标记为B-1,理论羟基官能当量为154g/mol,理论马来酰亚胺双键官能当量为308g/mol;当x与y量中结构单元的比例为1:5时,理论羟基官能当量为122g/mol,理论马来酰亚胺双键官能当量为732g/mol;得到的含马来酰亚胺基的酚醛树脂标记为B-2。参照下面的方法,同样的条件下合成得到普通的苯酚酚醛树脂标记为B-3,理论羟基官能当量为106g/mol。
上述化合物可以按照现有电子材料用热固性酚醛树脂的合成方法合成,具体合成方法可以是:在安装有温度计、冷凝管、搅拌器的烧瓶中投入要求配比量的N-(4-羟基苯基)马来酰亚胺、苯酚和草酸,混合搅拌均匀后,置于70℃的恒温水浴中;然后,在搅拌下,用0.5小时向烧瓶中滴加甲醛溶液(125mL,酚/醛的比例为1/0.8);加完甲醛后,维持70℃的温度和搅拌条件,反应15小时;接着,用400mL丙酮将反应产物溶解稀释,然后再用40%的甲醇的水溶液沉淀反应产物;重复以上溶解-沉淀操作3~5次,将其过滤、分离、干燥,即可得到纯净的前述结构式所示的含马来酰亚胺基的酚醛树脂。
取上述含马来酰亚胺基的酚醛树脂B-1按照现有技术中酚羟基酯化的方法,将马来酰亚胺酚醛树脂中的酚羟基酯化后得到活性酯化后的含马来酰亚胺树脂,标记为B-4,理论酯基官能当量为208g/mol,理论马来酰亚胺双键官能当量为415g/mol。
根据表1和表2的配方,将上述合成得到的含马来酰亚胺基的酚醛树脂、环氧树脂、环氧树脂固化促进剂、溶剂及其他组分混合均匀制备成50%固含量的树脂组合物,得到实施例1~11。同时在同样的条件下制备得到对比例1~5的树脂组合物胶液。表1和表2中的其他原材料来源如下:
A-1:含磷环氧树脂,同宇新材料;
A-2:双酚A酚醛型环氧树脂,迈图;
A-3:双酚A环氧树脂,国都化工;
A-4:联苯环氧,迈图;
B-1:含马来酰亚酚醛树脂,自制;
B-2:含马来酰亚酚醛树脂,自制;
B-3:酚醛树脂,自制;
B-4:多马来酰亚胺活性酯,自制;
C-1:咪唑,四国化成;
D-1:CTBN,瑞翁;
E-1:丙烯酸丁酯,国产试剂;
E-2:烯丙基双酚A,山东莱玉;
E-3:对羟基苯乙烯,国产试剂
F-1:DICY,宁夏大荣;
F-2:DDS(二氨基二苯砜),河北建兴;
H-1:球硅,锦艺;
I-1:BMI,西安双马;
然后,使用电子级2116玻纤布作为增强材料含浸上述树脂溶液,而后按照一定的温度、时间程序将预浸料于烘箱中加热固化即得低流胶半固化片,将部分半固化片按下述条件压制成层压板,然后通过下述方法评价半固化片和层压板的各项性能。半固化片及层压板的具体制作条件如下:
预浸料半固化条件:130℃/3-10min+190℃/2-10min;板材的制作条件:叠构为1/2OZ Cu+2x2116粘结片+1/2OZ Cu,铜箔厚度为1OZ,成型后板材厚度:0.25mm,固化条件为温升3-5℃/min,料温220℃/1-2h;PI结合力测试板的制作条件:叠构为1/2OZ Cu+25umPI膜+1x2116+1/2OZ Cu,固化条件为温升3-5℃/min,料温220℃/1-2h。
半固化片测试项目:溢胶量、掉粉率。
<溢胶量>的测定:将PP制成100mm*100mm大小的正方形样,在中间位置冲一个1英寸的圆孔,然后将PP样按照“钢板+覆铜板+PP样+离型膜+缓冲材料+钢板”的叠好方式叠在一起,使用设定好温度/压力/时间的的压机压合,压合完成后取出试样圆孔位置的溢胶量,以评价其在热压条件下的流胶大小。
<韧性(脱粉率)>的测定:以半固化片经冲切/剪切处理后树脂粉脱落程度为判断依据。具体测试方法为,取10cm*10cm大小的半固化片4小片,称重并记录为m1。用剪刀在其某一边剪出9cm纵深的缺口,共剪29刀,每片样品制成含30条长9cm的小条,每片均做同样处理。手持处理好的样品以腕部为中心位置上下振动30次,一个来回记为一次振动。完成后再次称重并记录为m2,按(m1-m2)/m1*100%计算即得该半固化片的脱粉率。
<耐热性>:用玻璃化转变温度(Tg)表征耐热性,采用DMA法,按照IPC-TM-6502.4.25所规定方法进行测试。
<PI膜剥离强度>测定:模拟软硬结合板的叠构情况,将低流胶粘结片和PI覆盖膜的无胶面压合在一起,使用万能材料试验机,90°剥离测试低流胶粘结片和PI覆盖膜之间的粘结强度。
<玻纤布浸润性>测定:使用单张2116的低流胶粘结片在设定好的程序下压合成层压板,蚀刻掉铜箔后,制成50mmx10mm的试样,在湿法显微镜下查看基材中白纹的数量。
表1
表2
从上表可见,是采用本发明的方案制得的低流胶粘结片,相比对比例1~5,实施例1~11的低流胶粘结片都具有更优异的玻纤布浸润性,相比对比例1、对比例2、对比例4具有更优异的耐热性能、更优异的PI覆盖膜粘结强度,相比对比3具有更优异的PI覆盖膜粘结强度,相比对比例5具有更低的掉粉率。由此可见,采用本发明的方案制得的低流胶粘结片兼具优异的耐热性能、PI覆盖膜粘结强度、玻纤布浸润性和很低的掉粉率。
对所公开的实施例的上述说明,使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的,本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下,在其它实施例中实现。因此,本发明将不会被限制于本文所示的这些实施例,而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (10)
1.一种树脂组合物,其特征在于,以重量计,包括如下组分:
(a)环氧树脂,100份;
(b)含马来酰亚胺基的酚醛树脂;
(c)环氧树脂固化促进剂,0.05~5份;
(d)韧性树脂;
(e)含有不饱和双键的液体树脂;
所述组分(b)的添加量如下:所述环氧树脂与含马来酰亚胺基的酚醛树脂的官能当量比为1:0.5~5;
所述组分(d)的添加量如下:所述韧性树脂与其他组分的重量比为1~20:100;
所述组分(e)的添加量如下:含有不饱和双键的液体树脂和含马来酰亚胺基的酚醛树脂双键官能当量比为1:0.5~10。
2.根据权利要求1所述的树脂组合物,其特征在于:所述Ar*为苯环。
4.根据权利要求1所述的树脂组合物,其特征在于:所述组分(b)的结构式中,x结构单元和y结构单元的摩尔比为1:1~1:5。
5.根据权利要求1所述的树脂组合物,其特征在于:所述环氧树脂选自DOPO-HQ改性环氧树脂、联苯型环氧树脂、双酚型酚醛环氧树脂、含双酚A环氧树脂、双酚F环氧树脂、二羟基二苯醚环氧树脂、烯丙基缩水甘油醚中的一种或几种。
6.根据权利要求1所述的树脂组合物,其特征在于:所述韧性树脂选自酚氧树脂、丁腈橡胶、核壳橡胶、聚丙烯酸酯树脂中的一种或几种。
7.根据权利要求1所述的树脂组合物,其特征在于:还包括共固化剂,所述共固化剂的添加量为:按照官能当量计算,在所述含马来酰亚胺基的酚醛树脂和共固化剂总官能当量和所述环氧树脂的官能当量比为0.5~5:1的前提下,含马来酰亚胺基的酚醛树脂占固化剂总官能当量的50~90%;优选的,所述共固化剂为胺类固化剂。
8.根据权利要求1所述的树脂组合物,其特征在于:还包括填料,以重量计,填料占树脂组合物的5~80%。
9.根据权利要求1所述的树脂组合物,其特征在于:所述含有不饱和双键的液体树脂选自丙烯酸树脂、烯丙基树脂、苯乙烯及取代苯乙烯树脂中的一种或几种;优选的,所述含有不饱和双键的液体树脂的添加量,按照含不饱和双键的液体树脂和其他总树脂重量比的1%-10%添加。
10.采用如权利要求1至9中任一所述的树脂组合物制备的低流胶半固化片。
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