CN111801395B - 粘合剂组合物及使用其的带粘合剂层的层压体 - Google Patents
粘合剂组合物及使用其的带粘合剂层的层压体 Download PDFInfo
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- CN111801395B CN111801395B CN201980017021.5A CN201980017021A CN111801395B CN 111801395 B CN111801395 B CN 111801395B CN 201980017021 A CN201980017021 A CN 201980017021A CN 111801395 B CN111801395 B CN 111801395B
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- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
- YNOWBNNLZSSIHM-UHFFFAOYSA-N tris(oxiran-2-ylmethyl) benzene-1,2,4-tricarboxylate Chemical compound C=1C=C(C(=O)OCC2OC2)C(C(=O)OCC2OC2)=CC=1C(=O)OCC1CO1 YNOWBNNLZSSIHM-UHFFFAOYSA-N 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
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Abstract
本发明提供:对由聚酰亚胺树脂等构成的基材膜和铜箔的粘合性良好、且介电特性进一步提高的粘合剂组合物。所述粘合剂组合物的特征在于,含有改性聚丙烯系树脂(A)、环氧树脂(B)和未改性的聚丙烯系树脂(C),上述改性聚丙烯系树脂(A)是将未改性的聚丙烯系树脂(D)用含有α,β‑不饱和羧酸或其衍生物的改性剂进行接枝改性而得到的树脂,按固体成分换算计,上述改性聚丙烯系树脂(A)的含量为10质量%以上,而且,按固体成分换算计,上述未改性的聚丙烯系树脂(C)的含量为1质量%以上且90质量%以下。
Description
技术领域
本发明涉及粘合剂组合物及使用其的带粘合剂层的层压体,更详细地说,涉及电子零部件的粘合用途,特别是适用于制造柔性印刷线路板(以下,也称为“FPC”)相关产品的粘合剂组合物、以及带粘合剂层的层压体。
背景技术
柔性印刷线路板即使在有限的空间里也能够立体且高密度地安装,因此其用途正在扩大。近年来,伴随着电子设备的小型化、轻量化等,柔性印刷线路板的相关产品变得多样化,其需求正在增加。作为这样的相关产品,可举出:在聚酰亚胺膜上贴合了铜箔的柔性覆铜层压板、在柔性覆铜层压板上形成了电子电路的柔性印刷线路板、将柔性印刷线路板和加强板贴合在一起的带加强板的柔性印刷线路板、将柔性覆铜层压板或柔性印刷线路板重叠接合在一起的多层板、在基材膜上贴合了铜布线的柔性扁平线缆(以下,也称为“FFC”)等,例如,在制造柔性覆铜层压板时,为了将聚酰亚胺膜和铜箔粘合在一起,通常使用粘合剂。
另外,在制造柔性印刷线路板时,为了保护配线部分,通常使用被称为“覆盖膜”的膜,该覆盖膜具备绝缘树脂层和在其表面上形成的粘合剂层;在绝缘树脂层的形成中,广泛使用聚酰亚胺树脂组合物。例如,通过利用热压等在具有配线部分的表面上通过粘合剂层贴附覆盖膜,由此制造成柔性印刷线路板,此时,覆盖膜的粘合剂层需要对配线部分和膜基层这两者都具有牢固的粘合性。
另外,作为印刷线路板,已知有在基板的表面上交替层压导体层和有机绝缘层的层叠型的多层印刷线路板。制造这样的多层印刷线路板时,为了接合导体层和有机绝缘层,使用被称为“粘合片”的绝缘粘合层形成材料。对于绝缘粘合层来说,它必须具有向配线部分的埋入性以及对形成电路的导体部的构成材料(铜等)和有机绝缘层(聚酰亚胺树脂等)这两者都具有牢固的粘合性。
作为用于这种FPC相关产品的粘合剂,提出了含有与环氧树脂具有高反应性的热塑性树脂的环氧系粘合剂组合物。例如,专利文献1中公开了乙烯-丙烯酸酯共聚橡胶/环氧树脂系粘合剂。另外,专利文献2中公开了含有缩水甘油基的热塑性弹性体/环氧树脂系粘合剂。进而,专利文献3中公开了苯乙烯-马来酸共聚物/环氧树脂系粘合剂。这些文献中记载的粘合剂组合物,通过利用橡胶或弹性体成分的羧基与环氧树脂的反应性,实现快速的固化反应,粘合性也优异,因此被广泛利用。
另外,在近年来需求迅速扩大的手机、或信息设备终端等移动通讯设备中,需要高速处理大量数据,因此正在推进信号的高频化。伴随信号速度的高速化和信号的高频化,对用于FPC相关产品的粘合剂来说,要求可耐受高频区域的使用的介电特性(低介电常数和低介电损耗角正切)。为了应对这样的介电特性的要求,例如,专利文献4中公开了一种环氧树脂组合物,其包含以环氧树脂、芳族乙烯基化合物和马来酸酐为必须成分而得到的共聚树脂、以及特定的苯酚化合物。另外,专利文献5中公开了一种含有改性聚烯烃系树脂和环氧树脂的粘合剂组合物,其中,改性聚烯烃系树脂和环氧树脂为特定的含量。
现有技术文献
专利文献
专利文献1:特开平7-235767号公报
专利文献2:特开2001-354936号公报
专利文献3:特开2007-2121号公报
专利文献4:特开平10-17685号公报
专利文献5:国际公开第2016/047289号
发明内容
发明要解决的课题
然而,如上所述,伴随着信号的高频化,专利文献1~4中记载的粘合剂组合物存在在超短波的微波频带(1~3GHz)的介电特性不充分的问题。另外,使用这些粘合剂组合物的带粘合剂层的层压体存在以下问题:在热固化前(B-阶(B-stage)状态)有层压体翘曲的情况,在FPC制造过程中作业性差。为了提高上述介电特性,必须使基材膜变得更薄,还期望在基材膜变薄的情况下,带粘合剂层的层压体的翘曲减少。进而,使用这些粘合剂组合物的带粘合剂层的层压体还存在以下问题:在储存期间有时发生翘曲,层压体的储存稳定性差。
专利文献5中记载的粘合剂组合物虽然粘合性、介电特性、以及用于层压体的粘合剂层时的在层压体中的储存稳定性优异,但为了应对近年来信号速度的更高速化和信号的更高频化,需要进一步提高介电特性。
本发明正是鉴于上述课题而完成的,其目的在于提供对由聚酰亚胺树脂等制成的基材膜、以及铜箔的粘合性良好、介电特性进一步提高的粘合剂组合物。另外,本发明的目的在于,提供介电特性进一步提高、翘曲被抑制、储存稳定性良好的带粘合剂层的层压体。
解决课题的手段
本发明人等发现:对于含有改性聚丙烯系树脂、环氧树脂和未改性的聚丙烯系树脂的粘合剂组合物来说,当上述改性聚丙烯系树脂和未改性的聚丙烯系树脂的含量在特定范围内时,粘合性良好,介电特性进一步提高。另外发现:对于使用该粘合剂组合物得到的带粘合剂层的层压体来说,当粘合剂层为B阶状态时,不仅粘合性优异,而且几乎没有层压体的翘曲,储存稳定性也优异,至此完成了本发明。
根据本发明的一个方面,提供一种粘合剂组合物,其特征在于,含有改性聚丙烯系树脂(A)、环氧树脂(B)和未改性的聚丙烯系树脂(C),上述改性聚丙烯系树脂(A)是将未改性的聚丙烯系树脂(D)用含有α,β-不饱和羧酸或其衍生物的改性剂进行接枝改性而得到的树脂,上述改性聚丙烯系树脂(A)的含量相对于上述粘合剂组合物的固体成分100质量份,为10质量份以上,而且,上述未改性的聚丙烯系树脂(C)的含量相对于上述粘合剂组合物的固体成分100质量份,为1质量份以上且90质量份以下。
根据本发明的优选实施方式,上述α,β-不饱和羧酸的衍生物是选自衣康酸酐、马来酸酐、乌头酸酐和柠康酸酐中的至少1种。
根据本发明的另一优选实施方式,源自上述α,β-不饱和羧酸或其衍生物的接枝部分的含量比例相对于上述改性聚丙烯系树脂(A)100质量%,为0.1~20质量%。
根据本发明的另一优选实施方式,上述环氧树脂(B)是具有脂环骨架的多官能环氧树脂。
根据本发明的另一优选实施方式,上述改性聚丙烯系树脂(A)中的丙烯的共聚比为70质量%以下。
根据本发明的另一优选实施方式,上述未改性的聚丙烯系树脂(C)中的丙烯的共聚比为70质量%以下。
根据本发明的另一优选实施方式,上述未改性的聚丙烯系树脂(C)和上述未改性的聚丙烯系树脂(D)是选自乙烯-丙烯共聚物、丙烯-丁烯共聚物和乙烯-丙烯-丁烯共聚物中的至少1种。
根据本发明的另一优选实施方式,上述粘合剂组合物含有抗氧化剂。
根据本发明的另一优选实施方式,上述粘合剂组合物还含有有机溶剂,并且上述改性聚丙烯系树脂(A)、上述环氧树脂(B)和上述未改性的聚丙烯系树脂(C)溶解在上述有机溶剂中。
根据本发明的另一优选实施方式,上述有机溶剂含有脂环式烃溶剂和醇系溶剂,上述脂环式烃溶剂为甲基环已烷和/或环已烷,相对于上述有机溶剂100质量份,上述脂环式烃溶剂的含量为20质量份以上且90质量份以下;相对于上述有机溶剂100质量份,上述醇系溶剂的含量为1质量份以上且20质量份以下。
根据本发明的另一优选实施方式,上述粘合剂组合物含有甲苯作为上述有机溶剂。
根据本发明的另一优选实施方式,含有上述有机溶剂的粘合剂组合物的固体成分的浓度为5质量%以上且50质量%以下。
根据本发明的另一方面,提供一种带粘合剂层的层压体,其特征在于,具备:含有上述本发明粘合剂组合物的粘合剂层、以及,与该粘合剂层的至少一侧表面相接的基材膜;上述粘合剂层为B阶状态。
根据本发明的另一优选实施方式,上述基材膜是选自聚酰亚胺膜、聚醚醚酮膜、聚苯硫醚膜、芳族聚酰胺膜、聚萘二甲酸乙二醇酯膜、液晶聚合物膜、聚对苯二甲酸乙二醇酯膜、聚乙烯膜、聚丙烯膜、有机硅离型处理纸、聚烯烃树脂涂布纸、聚甲基戊烯膜(TPX膜)、氟系树脂膜、和铜箔中的至少1种。
根据本发明的另一方面,提供一种印刷线路板,其包括:含有上述本发明粘合剂组合物的粘合剂层。
根据本发明的另一方面,提供一种柔性扁平电缆,其包括:含有上述本发明粘合剂组合物的粘合剂层。
本说明书中,“丙烯系树脂”是指具有来自丙烯的单体单元的树脂。另外,“未改性”是指没有通过α,β-不饱和羧酸或其衍生物进行改性。
另外,本说明书中,重均分子量(以下,也称为“Mw”)是通过凝胶渗透色谱法(以下,也称为“GPC”)测定的按标准聚苯乙烯换算的值。
另外,本说明书中,“(甲基)丙烯酸系”的表述是指丙烯酸系和甲基丙烯酸系。
发明效果
本发明的粘合剂组合物对由聚酰亚胺树脂等构成的基材膜和铜箔的粘合性良好,介电特性(低介电常数和低介电损耗角正切)也优异。另外,使用本发明粘合剂组合物的带粘合剂层的层压体几乎没有翘曲,因此在各种零部件的制造过程中作业性优异,层压体的储存稳定性也良好。因此,本发明的粘合剂组合物以及使用其的带粘合剂层的层压体适用于FPC相关产品的制造等。
如下所述说明本发明的一实施方式,但本发明并不限定于此。
1.粘合剂组合物
本发明的粘合剂组合物的特征在于,含有改性聚丙烯系树脂(A)、环氧树脂(B)和未改性的聚丙烯系树脂(C),上述改性聚丙烯系树脂(A)是将未改性的聚丙烯系树脂(D)用含有α,β-不饱和羧酸或其衍生物的改性剂进行接枝改性而得到的树脂,上述改性聚丙烯系树脂(A)的含量相对于上述粘合剂组合物的固体成分100质量份,为10质量份以上,而且,上述未改性的聚丙烯系树脂(C)的含量相对于上述粘合剂组合物的固体成分100质量份,为1质量份以上且90质量份以下。以下,具体说明特定本发明的事项。
1.1.改性聚丙烯系树脂(A)
上述改性聚丙烯系树脂(A)是具有来自未改性的聚丙烯系树脂(D)的部分和来自改性剂的接枝部分的树脂,优选通过在未改性的聚丙烯系树脂(D)的存在下接枝聚合含有α,β-不饱和羧酸或其衍生物的改性剂而得到。通过接枝聚合的改性聚丙烯系树脂(A)的制造可通过公知的方法进行,在制造时,也可以使用自由基引发剂。作为上述改性聚丙烯系树脂(A)的制造方法,例如可举出:将未改性的聚丙烯系树脂(D)在甲苯等溶剂中加热溶解,添加上述改性剂和自由基引发剂的溶液法;或者,使用班伯里密炼机、捏合机、挤出机等将未改性的聚丙烯系树脂(D)、改性剂和自由基引发剂进行熔融捏合的熔融法等。未改性的聚丙烯系树脂(D)、改性剂和自由基引发剂的使用方法没有特别限制,可以将它们一次全部添加到反应体系中,也可以逐次添加。
制造上述改性聚丙烯系树脂(A)时,还可以使用用于提高α,β-不饱和羧酸的接枝效率的改性助剂、用于调节树脂稳定性的稳定剂等。
用于制造改性聚丙烯系树脂(A)的未改性的聚丙烯系树脂(D)只要是具有来自丙烯的结构单元、且没有通过α,β-不饱和羧酸或其衍生物改性的树脂,就没有特别限制,优选使用丙烯与乙烯、丁烯、戊烯、己烯、庚烯、辛烯、4-甲基-1-戊烯等碳数2以上且20以下的烯烃的共聚物。本发明中,特别优选丙烯与碳数2以上且6以下的烯烃的共聚物。
为了使溶液稳定,有时将用于电子零部件等的粘接用途的粘合剂组合物在约5℃的低温下保存数天至数月的时间,但在存放期间粘合剂组合物可能变成凝胶状,流动性消失。因此,对于用于该用途的粘合剂组合物来说,也要求低温下的储存稳定性。从获得低温下的储存稳定性的观点考虑,改性聚丙烯系树脂(A)中的丙烯的共聚比优选为70质量%以下,更优选为68质量%以下。另外,从获得优异的粘合性的同时向两个部件粘合后的粘合部赋予柔软性的观点考虑,改性聚丙烯系树脂(A)中的丙烯的共聚比的下限值优选为50质量%以上。关于未改性的聚丙烯系树脂(D)中的丙烯以外的结构单元及其含量比例,只要是使改性聚丙烯系树脂(A)中的丙烯的共聚比为上述上限值以下,就可以任意选择。在与难粘合性的被粘接体进行粘接时,上述改性聚丙烯系树脂(A)优选为选自乙烯-丙烯、丙烯-丁烯和乙烯-丙烯-丁烯共聚物中的至少1种未改性聚丙烯系树脂(D)的改性树脂。另外,未改性的聚丙烯系树脂(D)的分子量没有特别限制。
改性剂含有α,β-不饱和羧酸或其衍生物。作为α,β-不饱和羧酸,可举出:马来酸、富马酸、四氢邻苯二甲酸、衣康酸、柠康酸、巴豆酸、乌头酸、降冰片烯二羧酸、(甲基)丙烯酸等。另外,作为上述α,β-不饱和羧酸的衍生物,可举出:酸酐、酰卤、酰胺、酰亚胺、酯等。作为上述改性剂,优选为聚羧酸,更优选为衣康酸酐、马来酸酐、乌头酸酐和柠康酸酐,从粘合性的观点考虑,特别优选为衣康酸酐和马来酸酐。改性剂可以包括选自α,β-不饱和羧酸或其衍生物中的1种以上,例如,可以为1种以上α,β-不饱和羧酸和1种以上其衍生物的组合、2种以上α,β-不饱和羧酸的组合、或者2种以上α,β-不饱和羧酸的衍生物的组合。
根据目的,本发明的改性剂除了α,β-不饱和羧酸等或其衍生物以外,还可以含有其他化合物(其他改性剂)。作为其他化合物(其他改性剂),例如可举出:下述式(1)表示的(甲基)丙烯酸酯、其他的(甲基)丙烯酸衍生物、芳族乙烯基化合物、环己基乙烯基醚等。这些其他化合物可以单独使用1种或组合使用2种以上。
CH2=CR1COOR2…………(1)
(式中,R1是氢原子或甲基,R2是烃基。)
在上述表示(甲基)丙烯酸酯的式(1)中,R1是氢原子或甲基,优选为甲基。R2是烃基,优选为碳数8~18的烷基。作为上述式(1)表示的化合物,可举出:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸戊酯、(甲基)丙烯酸己酯、(甲基)丙烯酸庚酯、(甲基)丙烯酸辛酯、(甲基)丙烯酸癸酯、(甲基)丙烯酸月桂基酯、(甲基)丙烯酸十三烷基酯、(甲基)丙烯酸硬脂基酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸苄酯等。这些化合物可以单独使用1种或组合使用2种以上。本发明中,从改善耐热粘合性的观点考虑,优选使用还含有具有碳数8~18的烷基的(甲基)丙烯酸酯的改性剂,特别优选含有(甲基)丙烯酸辛酯、(甲基)丙烯酸月桂基酯、(甲基)丙烯酸十三烷基酯或(甲基)丙烯酸硬脂基酯。
作为(甲基)丙烯酸酯以外的(甲基)丙烯酸衍生物,可举出:(甲基)丙烯酸羟乙酯、(甲基)丙烯酸缩水甘油基酯、含有异氰酸酯的(甲基)丙烯酸等。作为芳族乙烯基化合物,可举出:苯乙烯、邻甲基苯乙烯、对甲基苯乙烯、α-甲基苯乙烯等。作为上述改性剂,通过并用α,β-不饱和羧酸或其衍生物与其他改性剂,可以提高改性剂的接枝率,提高对溶剂的溶解度,还可以进一步提高粘合性。予以说明,使用上述式(1)表示的(甲基)丙烯酸酯以外的其他改性剂时,其使用量期望不超过α,β-不饱和羧酸及其衍生物与(甲基)丙烯酸酯的使用量的合计。
如上所述,改性聚丙烯系树脂(A)至少具有来自改性剂的接枝部分。以下,说明改性聚丙烯系树脂(A)中含有的接枝部分的含有比例(以下,也称为“接枝质量”)。
上述改性聚丙烯系树脂(A)具有来自α,β-不饱和羧酸或其衍生物的接枝部分。在上述改性聚丙烯系树脂(A)中,从粘合性的观点考虑,来自α,β-不饱和羧酸或其衍生物的接枝部分的接枝质量相对于改性聚丙烯系树脂(A)100质量%时,优选为0.1~20质量%,更优选为0.2~18质量%。当接枝质量为0.1质量%以上时,对溶剂的溶解度优异,对由金属等制成的被粘接体的粘合性特别优异。
另外,当接枝质量为20质量%以下时,可以得到对由树脂等制成的被粘接体的充分的粘合性。
上述改性聚丙烯系树脂(A)中的来自α,β-不饱和羧酸或其衍生物的接枝质量可以通过碱滴定法求出,但是在α,β-不饱和羧酸的衍生物为不具有酸基的酰亚胺等的情况下,接枝质量可以通过傅立叶变换红外光谱法求出。
当上述改性聚丙烯系树脂(A)含有来自上述式(1)表示的(甲基)丙烯酸酯的接枝部分时,其接枝质量相对于改性聚丙烯系树脂(A)100质量%,优选为0.1~30质量%,更优选为0.3~25质量%。当接枝质量为0.1~30质量%时,对溶剂的溶解度优异,在含有后述的其他的树脂或弹性体时与它们的相容性优异,可进一步提高对被粘接体的粘合性。
当上述改性剂含有上述式(1)表示的(甲基)丙烯酸酯时,得到的改性聚丙烯系树脂(A)中的接枝质量可以通过傅立叶变换红外光谱法求出。
用于制造上述改性聚丙烯系树脂(A)的自由基引发剂可以从公知的引发剂中适当选择,例如,优选使用过氧化苯甲酰、过氧化二枯基、过氧化月桂酰、过氧化二叔丁基、2,5-二甲基-2,5-二(叔丁基过氧基)己烷、氢过氧化枯烯等有机过氧化物。
作为可用于制造上述改性聚丙烯系树脂(A)的改性助剂,可举出:二乙烯基苯、己二烯、二环戊二烯等。作为稳定剂,可举出:氢醌、苯醌、亚硝基苯基羟基化合物等。
上述改性聚丙烯系树脂(A)的重均分子量(Mw)优选为30,000~250,000,更优选为50,000~200,000。通过使重均分子量(Mw)为30,000~250,000,对溶剂的溶解度以及对被粘接体的初始粘合性均优异,进而可以制成粘合后的粘合部的耐溶剂性也优异的粘合剂组合物。
改性聚丙烯系树脂(A)的酸值优选为0.1~50mg KOH/g,更优选为0.5~40mg KOH/g,进一步优选为1.0~30mg KOH/g。通过使该酸值为0.1~50mg KOH/g,粘合剂组合物充分固化,得到了良好的粘合性、耐热性和树脂流出性。
改性聚丙烯系树脂(A)的含量相对于粘合剂组合物的固体成分100质量份,必须为10质量份以上,优选为30质量份以上,更优选为40质量份以上。通过使改性聚丙烯系树脂(A)的含量在上述下限值以上,可以提高回流焊(solder reflow)时的耐热性。
另外,改性聚丙烯系树脂(A)的含量相对于粘合剂组合物的固体成分100质量份,优选99质量份以下。
1.2.环氧树脂(B)
接着,说明上述粘合剂组合物的一个成分“环氧树脂(B)”。环氧树脂(B)为与上述改性聚丙烯系树脂中的羧基反应,发挥对被粘接体的高粘合性和粘合剂固化物的耐热性的成分。
作为环氧树脂(B)的实例,可举出双酚A型环氧树脂、双酚F型环氧树脂、或它们的氢化物;邻苯二甲酸二缩水甘油基酯、间苯二甲酸二缩水甘油基酯、对苯二甲酸二缩水甘油基酯、对羟基苯甲酸缩水甘油基酯、四氢邻苯二甲酸二缩水甘油基酯、琥珀酸二缩水甘油基酯、己二酸二缩水甘油基酯、癸二酸二缩水甘油基酯、偏苯三酸三缩水甘油基酯等缩水甘油基酯系环氧树脂;乙二醇二缩水甘油基醚、丙二醇二缩水甘油基醚、1,4-丁二醇二缩水甘油基醚、1,6-己二醇二缩水甘油基醚、三羟甲基丙烷三缩水甘油基醚、季戊四醇四缩水甘油基醚、四苯基缩水甘油基醚乙烷、三苯基缩水甘油基醚乙烷、山梨糖醇的聚缩水甘油基醚、聚甘油的聚缩水甘油基醚等缩水甘油基醚系环氧树脂;异氰尿酸三缩水甘油基酯,四缩水甘油基二氨基二苯基甲烷等缩水甘油胺系环氧树脂;环氧化聚丁二烯、环氧化大豆油等直链脂族环氧树脂等,但并不限定于此。另外,也可以使用苯酚酚醛清漆型环氧树脂、邻甲酚酚醛清漆型环氧树脂、双酚A酚醛清漆型环氧树脂等酚醛型环氧树脂。
进而,作为环氧树脂(B)的实例,可举出:溴化双酚A型环氧树脂、含磷环氧树脂、含二环戊二烯骨架的环氧树脂、含有萘骨架的环氧树脂、蒽型环氧树脂、叔丁基儿茶酚型环氧树脂、三苯甲烷型环氧树脂、四苯基乙烷型环氧树脂、联苯型环氧树脂、双酚S型环氧树脂等。这些环氧树脂可以仅使用1种,也可以并用2种以上。
上述环氧树脂中,优选没有缩水甘油氨基的环氧树脂。因为提高了带粘合剂层的层压体的储存稳定性。另外,为了得到介电特性优异的粘合剂组合物,优选具有脂环骨架的环氧树脂,更优选具有二环戊二烯骨架的环氧树脂。
作为本发明中使用的环氧树脂(B),优选为1分子中具有2个以上环氧基的环氧树脂,因为可以通过与改性聚丙烯系树脂(A)的反应形成交联结构,从而发挥高的耐热性。另外,使用环氧基为2个以上的环氧树脂时,与改性聚丙烯系树脂(A)的交联度充分,可以得到充分的耐热性。
上述环氧树脂(B)的含量相对于上述改性聚丙烯系树脂(A)100质量份,优选为1~20质量份。上述含量更优选为3~15质量份。当该含量为1质量份以上时,可得到充分的粘合性和耐热性。另一方面,当该含量为20质量份以下时,剥离粘合强度和介电特性优异。
1.3.未改性的聚丙烯系树脂(C)
未改性的聚丙烯系树脂(C)只要具有来自丙烯的结构单元、并且不会被α,β-不饱和羧酸或其衍生物改性,就没有特别限制,优选使用丙烯与乙烯、丁烯、戊烯、己烯、庚烯、辛烯、4-甲基-1-戊烯等碳数2以上20以下的烯烃的共聚物。本发明中,特别优选丙烯与碳数2以上6以下的烯烃的共聚物。从得到低温下的储存稳定性的观点考虑,未改性的聚丙烯系树脂(C)中的丙烯的共聚比优选为70质量%以下,更优选为68质量%以下。另外,从获得优异的粘合性且向粘接2个部件后的粘合部赋予柔软性的观点考虑,未改性的聚丙烯系树脂(C)中的丙烯的共聚比的下限值优选为50质量%以上。对于未改性的聚丙烯系树脂(C)中的丙烯以外的结构单元及其含量比例来说,只要使未改性的聚丙烯系树脂(C)中的丙烯的共聚比为上述下限值以下,就可以任意选择,在进行难粘接性被粘接体的粘接时,上述未改性的聚丙烯系树脂(C)优选为乙烯-丙烯、丙烯-丁烯或乙烯-丙烯-丁烯共聚物。另外,未改性的聚丙烯系树脂(C)的分子量没有特别限制。
上述未改性的聚丙烯系树脂(C)的重均分子量(Mw)优选为30,000~250,000,更优选为50,000~200,000。通过使重均分子量(Mw)为30,000~250,000,对溶剂的溶解度以及对被粘接体的初始粘合性都优异,进而可以得到粘合后的粘合部的耐溶剂性也优异的粘合剂组合物。
未改性的聚丙烯系树脂(C)的含量相对于粘合剂组合物的固体成分100质量份,必须为1质量份以上且90质量份以下,优选为20质量份以上且70质量份以下,更优选为30质量份以上且60质量份以下。通过使未改性的聚丙烯系树脂(C)的含量在上述范围内,可以提高回流焊时的耐热性,而且提高介电特性。
在本发明的粘合剂组合物中,改性聚丙烯系树脂(A)和未改性的聚丙烯系树脂(C)的含量的合计相对于粘合剂组合物的固体成分100质量份,优选为50质量份以上,更优选为60质量份以上。通过使该含量的合计为50质量份以上,可以赋予粘合剂层柔软性,并且防止层压体翘曲。
另外,该含量的合计相对于粘合剂组合物的固体成分100质量份,优选为99质量份以下。
本发明的粘合剂组合物的特征在于,以规定量含有改性聚丙烯系树脂(A)、环氧树脂(B)和未改性的聚丙烯系树脂(C),在1GHz的频率下测定的粘合剂固化物的介电常数(ε)小于2.2。当该介电常数小于2.2时,适合用于应对近年来信号速度的进一步高速化、信号的进一步高频化的FPC相关产品。另外,在1GHz的频率下测定的粘合剂固化物的介电损耗角正切(tanδ)优选小于0.001。当该介电损耗角正切小于0.001时,可以制造介电特性优异的FPC相关产品。介电常数和介电损耗角正切可以根据粘合剂组合物中的改性聚丙烯系树脂(A)、环氧树脂(B)和未改性的聚丙烯系树脂(C)的比例来调节,可根据用途来设定各种构成的粘合剂组合物。予以说明,介电常数和介电损耗角正切的测定方法将在后面说明。
1.4.其他成分
上述粘合剂组合物除了改性聚丙烯系树脂(A)、环氧树脂(B)和未改性的聚丙烯系树脂(C)以外,还可以以不影响粘合剂组合物功能的程度含有改性聚丙烯系树脂(A)和未改性的聚丙烯系树脂(C)以外的其他的热塑性树脂、增粘剂、阻燃剂、固化剂、固化促进剂、偶联剂、抗热老化剂、流平剂、消泡剂、无机填料、颜料、和溶剂等。
(热塑性树脂)
作为上述其他热塑性树脂,例如可举出:苯氧树脂、聚酰胺树脂、聚酯树脂、聚碳酸酯树脂、聚苯醚树脂、聚氨酯树脂、聚缩醛树脂、聚乙烯系树脂、聚丙烯系树脂和聚乙烯基系树脂等。这些热塑性树脂可以单独使用1种,也可以并用2种以上。
(增粘剂)
作为上述增粘剂,例如可举出:苯并呋喃-茚树脂、萜烯树脂、萜烯-酚醛树脂、松香树脂、对叔丁基苯酚-乙炔树脂、苯酚-甲醛树脂、二甲苯-甲醛树脂、石油系烃树脂、氢化烃树脂、松节油系树脂等。这些增粘剂可以单独使用1种,也可以并用2种以上。
(阻燃剂)
上述阻燃剂可以是有机系阻燃剂和无机系阻燃剂的任一种。作为有机系阻燃剂,例如可举出:磷酸三聚氰胺、聚磷酸三聚氰胺、磷酸胍、聚磷酸胍、磷酸铵、聚磷酸铵、磷酸酰胺铵、聚磷酸酰胺铵、磷酸氨基甲酸酯、聚磷酸氨基甲酸酯、三-二乙基次膦酸铝、三甲基乙基次膦酸铝、三-二苯基次膦酸铝、双二乙基次膦酸锌、双甲基乙基次膦酸锌、双二苯基次膦酸锌、双二乙基次膦酸氧钛、四(二乙基次膦酸)钛、双甲基乙基次膦酸氧钛、四甲基乙基次膦酸钛、双二苯基次膦酸氧钛、四(二苯基次膦酸)钛等磷系阻燃剂;三聚氰胺、蜜白胺、三聚氰胺氰尿酸酯等三嗪系化合物,或者氰尿酸化合物、异氰尿酸化合物、三唑系化合物、四唑系化合物、重氮化合物、尿素等氮系阻燃剂;有机硅化合物、硅烷化合物等硅系阻燃剂等。另外,作为无机系阻燃剂,可举出:氢氧化铝、氢氧化镁、氢氧化锆、氢氧化钡、氢氧化钙等金属氢氧化物;氧化锡、氧化铝、氧化镁、氧化锆、氧化锌、氧化钼、氧化镍等金属氧化物;碳酸锌、碳酸镁、碳酸钡、硼酸锌、水合玻璃等。这些阻燃剂可以并用2种以上。
(固化剂)
作为上述固化剂,可举出氨系固化剂、酸酐系固化剂等,但并不限定于此。作为氨系固化剂,例如可举出:甲基化三聚氰胺树脂、丁基化三聚氰胺树脂、苯并胍胺树脂等三聚氰胺树脂;双氰胺、4,4’-二苯基二氨基砜等。另外,作为酸酐,可举出:芳族系酸酐、和脂族系酸酐等。这些固化剂可以单独使用,也可以并用2种以上。
固化剂的含量相对于环氧树脂(B)100质量份,优选为1~100质量份,更优选为5~70质量份。
(固化促进剂)
上述固化促进剂是以促进改性聚丙烯系树脂(A)和环氧树脂的反应为目的而使用的,可以使用叔胺系固化促进剂、叔胺盐系固化促进剂和咪唑系固化促进剂等。
作为叔胺系固化促进剂,可举出:苄基二甲胺、2-(二甲氨基甲基)苯酚、2,4,6-三(二甲氨基甲基)苯酚、四甲基胍、三乙醇胺、N,N’-二甲基哌嗪、三亚乙基二胺、1,8-二氮杂双环[5.4.0]十一碳烯等。
作为叔胺盐系固化促进剂,可举出:1,8-二氮杂双环[5.4.0]十一碳烯酸的甲酸盐、辛酸盐、对甲苯磺酸盐、邻苯二甲酸盐、苯酚盐或苯酚酚醛清漆树脂盐,或者1,5-二氮杂双环[4.3.0]壬烯的甲酸盐、辛酸盐、对甲苯磺酸盐、邻苯二甲酸盐、苯酚盐或苯酚酚醛清漆树脂盐等。
作为咪唑系固化促进剂,可举出:2-甲基咪唑、2-十一烷基咪唑、2-十七烷基咪唑、1,2-二甲基咪唑、2-甲基-4-乙基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑、1-苄基-2-甲基咪唑、1-苄基-2-苯基咪唑、2,4-二氨基-6-[2’-甲基咪唑基-(1’)]乙基-均三嗪、2,4-二氨基-6-[2’-十一烷基咪唑基-(1’)]乙基-均三嗪、2,4-二氨基-6-[2’-乙基-4’-甲基咪唑基-(1’)]乙基-均三嗪、2,4-二氨基-6-[2’-甲基咪唑基-(1’)]乙基-均三嗪异氰尿酸加成物、2-苯基咪唑异氰尿酸加成物、2-苯基-4,5-二羟基甲基咪唑、2-苯基-4-甲基-5-羟基甲基咪唑等。这些固化促进剂可以单独使用,也可以并用2种以上。
当粘合剂组合物含有固化促进剂时,固化促进剂的含量相对于环氧树脂(B)100质量份,优选为1~15质量份,更优选为1~10质量份,进一步优选为2~5质量份。只要固化促进剂的含量在上述范围内,就具有优异的粘合性和耐热性。
(偶联剂)
另外,作为上述偶联剂,可举出:乙烯基三甲氧基硅烷、3-环氧丙氧基丙基三甲氧基硅烷、对苯乙烯基三甲氧基硅烷、3-甲基丙烯酰氧基丙基甲基二甲氧基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷、N-2-(氨基乙基)-3-氨基丙基甲基二甲氧基硅烷、3-脲基丙基三乙氧基硅烷、3-巯基丙基甲基二甲氧基硅烷、双(三乙氧基甲硅烷基丙基)四硫化物、3-异氰酸酯基丙基三乙氧基硅烷、咪唑硅烷等硅烷系偶联剂;钛酸酯系偶联剂;铝酸酯系偶联剂;锆系偶联剂等。这些偶联剂可以单独使用,也可以并用2种以上。
(抗热老化剂)
作为上述抗热老化剂,例如可举出抗氧化剂,作为其具体例,可举出:2,6-二叔丁基-4-甲基苯酚、正十八烷基-3-(3’,5’-二叔丁基-4’-羟基苯基)丙酸酯、四[亚甲基-3-(3,5-二叔丁基-4-羟基苯基)丙酸酯]甲烷、季戊四醇四[3-(3,5-二叔丁基-4-羟基苯基)丙酸酯]、三甘醇-双[3-(3-叔丁基-5-甲基-4-羟基苯基)丙酸酯]等苯酚系抗氧化剂,3,3’-硫代二丙酸二月桂基酯、3,3’-二硫代丙酸二肉豆蔻基酯等硫系抗氧化剂;亚磷酸三壬基苯基酯、三(2,4-二叔丁基苯基)亚磷酸酯等磷系抗氧化剂。这些抗热老化剂可以单独使用,也可以并用2种以上。
通过使本发明的粘合剂组合物含有抗热老化剂,即使在高温条件下以短时间进行下述的后固化,也容易发挥优异的介电特性。
当粘合剂组合物含有抗热老化剂时,抗热老化剂的含量相对于粘合剂组合物的固体成分100质量份,优选为0.5~5质量份,更优选为1~3质量份。只要抗热老化剂的含量在上述范围内,就可以抑制180℃加热固化时的介电特性的变差。
(无机填料)
作为上述无机填料,可举出:氧化钛、氧化铝、氧化锌、炭黑、二氧化硅、滑石粉、铜、和银等制成的粉体。这些无机填料可以单独使用,也可以并用2种以上。
上述粘合剂组合物可以通过混合改性聚丙烯系树脂(A)、环氧树脂(B)、未改性的聚丙烯系树脂(C)和其他成分来制造。混合方法没有特别限制,只要能使粘合剂组合物变得均匀即可。由于粘合剂组合物优选以溶液或分散液的状态使用,因此通常也使用有机溶剂等溶剂。
1.5.有机溶剂
作为本发明使用的有机溶剂,例如可举出:甲醇、乙醇、异丙醇、正丙醇、异丁醇、正丁醇、苄醇、乙二醇单甲基醚、丙二醇单甲基醚、二甘醇单甲基醚、双丙酮醇等醇系溶剂;丙酮、甲乙酮、甲基异丁基酮、甲基戊基酮、环己酮、异佛尔酮等酮系溶剂;甲苯、二甲苯、乙基苯、均三甲苯等芳族烃系溶剂;乙酸甲酯、乙酸乙酯、乙二醇单甲基醚乙酸酯、乙酸3-甲氧基丁酯等酯系溶剂;环己烷、甲基环己烷等脂环式烃系溶剂等。这些溶剂可以单独使用,也可以并用2种以上。当粘合剂组合物含有有机溶剂、上述改性聚丙烯系树脂(A)、上述环氧树脂(B)和上述未改性的聚丙烯系树脂(C)为溶解或分散于有机溶剂中的溶液或分散液(树脂清漆)时,可以顺利地进行基材膜的涂布和粘合剂层的形成,可以容易地得到期望厚度的粘合剂层。
在上述例示的溶剂中,本发明使用的有机溶剂优选含有脂环式烃系溶剂和醇系溶剂,上述脂环式烃系溶剂为甲基环己烷和/或环己烷。在这样的方式中,上述脂环式烃的含量相对于有机溶剂100质量份,优选为20质量份以上且90质量份以下,更优选为40质量份以上且80质量份以下。
另外,上述醇系溶剂的含量相对于有机溶剂100质量份,优选为1质量份以上且20质量份以下,更优选为3质量份以上且10质量份以下。
通过使脂环式烃和/或醇系溶剂的含量在上述范围内,可以获得低温下的储存稳定性优异的粘合剂组合物。
另外,在上述例示的溶剂中,本发明使用的有机溶剂优选含有甲苯。在这样的方式中,甲苯的含量相对于粘合剂组合物100质量份,优选为10质量份以上且60质量份以下,更优选为20质量份以上且40质量份以下。通过使甲苯的含量在上述范围内,可以提高环氧树脂(B)等在有机溶剂中的溶解度。
当粘合剂组合物含有有机溶剂时,从包括形成粘合剂层的作业性等的观点考虑,固体成分浓度优选为5质量%以上且50质量%以下,更优选为10质量%以上且40质量%以下的范围。当固体成分浓度在80质量%以下时,溶液的粘度适度,容易均匀地涂布。
2.带粘合剂层的层压体
本发明的带粘合剂层的层压体的特征在于,具备:包含上述粘合剂组合物的粘合剂层、和与该粘合剂层的至少一侧表面接触的基材膜。上述粘合剂层是B-阶(B-stage)状态。此处,粘合剂层为B-阶状态是指:粘合剂组合物的一部分开始固化的半固化状态,并且通过加热等粘合剂组合物的固化进一步进行的状态。
作为本发明的带粘合剂层的层压体的一个方式,可举出覆盖膜。覆盖膜是在基材膜的至少一侧表面上形成有粘合剂层,且基材膜和粘合剂层的剥离困难的层压体。
作为带粘合剂层的层压体为覆盖膜时的基材膜,可举出:聚酰亚胺膜、聚醚醚酮膜、聚苯硫醚膜、芳族聚酰胺膜、聚萘二甲酸乙二醇酯膜、和液晶聚合物膜等。在这些膜中,从粘合性和介电特性的观点考虑,优选聚酰亚胺膜、聚萘二甲酸乙二醇酯膜、和液晶聚合物膜。
这样的基材膜已有市售品,关于聚酰亚胺膜,可以使用东丽-杜邦(株)制的“Kapton(注册商标)”、东洋纺织(株)制的“ゼノマックス(注册商标)”、宇部兴产(株)制的“Upilex(注册商标)-S”、(株)钟化制的“アピカル(注册商标)”等。另外,关于聚萘二甲酸乙二醇酯膜,可以使用帝人-杜邦膜(株)制的“Teonex(注册商标)”等。另外,关于液晶聚合物膜,可以使用(株)可乐丽制的“ベクスター(注册商标)”、(株)Prima Tech制的“バイアック(注册商标)”等。基材膜可以通过将这些树脂进行膜化成期望厚度来使用。
作为制造覆盖膜的方法,例如可举出如下方法:将含有上述粘合剂组合物和溶剂的树脂清漆涂布在聚酰亚胺膜等基材膜的表面,形成树脂清漆层,然后从该树脂清漆层中除去上述溶剂,由此制造形成有B阶状态的粘合剂层的覆盖膜。
除去上述溶剂时的干燥温度优选为40~250℃,更优选为70~170℃。通过使涂布有粘合剂组合物的层压体通过炉子中来进行干燥,在炉子中进行热风加热、远红外线加热、和高频感应加热等。
予以说明,根据需要,为了保管等,可以在粘合剂层的表面层压离型膜。作为上述离型膜,可以使用聚对苯二甲酸乙二醇酯膜、聚乙烯膜、聚丙烯膜、有机硅离型处理纸、聚烯烃树脂涂布纸、聚甲基戊烯(TPX)膜、氟系树脂膜等公知的膜。
作为带粘合剂层的层压体的其他方式,可举出粘合片。粘合片也是在基材膜的表面形成有上述粘合剂层的层压体,基材膜使用离型膜。另外,粘合片也可以是在2片离型膜之间具备粘合剂层的方式,使用粘合片时,剥离离型膜后使用。离型膜可以使用与上述同样的离型膜。
这样的离型膜已有市售品,可以使用东丽膜加工(株)制的“Lumirror(注册商标)”、东洋纺织(株)制的“东洋纺酯(注册商标)膜”、旭硝子(株)制的“アフレックス(注册商标)”、三井化学东セロ(株)制的“オピュラン(注册商标)”等。
作为制造粘合片的方法,例如有如下方法:在离型膜的表面上涂布含有上述粘合剂组合物和溶剂的树脂清漆,与上述覆盖膜的情况同样地进行干燥。
为了使带粘合剂层的层压体薄膜化,基材膜的厚度优选为5~100μm,更优选为5~50μm,进一步优选为5~30μm。
B阶状态的粘合剂层的厚度优选为5~100μm,更优选为10~70μm,进一步优选为10~50μm。
上述基材膜和粘合剂层的厚度根据用途来选择,为了提高介电特性,基材膜有变得更薄的倾向。一般来说,当基材膜的厚度变薄、粘合剂层的厚度变厚时,带粘合剂层的层压体容易产生翘曲,操作性降低,但本发明的带粘合剂层的层压体即使在基材膜的厚度薄、粘合剂层的厚度厚的情况下,也几乎不发生层压体的翘曲。在本发明的带粘合剂层的层压体中,粘合剂层的厚度(A)、和基材膜的厚度(B)的比(A/B)优选为1以上且10以下,更优选为1以上且5以下。进而,粘合剂层的厚度优选比基材膜的厚度厚。
带粘合剂层的层压体的翘曲由于会影响FPC相关产品的制造工序的作业性,因此优选尽可能地减少翘曲。具体来说,将正方形的带粘合剂层的层压体以粘合剂层在上的方式载置在水平面上,此时,上述层压体的端部浮起的高度(H)与上述层压体的一边的长度(L)的比(H/L)优选小于0.05。该比更优选小于0.04,进一步优选小于0.03。当该比(H/L)小于0.05时,可更加抑制层压体的翘曲或卷曲,因此作业性极优。
另外,上述H/L的下限值,在H为0的情况,即为0。
使上述层压体的粘合剂层固化后,优选地,在1GHz的频率下测定的带粘合剂层的层压体的介电常数(ε)小于3.0,而且该介电损耗角正切(tanδ)小于0.01。上述介电常数更优选为2.7以下,介电损耗角正切更优选为0.003以下。只要介电常数小于3.0、且介电损耗角正切小于0.01,就可以适合用于应对近年来信号速度的进一步高速化、信号的进一步高频化的、介电特性的要求严格的FPC相关产品。介电常数和介电损耗角正切可以根据粘合剂成分的种类和含量、以及基材膜的种类等来调节,因此可以根据用途设定各种构成的层压体。
另外,将上述层压体的粘合剂层固化后,优选地,在1GHz的频率下测定的带粘合剂层的层压体的介电常数(ε)为2.0以上,而且该介电损耗角正切(tanδ)为0以上。
3.柔性覆铜层压板
本发明的柔性覆铜层压板的特征在于,使用上述带粘合剂层的层压体,将基材膜和铜箔贴合。即,本发明的柔性覆铜层压板按照基材膜、粘合剂层和铜箔的顺序构成。予以说明,粘合剂层和铜箔可以形成在基材膜的两面上。本发明的粘合剂组合物与含铜物品的粘合性优异,因此,本发明的柔性覆铜层压板作为一体化物的稳定性优异。
作为制造本发明的柔性覆铜层压板的方法,例如有如下方法:使上述层压体的粘合剂层与铜箔面接触,在80℃~150℃下进行热层压,再通过后固化,使粘合剂层固化。后固化的条件例如可以是100℃~200℃,30分钟~4小时。予以说明,上述铜箔没有特别限定,可以使用电解铜箔、轧制铜箔等。
4.柔性扁平电缆(FFC)
本发明的柔性扁平电缆的特征在于,使用上述带粘合剂层的层压体,将基材膜和铜配线贴合。即,本发明的柔性扁平电缆按照基材膜、粘合剂层和铜配线的顺序构成。予以说明,粘合剂层和铜配线可以形成在基材膜的两面上。本发明的粘合剂组合物与含铜物品的粘合性优异,因此,本发明的柔性扁平电缆作为一体化物的稳定性优异。
作为制造本发明的柔性扁平电缆的方法,例如有如下方法:使上述层压体的粘合剂层与铜配线接触,在80℃~150℃下进行热层压,再通过后固化,使粘合剂层固化。后固化的条件例如可以是100℃~200℃,30分钟~4小时。上述铜配线的形状没有特别限定,可以根据期望选择适宜的形状等。
实施例
基于实施例更具体地说明本发明,但本发明不限定于此。予以说明,在下述中,除非另有说明,份和%为质量基准。
1.评价方法
(1)重均分子量
按下述条件进行GPC测定,求出改性聚丙烯系树脂的Mw(A)。
Mw是通过将用GPC测定的滞留时间以标准聚苯乙烯的滞留时间为基准换算得到的。
装置:Alliance 2695(Waters公司制)
柱:TSKgel SuperMultipore HZ-H 2根,TSKgel SuperHZ2500 2根(东曹公司制)
柱温:40℃
洗脱液:四氢呋喃0.35ml/分钟
检测器:RI(差示折射率检测器)
(2)酸值
将1g改性聚丙烯系树脂(A)溶解在30ml甲苯中,使用与京都电子工业社制的滴定管“APB-510-20B”连接的该公司制的自动滴定装置“AT-510”。使用0.01mol/L的苄醇性KOH溶液作为滴定试剂,进行电位差滴定,计算出滴定每1g树脂的KOH的mg数。
(3)剥离粘合强度
准备厚度25μm的聚酰亚胺膜,在其中一侧表面上分别辊涂具有表1所示组成的实施例1~28、比较例1~13的粘合剂组合物。接着,将该带涂膜的膜静置于烘箱内,在90℃干燥3分钟,形成B阶状态的粘合剂层(厚度25μm),得到覆盖膜(实施例1~28、比较例1~13的带粘合剂层的层压体)。然后,将厚度35μm的压延铜箔以与覆盖膜的粘合剂层的表面接触的方式重叠在粘合剂层上,在温度120℃、压力0.4MPa、和速度0.5m/分钟的条件下进行层压。接着,将该层压体(聚酰亚胺膜/粘合剂层/铜箔)在温度180℃和压力3MPa的条件下,热压粘合30分钟,得到柔性覆铜层压板A。切割该柔性覆铜层压板A,制作规定大小的粘合试验片。
为了评价粘合性,以JIS C 6481“印刷线路板用覆铜层压板试验方法”为基准,在温度23℃和拉伸速度50mm/分钟的条件下,测定从聚酰亚胺膜剥离各粘合试验片的铜箔时的180°剥离粘合强度(N/mm)。测定时的粘合试验片的宽度为10mm。
(4)翘曲性
准备厚度25μm的聚酰亚胺膜(长200mm×宽200mm),在其一侧表面上辊涂具有表1所示组成的实施例1~28、比较例1~13的粘合剂组合物。接着,将该带涂膜的膜静置于烘箱内,在90℃干燥3分钟,形成B阶状态的粘合剂层(厚度25μm),得到覆盖膜(实施例1~28、比较例1~13的带粘合剂层的层压体,厚度50μm)。将上述覆盖膜以粘合剂层在上的方式载置在水平面上,测定4个角中每个角的垂直方向的浮起高度。求出这4点的平均高度(H)与层压体的一边的长度(L)的比(H/L),评价翘曲性。
<评价标准>
◎:H/L小于0.020
○:H/L为0.030以上、且小于0.05
×:H/L为0.10以上
(5)焊锡耐热性
以JIS C 6481“印刷线路板用覆铜层压板试验方法”为基准,在以下的条件下进行试验。将各粘合试验片剪切成20mm见方,在120℃进行30分钟的加热处理。然后,将聚酰亚胺膜的面朝上,在260℃的焊锡浴中漂浮60秒,观察粘合试验片表面的发泡状态。
<评价标准>
○:无起泡
×:有起泡
(6)介电特性(介电常数和介电损耗角正切)
(a)粘合剂固化物
准备厚度38μm的离型聚对苯二甲酸乙二醇酯膜,在其一侧表面上分别辊涂具有表1所示组成的实施例1~28、比较例1~13的粘合剂组合物。接着,将该带涂膜的膜静置于烘箱内,在90℃干燥3分钟,形成厚度50μm的覆膜(粘合性层),得到粘合片。接着,将该粘合片静置于烘箱内,进行150℃/60分钟或180℃/30分钟的加热处理。然后,剥离上述离型膜,制作试验片(150×120mm)。介电常数(ε)和介电损耗角正切(tanδ)使用网络分析仪85071E-300(Agilent公司制),通过分离介电质共振器法(SPDR法),在温度23℃、频率1GHz的条件下测定。
(b)带粘合剂层的层压体
准备厚度25μm的聚酰亚胺膜,其一侧表面上,辊涂具有表1所示组成的实施例1~28、比较例1~13的粘合剂组合物。接着,将该附涂膜的膜静置于烘箱内,在90℃使其干燥3分钟,制成B阶状态的粘合剂层(厚度25μm),得到覆盖膜(实施例1~28、比较例1~13的带粘合剂层的层压体,厚度50μm)。接着,将该覆盖膜静置于烘箱内,在150℃加热固化处理60分钟,制作试验片(120mm×100mm)。带粘合剂层的层压体的介电常数(ε)和介电损耗角正切(tanδ)使用网络分析仪85071E-300(Agilent公司制),通过分离介质谐振器法(SPDR法),在温度23℃、频率1GHz的条件下测定。
(7)粘合剂组合物的储存稳定性
将具有表1所示组成的实施例1~28、比较例1~13的粘合剂组合物分别装入玻璃瓶中密封,在5℃保存规定时间,观察组合物的结晶性。将保存规定时间后粘合剂组合物的流动性消失的点视为树脂的结晶化(储存稳定性不良)来进行评价。
<评价标准>
◎:1个月以上
○:2周以上、且不到1个月
△:1周以上、且不到2周
×:不到1周
(8)带粘合剂层的层压体的储存稳定性
准备厚度25μm的聚酰亚胺膜,在其一侧表面上辊涂具有表1所示组成的实施例1~28、比较例1~13的粘合剂组合物。接着,将该带涂膜的膜静置于烘箱内,在90℃干燥3分钟,形成B阶状态的粘合剂层(厚度25μm),得到覆盖膜(实施例1~28、比较例1~13的带粘合剂层的层压体,厚度50μm)。将制成的覆盖膜在23℃保存规定时间,将保存后的覆盖膜与单面铜基板(L/S=50μm/50μm,铜厚度18μm)在温度180℃、压力3MPa的条件下热压3分钟,评价树脂的埋入性。按以下基准评价树脂不向基板中埋入的保存时间。
<评价标准>
○:2个月以上
△:1周以上、且不到1个月
2.改性聚丙烯系树脂(A)的制造
通过以下所示的方法,制造改性聚丙烯系树脂a1~a3作为改性聚丙烯系树脂(A)。
(1)改性聚丙烯系树脂a1
制造金属茂催化剂作为聚合催化剂,使用圆筒部的最高温度设为170℃的双螺杆挤出机,将由65质量%的丙烯单元和35质量%的1-丁烯单元构成的丙烯-丁烯无规共聚物100质量份、马来酸酐1质量份、甲基丙烯酸月桂基酯0.3质量份和过氧化二叔丁基0.4质量份进行捏合反应。然后,在挤出机内进行减压脱气,除去残留的未反应物,制造改性聚丙烯系树脂a1。改性聚丙烯系树脂a1的重均分子量为7万,酸值为10mg KOH/g,丙烯/丁烯的质量比为65/35。
(2)改性聚丙烯系树脂a2
制造金属茂催化剂作为聚合催化剂,使用圆筒部的最高温度设定为170℃的双螺杆挤出机,将由60质量%的丙烯单元和40质量%的丁烯单元构成的丙烯-丁烯无规共聚物100质量份、马来酸酐1质量份、甲基丙烯酸月桂基酯0.3质量份和过氧化二叔丁基0.4质量份进行捏合反应。然后,在挤出机内进行减压脱气,除去残留的未反应物,制造改性聚丙烯系树脂a2。改性聚丙烯系树脂a2的重均分子量为6万,酸值为10mg KOH/g,丙烯/丁烯的质量比为60/40。
(3)改性聚丙烯系树脂a3
制造金属茂催化剂作为聚合催化剂,使用圆筒部的最高温度设定为170℃的双螺杆挤出机,将由80质量%的丙烯单元和20质量%的丁烯单元构成的丙烯-丁烯无规共聚物100质量份、马来酸酐1质量份、甲基丙烯酸月桂基酯0.3质量份和过氧化二叔丁基0.4质量份进行捏合反应。然后,在挤出机内进行减压脱气,除去残留的未反应物,制造改性聚丙烯系树脂a3。改性聚丙烯系树脂a3的重均分子量为6万,酸值为10mg KOH/g,丙烯/丁烯的质量比为80/20。
3.未改性的聚丙烯系树脂的制造
(1)未改性的聚丙烯系树脂c1
制造金属茂催化剂作为聚合催化剂,使65质量%的丙烯单元和35质量%的丁烯单元反应,得到未改性的聚丙烯系树脂c1。未改性的聚丙烯系树脂c1的重均分子量为15万,丙烯/丁烯的质量比为65/35。
(2)未改性的聚丙烯系树脂c2
制造金属茂催化剂作为聚合催化剂,使60质量%的丙烯单元和40质量%的丁烯单元反应,得到未改性的聚丙烯系树脂c2。未改性的聚丙烯系树脂c2的重均分子量为15万,丙烯/丁烯的质量比为60/40。
(3)未改性的聚丙烯系树脂c3
制造金属茂催化剂作为聚合催化剂,使75质量%的丙烯单元和25质量%的丁烯单元反应,得到未改性的聚丙烯系树脂c3。未改性的聚丙烯系树脂c3的重均分子量为15万,丙烯/丁烯的质量比为75/25。
4.粘合剂组合物的原料
4-1.环氧树脂(B)
(1)环氧树脂b1
使用DIC公司制的商品名“EPICLON HP-7200”(含有二环戊二烯骨架的环氧树脂)。
4-2.添加剂
(1)固化促进剂
使用四国化成社制的商品名“CUREZOL C11-Z”(咪唑系固化促进剂)。
(2)抗氧化剂
使用ADEKA公司制的商品名“AO-60”(受阻酚系抗氧化剂)。
4-3.有机溶剂
使用甲基环己烷、环己烷、甲苯、异丙醇、苄醇和甲乙酮。
5.粘合剂组合物的制造
将上述原料按照表1所示的比例添加到带有搅拌装置的1000ml烧瓶中,在室温下搅拌6小时使其溶解,由此制备粘合剂组合物并进行评价,结果示于表1和表2。予以说明,由于比较例4、5和13的粘合剂组合物的树脂成分没有溶解在溶剂中,因此未进行上述评价。
6.带粘合剂层的层压体的制造和评价
使用上述粘合剂组合物,如关于上述各评价方法的说明所述,制造带粘合剂层的层压体并进行评价,结果示于表1和表2。
根据上述表1和表2的结果,实施例1~11和13~28的粘合剂组合物在150℃加热固化60分钟的情况以及180℃加热固化30分钟的情况的任一种情况下,固化物的介电特性均优异,粘合性和焊锡耐热性也良好。另外,实施例12的粘合剂组合物在150℃加热固化60分钟时的固化物的介电特性优异,粘合性和焊锡耐热性也良好。进而,实施例1~17和20~28的粘合剂组合物在低温下的储存稳定性良好。
另外,实施例1~28的带粘合剂层的层压体的介电特性和储存稳定性均优异,翘曲得以抑制。
另一方面,只含有改性聚丙烯系树脂的比较例1和9~12以及未改性的聚丙烯系树脂的含量小于本发明范围的比较例8的粘合剂组合物的介电特性差,比较例9、11和12的低温储存稳定性也差。只含有未改性的聚丙烯系树脂的比较例2以及改性聚丙烯系树脂的含量小于本发明范围的比较例6和7的粘合剂组合物的粘合性差,而且介电特性和焊锡耐热性的至少一者也差。不含环氧树脂的比较例3的粘合剂组合物的粘合性和焊锡耐热性也差。
产业实用性
本发明的粘合剂组合物的粘合性和低温下的储存稳定性良好,介电特性优异。另外,使用该粘合剂组合物的带粘合剂层的层压体即使在基材膜很薄的情况下也几乎没有发生翘曲,作业性良好。因此,本发明的粘合剂组合物及使用其的带粘合剂层的层压体适用于制造FPC相关产品。
Claims (15)
1.粘合剂组合物,其特征在于,含有改性聚丙烯系树脂(A)、环氧树脂(B)和未改性的聚丙烯系树脂(C),
上述改性聚丙烯系树脂(A)是将未改性的聚丙烯系树脂(D)用含有α,β-不饱和羧酸或其衍生物的改性剂进行接枝改性而得到的树脂,
上述改性聚丙烯系树脂(A)的含量相对于上述粘合剂组合物的固体成分100质量份,为10质量份以上,且
上述未改性的聚丙烯系树脂(C)的含量相对于上述粘合剂组合物的固体成分100质量份,为20质量份以上且90质量份以下,
上述未改性的聚丙烯系树脂(C)的重均分子量Mw为30,000~250,000,
上述改性聚丙烯系树脂(A)中的丙烯的共聚比为70质量%以下,
在1GHz的频率下测定的上述粘合剂组合物的固化物的介电常数ε小于2.2。
2.权利要求1所述的粘合剂组合物,其特征在于,上述α,β-不饱和羧酸的衍生物是选自衣康酸酐、马来酸酐、乌头酸酐和柠康酸酐中的至少1种。
3.权利要求1或2所述的粘合剂组合物,其特征在于,来自上述α,β-不饱和羧酸或其衍生物的接枝部分的含有比例相对于上述改性聚丙烯系树脂(A)100质量%,为0.1~20质量%。
4.权利要求1~3任一项所述的粘合剂组合物,其特征在于,上述环氧树脂(B)是具有脂环骨架的多官能环氧树脂。
5.权利要求1~4任一项所述的粘合剂组合物,其特征在于,上述未改性的聚丙烯系树脂(C)中的丙烯的共聚比为70质量%以下。
6.权利要求1~5任一项所述的粘合剂组合物,其特征在于,上述未改性的聚丙烯系树脂(C)和上述未改性的聚丙烯系树脂(D)是选自乙烯-丙烯共聚物、丙烯-丁烯共聚物和乙烯-丙烯-丁烯共聚物中的至少1种。
7.权利要求1~6任一项所述的粘合剂组合物,其特征在于,含有抗氧化剂。
8.权利要求1~7任一项所述的粘合剂组合物,其特征在于,还含有有机溶剂,并且上述改性聚丙烯系树脂(A)、上述环氧树脂(B)和上述未改性的聚丙烯系树脂(C)溶解在上述有机溶剂中。
9.权利要求8所述的粘合剂组合物,其特征在于,上述有机溶剂含有脂环式烃溶剂和醇系溶剂,上述脂环式烃溶剂为甲基环己烷和/或环己烷,
相对于上述有机溶剂100质量份,上述脂环式烃的含量为20质量份以上且90质量份以下,
相对于上述有机溶剂100质量份,上述醇系溶剂的含量为1质量份以上且20质量份以下。
10.权利要求8或9所述的粘合剂组合物,其特征在于,含有甲苯。
11.权利要求8~10任一项所述的粘合剂组合物,其特征在于,固体成分的浓度为5质量%以上且50质量%以下。
12.带粘合剂层的层压体,其特征在于,具备:
含有权利要求1~11任一项所述的粘合剂组合物的粘合剂层,以及
与该粘合剂层的至少一侧表面相接的基材膜;
其中,上述粘合剂层为B阶状态。
13.权利要求12所述的带粘合剂层的层压体,其特征在于,上述基材膜是选自聚酰亚胺膜、聚醚醚酮膜、聚苯硫醚膜、芳族聚酰胺膜、聚萘二甲酸乙二醇酯膜、液晶聚合物膜、聚对苯二甲酸乙二醇酯膜、聚乙烯膜、聚丙烯膜、有机硅离型处理纸、聚烯烃树脂涂布纸、TPX膜、氟系树脂膜、和铜箔中的至少1种。
14.印刷线路板,其特征在于,包括含有权利要求1~11任一项所述的粘合剂组合物的粘合剂层。
15.柔性扁平电缆,其特征在于,包括含有权利要求1~11任一项所述的粘合剂组合物的粘合剂层。
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