CN105940561B - 各向异性导电膜及其制备方法 - Google Patents

各向异性导电膜及其制备方法 Download PDF

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CN105940561B
CN105940561B CN201580007303.9A CN201580007303A CN105940561B CN 105940561 B CN105940561 B CN 105940561B CN 201580007303 A CN201580007303 A CN 201580007303A CN 105940561 B CN105940561 B CN 105940561B
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articulamentum
conducting particles
resin layer
anisotropic conductive
conductive film
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CN105940561A (zh
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塚尾怜司
阿久津恭志
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Dexerials Corp
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Dexerials Corp
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Priority claimed from JP2014019855A external-priority patent/JP6409281B2/ja
Priority claimed from JP2014019866A external-priority patent/JP6233069B2/ja
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    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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Abstract

各向异性导电膜具有第1连接层和在其一面形成的第2连接层。第1连接层为光聚合树脂层，第2连接层为热或光阳离子、阴离子或自由基聚合性树脂层。在第1连接层的第2连接层一侧表面，各向异性导电连接用的导电粒子以相对于第1连接层的埋入率为80%以上或1%以上且20%以下的方式排列。

Description

各向异性导电膜及其制备方法
技术领域
本发明涉及各向异性导电膜及其制备方法。
背景技术
在IC芯片等电子零件的安装中广泛使用各向异性导电膜，近年来，从适用于高密度安装的观点出发，为了提高导通可靠性、绝缘性、提高安装导电粒子捕捉率、降低制备成本等，提出了在绝缘性粘接层上以单层排列有各向异性导电连接用的导电粒子的双层结构的各向异性导电膜(专利文献1)。
该双层结构的各向异性导电膜可通过以下方法来制备：在转印层上以单层且紧密填充的方式排列导电粒子后，将转印层进行双轴拉伸处理，由此形成以规定间隔均匀地排列有导电粒子的转印层后，将该转印层上的导电粒子转印于含有热固性树脂和聚合引发剂的绝缘性树脂层上，进而在已转印的导电粒子上层合含有热固性树脂但不含有聚合引发剂的另外的绝缘性树脂层(专利文献1)。
现有技术文献
专利文献
专利文献1：日本特许第4789738号说明书。
发明内容
发明所要解决的课题
但是，由于专利文献1的双层结构的各向异性导电膜使用不含有聚合引发剂的绝缘性树脂层，尽管以单层且以规定间隔均匀地排列导电粒子，但由于各向异性导电连接时的加热，不含有聚合引发剂的绝缘性树脂层中容易产生较大的树脂流动，沿着该树脂流动，导电粒子也变得容易流动，因此产生安装导电粒子捕捉率降低、发生短路、绝缘性降低等问题。
本发明的目的在于：解决以上现有的技术的问题点，在具有单层排列的导电粒子的多层结构的各向异性导电膜中实现良好的导通可靠性、良好的绝缘性和良好的安装导电粒子捕捉率。
解决课题的手段
本发明人等发现，在光聚合性树脂层上将导电粒子以按特定的比例埋入的方式单层排列后，通过照射紫外线而将导电粒子固定或临时固定，进而在已固定或临时固定的导电粒子上层合热或光阳离子、阴离子或自由基聚合性树脂层，由此得到的各向异性导电膜为可达成上述本发明的目的的构成；从而完成本发明。
即，本发明提供各向异性导电膜，其具有第1连接层和在其一面形成的第2连接层，其特征在于：
第1连接层为光聚合树脂层，
第2连接层为热或光阳离子、阴离子或自由基聚合性树脂层，
在第1连接层的第2连接层一侧表面，各向异性导电连接用的导电粒子以单层排列，且导电粒子相对于第1连接层的埋入率为80%以上或1%以上且20%以下。在这里，埋入率指导电粒子埋入第1连接层中的程度，可定义为导电粒子在第1连接层中埋入的深度Lb相对于导电粒子的粒径La的比例(埋入率)，可用“埋入率(%)=(Lb/La)×100”的式求得。
需说明的是，第2连接层优选为使用通过加热来引发聚合反应的热聚合引发剂的热聚合性树脂层，但也可以是使用通过光来引发聚合反应的光聚合引发剂的光聚合性树脂层。还可以是并用热聚合引发剂和光聚合引发剂的热·光聚合性树脂层。在这里，第2连接层在制备方面有限定为使用热聚合引发剂的热聚合性树脂层的情况。
本发明的各向异性导电膜中，为了应力驰豫等防止接合体的翘曲的目的，可在第1连接层的另一面具有与第2连接层近似相同的构成的第3连接层。即，可在第1连接层的另一面具有由热或光阳离子、阴离子或自由基聚合性树脂层构成的第3连接层。
需说明的是，第3连接层优选为使用通过加热来引发聚合反应的热聚合引发剂的热聚合性树脂层，但也可以是使用通过光来引发聚合反应的光聚合引发剂的光聚合性树脂层。还可以是并用热聚合引发剂和光聚合引发剂的热·光聚合性树脂层。在这里，第3连接层在制备方面有限定为使用热聚合引发剂的热聚合性树脂层的情况。
另外，本发明提供制备方法，其是上述各向异性导电膜的制备方法，其具有通过一步的光聚合反应来形成第1连接层的以下工序(A)~(C)、或通过两步的光聚合反应来形成第1连接层的后述工序(AA)~(DD)。
(通过一步的光聚合反应来形成第1连接层的情况)
工序(A)
在光聚合性树脂层上以单层排列导电粒子，使得导电粒子相对于第1连接层的埋入率为80%以上或1%以上且20%以下的工序；
工序(B)
通过对排列有导电粒子的光聚合性树脂层照射紫外线来进行光聚合反应，形成在表面固定有导电粒子的第1连接层的工序；和
工序(C)
在第1连接层的导电粒子一侧表面形成由热或光阳离子、阴离子或自由基聚合性树脂层构成的第2连接层的工序。
(通过两步的光聚合反应来形成第1连接层的情况)
工序(AA)
在光聚合性树脂层上以单层排列导电粒子，使得导电粒子相对于第1连接层的埋入率为80%以上或1%以上且20%以下的工序；
工序(BB)
通过对排列有导电粒子的光聚合性树脂层照射紫外线来进行光聚合反应，在表面形成临时固定有导电粒子的临时第1连接层的工序；
工序(CC)
在临时第1连接层的导电粒子一侧表面形成由热阳离子、阴离子或自由基聚合性树脂层构成的第2连接层的工序；和
工序(DD)
通过从与第2连接层相反的一侧对临时第1连接层照射紫外线来进行光聚合反应，将临时第1连接层正式固化而形成第1连接层的工序。
将在工序(CC)中形成第2连接层时使用的引发剂限定为热聚合引发剂，这是因为使得不会对作为各向异性导电膜的制品寿命、连接和连接结构体的稳定性造成不良影响。即，在分两步对第1连接层照射紫外线的情况下，由于其工序方面的制约，有不得不将第2连接层限定为热聚合固化性的层的情况。需说明的是，在连续进行两步照射的情况下，由于可通过与一步近似相同的工序来形成，所以可期待同等的作用效果。
另外，本发明提供制备方法，其是在第1连接层的另一面具有与第2连接层同样的构成的第3连接层的各向异性导电膜的制备方法，其除了以上工序(A)~(C)以外，还在工序(C)之后具有以下工序(Z)，或除了以上工序(AA)~(DD)以外，还在工序(DD)之后具有以下工序(Z)。
工序(Z)
在第1连接层的导电粒子一侧的相反面形成由热或光阳离子、阴离子或自由基聚合性树脂层构成的第3连接层的工序。
此外，本发明提供制备方法，其是在第1连接层的另一面具有与第2连接层近似相同的构成的第3连接层的各向异性导电膜的制备方法，其除了以上工序(A)~(C)以外，还在工序(A)之前具有以下工序(a)，或除了以上工序(AA)~(DD)以外，还在工序(AA)之前具有以下工序(a)。
工序(a)
在光聚合性树脂层的一面形成由热或光阳离子、阴离子或自由基聚合性树脂层构成的第3连接层的工序。
需说明的是，在具有该工序(a)的制备方法的工序(A)或工序(AA)中，只要在光聚合性树脂层的另一面以单层排列导电粒子，使得导电粒子相对于第1连接层的埋入率为80%以上或1%以上且20%以下即可。
在通过这样的工序设置第3连接层的情况下，由于上述理由，聚合引发剂优选限定为利用热反应的聚合引发剂。但是，若在设置第1连接层后通过对制品寿命、连接不会造成不良影响的方法来设置含有光聚合引发剂的第2和第3连接层，则可无特殊限制地制备含有光聚合引发剂的符合本发明的主旨的各向异性导电膜。
需说明的是，本发明的第2连接层或第3连接层中的任一者作为粘合层起作用的方案也包含在本发明中。
此外，本发明提供用上述各向异性导电膜将第1电子零件与第2电子零件各向异性导电连接而成的连接结构体。
发明的效果
本发明的各向异性导电膜具有由光聚合树脂层构成的第1连接层，和在其一面形成的由热或光阳离子、阴离子或自由基聚合性树脂层构成的第2连接层，并且在第1连接层的第2连接层一侧表面，各向异性导电连接用的导电粒子以导电粒子相对于第1连接层的埋入率为80%以上或1%以上且20%以下的方式单层排列。因此，可将导电粒子牢固地固定在第1连接层上，特别是在以埋入率为80%以上的方式单层排列的情况下，可将导电粒子更牢固地固定在第1连接层上。自然而然地各向异性导电膜的贴附性稳定地提高，各向异性导电连接的生产性也提高。而且，第1连接层的导电粒子下方(背面侧)的光自由基聚合性树脂层因导电粒子的存在而未充分地照射紫外线，因此固化率相对地降低，显示良好的压入性，结果可实现良好的导通可靠性、绝缘性、安装导电粒子捕捉率。需说明的是，在以埋入率为1%以上且20%以下的方式单层排列的情况下，由于第1连接层的树脂量不会大幅减少，所以可提高粘合性和粘接强度。
需说明的是，在各向异性导电连接中利用热的情况下，变成与通常的各向异性导电膜的连接方法同样的方法。在利用光的情况下，只要在反应结束以前利用连接工具进行压入即可。在这种情况下，连接工具等中，为了促进树脂流动、粒子的压入，多数情况下进行加热。另外，在并用热和光的情况下，也只要与上述同样地进行即可。
附图说明
[图1] 图1为本发明的各向异性导电膜的截面图。
[图2] 图2为本发明的各向异性导电膜的制备工序(A)的说明图。
[图3A] 图3A为本发明的各向异性导电膜的制备工序(B)的说明图。
[图3B] 图3B为本发明的各向异性导电膜的制备工序(B)的说明图。
[图4A] 图4A为本发明的各向异性导电膜的制备工序(C)的说明图。
[图4B] 图4B为本发明的各向异性导电膜的制备工序(C)的说明图。
[图5] 图5为本发明的各向异性导电膜的截面图。
[图6] 图6为本发明的各向异性导电膜的制备工序(AA)的说明图。
[图7A] 图7A为本发明的各向异性导电膜的制备工序(BB)的说明图。
[图7B] 图7B为本发明的各向异性导电膜的制备工序(BB)的说明图。
[图8A] 图8A为本发明的各向异性导电膜的制备工序(CC)的说明图。
[图8B] 图8B为本发明的各向异性导电膜的制备工序(CC)的说明图。
[图9A] 图9A为本发明的各向异性导电膜的制备工序(DD)的说明图。
[图9B] 图9B为本发明的各向异性导电膜的制备工序(DD)的说明图。
具体实施方式
<<各向异性导电膜>>
以下详细地说明发明的各向异性导电膜的优选的一例。
如图1所示，本发明的各向异性导电膜1具有在由使光聚合性树脂层光聚合而成的光聚合树脂层构成的第1连接层2的一面、形成有由热或光阳离子、阴离子或自由基聚合性树脂层构成的第2连接层3的结构。而且，在第1连接层2的第2连接层3一侧的表面2a，导电粒子4为了各向异性导电连接而以单层排列，优选均匀地排列。在这里，均匀指导电粒子沿平面方向排列的状态。这种规律性也可以一定的间隔来设置。
<第1连接层2>
由于构成本发明的各向异性导电膜1的第1连接层2为使光阳离子、阴离子或自由基聚合性树脂层等光聚合性树脂层光聚合而成的光聚合树脂层，所以可固定导电粒子。另外，由于进行聚合，所以在各向异性导电连接时即使进行加热树脂也变得难以流动，因此可大幅抑制短路的发生，由此可提高导通可靠性和绝缘性，且也可提高安装粒子捕捉效率。特别优选的第1连接层2为使含有丙烯酸酯化合物和光自由基聚合引发剂的光自由基聚合性树脂层进行光自由基聚合而成的光自由基聚合树脂层。以下对第1连接层2为光自由基聚合树脂层的情况进行说明。
(丙烯酸酯化合物)
作为形成丙烯酸酯单元的丙烯酸酯化合物，可使用以往公知的光自由基聚合性丙烯酸酯。例如可使用单官能(甲基)丙烯酸酯(在这里，(甲基)丙烯酸酯包含丙烯酸酯和甲基丙烯酸酯)、双官能以上的多官能(甲基)丙烯酸酯。在本发明中，为了使粘接剂为热固性，优选丙烯酸类单体的至少一部分使用多官能(甲基)丙烯酸酯。
若第1连接层2中的丙烯酸酯化合物的含量过少，则有变得难以取得与第2连接层3的粘度差的倾向，若过多，则有固化收缩大从而操作性降低的倾向，因此优选为2~70质量%，更优选为10~50质量%。
(光自由基聚合引发剂)
作为光自由基聚合引发剂，可从公知的光自由基聚合引发剂中适宜地选择使用。例如可列举出苯乙酮类光聚合引发剂、苯偶酰缩酮类光聚合引发剂、磷类光聚合引发剂等。
相对于100质量份的丙烯酸酯化合物，光自由基聚合引发剂的使用量若过少，则光自由基聚合无法充分进行，若过多，则导致刚性降低，因此优选为0.1~25质量份，更优选为0.5~15质量份。
(导电粒子)
作为导电粒子，可从以往公知的在各向异性导电膜中使用的导电粒子中适宜地选择使用。例如可列举出镍、钴、银、铜、金、钯等金属粒子，金属被覆树脂粒子等。也可并用2种以上。
作为导电粒子的平均粒径，若过小，则无法吸收配线的高度偏差从而有电阻升高的倾向，若过大，则有导致短路的倾向，因此优选为1~10μm，更优选为2~6μm。
这样的导电粒子在第1连接层2中的粒子量若过少，则安装导电粒子捕捉数降低从而各向异性导电连接变得困难，若过多，则有短路之虞，因此优选每1平方mm为50~50000个，更优选为200~30000个。
在第1连接层2中，可根据需要并用苯氧树脂、环氧树脂、不饱和聚酯树脂、饱和聚酯树脂、聚氨酯树脂、丁二烯树脂、聚酰亚胺树脂、聚酰胺树脂、聚烯烃树脂等成膜树脂。在第2连接层和第3连接层中也可同样地并用。
第1连接层2的层厚度若过薄，则有安装导电粒子捕捉率降低的倾向，若过厚，则有导通电阻升高的倾向，因此优选为1.0~6.0μm，更优选为2.0~5.0μm。
在第1连接层2中也可进一步含有环氧化合物和热或光阳离子或阴离子聚合引发剂。在这种情况下，如下所述，第2连接层3也优选设为含有环氧化合物和热或光阳离子或阴离子聚合引发剂的热或光阳离子或阴离子聚合性树脂层。由此，可提高层间剥离强度。对于环氧化合物和热或光阳离子或阴离子聚合引发剂，在第2连接层3中进行说明。
在第1连接层2中，如图1所示，导电粒子4埋入在第1连接层2中。若将埋入的程度定义为导电粒子4在第1连接层2中埋入的深度Lb相对于导电粒子4的粒径La的比例(埋入率)，则埋入率可用“埋入率(%)=(Lb/La)×100”的式求得。
在本发明中，为了解决“为了实现良好的安装导电粒子捕捉性而使得导电粒子可固定在想要的位置”的课题，调整导电粒子4相对于第1连接层2的埋入率，使得为80%以上，优选为85%以上，更优选比90%大。在这种情况下，导电粒子4可完全埋没在第1连接层2中，但优选设为120%以下。
另外，在本发明中，为了平衡性良好地解决“为了实现良好的安装导电粒子捕捉性而使得导电粒子可固定在想要的位置”的课题、和“为了提高第1连接层2与被粘接体之间的粘接强度而确保在导电粒子的下方存在的树脂量从而实现良好的粘合性”的课题，调整导电粒子4相对于第1连接层2的埋入率，使得其下限为1%以上，优选比1%大，上限为20%以下，优选低于20%。
需说明的是，导电粒子4相对于第1连接层2的埋入率的调整例如可通过利用表面具备剥离材料的橡胶辊重复挤压来进行。具体而言，在要减小埋入率的情况下，只要减少重复次数即可，在要增大的情况下，只要增多重复次数即可。
另外，在对光聚合性树脂层照射紫外线从而形成第1连接层2的情况下，可从未配置导电粒子的一侧的面和配置导电粒子的一侧的面中的任一面进行照射，但在从配置导电粒子的一侧进行照射的情况下，在第1连接层2中，可使位于导电粒子4与第1连接层2的最外表面2b之间的第1连接层的区域2X的固化率比位于相互毗邻的导电粒子4间的第1连接层的区域2Y的固化率低。由此，在进行各向异性导电连接的热压接时，变得容易排除第1连接层的区域2X，导通可靠性提高。在这里，固化率是定义为乙烯基的减少比率的数值，第1连接层的区域2X的固化率优选为40~80%，第1连接层的区域2Y的固化率优选为70~100%。
在这里，在从未配置导电粒子的面进行照射的情况下，在第1连接层的区域2X和2Y实质上不再有固化率的差异。这在ACF制品品质方面是优选的。其原因在于：在ACF制备工序中，促进导电粒子的固定，可确保稳定的品质。其原因在于：在作为制品进行一般的长条化时，在卷绕开始和卷绕结束，可使对排列的导电粒子施加的压力近似相同，可防止排列的混乱。
需说明的是，形成第1连接层2时的光自由基聚合可通过一步(即一次光照射)来进行，但也可通过两步(即两次光照射)来进行。在这种情况下，第二步的光照射优选在第1连接层2的一面形成第2连接层3后，在含氧气氛(大气中)下从第1连接层2的另一面一侧进行。由此，可期待以下效果：自由基聚合反应被氧阻聚，未固化成分的表面浓度提高，可提高粘合性。另外，由于聚合反应也会因通过两步来进行固化而复杂化，所以也可期待能够细致地控制树脂、粒子的流动性。
在这样的两步的光自由基聚合中第1连接层的区域2X在第一步的固化率优选为10~50%，在第二步的固化率优选为40~80%，第1连接层的区域2Y在第一步的固化率优选为30~90%，在第二步的固化率优选为70~100%。
另外，在形成第1连接层2时的光自由基聚合反应通过两步来进行的情况下，作为自由基聚合引发剂也可只使用1种，但使用引发自由基反应的波长区域不同的2种光自由基聚合引发剂因粘合性提高而优选。例如优选将利用来自于LED光源的波长为365nm的光引发自由基反应的光自由基聚合引发剂(例如IRGACURE369，BASF Japan Ltd. (BASFジャパン(株)))和利用来自于高压汞灯光源的光引发自由基反应的光自由基聚合引发剂(例如IRGACURE2959、BASF Japan Ltd. (BASFジャパン(株)))并用。由于树脂的结合因这样使用2种不同的光自由基聚合引发剂而复杂化，所以能够更细致地控制连接时树脂的热流动的行为。其原因在于：在进行各向异性导电连接的压入时，粒子变得容易受到在厚度方向施加的力，向面方向的流动得到抑制，因此变得更容易展现本发明的效果。
另外，第1连接层2的用流变仪进行测定时的最低熔融粘度比第2连接层3的最低熔融粘度高，具体而言[第1连接层2的最低熔融粘度(mPa·s)]/[第2连接层3的最低熔融粘度(mPa·s)]的数值优选为1~1000，更优选为4~400。需说明的是，就各自的优选的最低熔融粘度而言，对前者为100~100000mPa·s，更优选为500~50000mPa·s。对后者优选为0.1~10000mPa·s，更优选为0.5~1000mPa·s。
第1连接层2的形成可通过以下方法来进行：通过膜转印法、模具转印法、喷墨法、静电附着法等方法使导电粒子附着于含有光自由基聚合性丙烯酸酯和光自由基聚合引发剂的光自由基聚合性树脂层上，从导电粒子一侧、其相反一侧、或两侧照射紫外线。特别是从可将第1连接层的区域2X的固化率抑制为相对较低的观点出发，优选只从导电粒子一侧照射紫外线。
<第2连接层3>
第2连接层3由热或光阳离子、阴离子或自由基聚合性树脂层构成，优选由含有环氧化合物和热或光阳离子或阴离子聚合引发剂的热或光阳离子或阴离子聚合性树脂层、或含有丙烯酸酯化合物和热或光自由基聚合引发剂的热或光自由基聚合性树脂层构成。在这里，由热聚合性树脂层形成第2连接层3，这由于第2连接层3的聚合反应不会因形成第1连接层2时的紫外线照射而发生，所以在生产的简便性和品质稳定性方面是理想的。
在第2连接层3为热或光阳离子或阴离子聚合性树脂层的情况下，可进一步含有丙烯酸酯化合物和热或光自由基聚合引发剂。由此可提高与第1连接层2的层间剥离强度。
(环氧化合物)
在第2连接层3为含有环氧化合物和热或光阳离子或阴离子聚合引发剂的热或光阳离子或阴离子聚合性树脂层的情况下，作为环氧化合物，可优选列举出分子内具有2个以上环氧基的化合物或树脂。它们可以是液态或固态。
(热阳离子聚合引发剂)
作为热阳离子聚合引发剂，可采用作为环氧化合物的热阳离子聚合引发剂公知的物质，例如为利用热产生能够使阳离子聚合性化合物进行阳离子聚合的酸的物质，可使用公知的碘盐、锍盐、盐、二茂铁类等，可优选使用对温度显示良好的潜伏性的芳族锍盐。
热阳离子聚合引发剂的掺混量若过少，则有固化不良的倾向，若过多，则有制品寿命降低的倾向，因此相对于100质量份的环氧化合物，优选为2~60质量份，更优选为5~40质量份。
(热阴离子聚合引发剂)
作为热阴离子聚合引发剂，可采用作为环氧化合物的热阴离子聚合引发剂公知的物质，例如为利用热产生能够使阴离子聚合性化合物进行阴离子聚合的碱的物质，可使用公知的脂族胺类化合物、芳族胺类化合物、仲胺或叔胺类化合物、咪唑类化合物、聚硫醇类化合物、三氟化硼-胺络合物、双氰胺、有机酸酰肼等，可优选使用对温度显示良好的潜伏性的胶囊化咪唑类化合物。
热阴离子聚合引发剂的掺混量若过少，则有固化不良的倾向，若过多，则有制品寿命降低的倾向，因此相对于100质量份的环氧化合物，优选为2~60质量份，更优选为5~40质量份。
(光阳离子聚合引发剂和光阴离子聚合引发剂)
作为环氧化合物用的光阳离子聚合引发剂或光阴离子聚合引发剂，可适宜地使用公知的物质。
(丙烯酸酯化合物)
在第2连接层3为含有丙烯酸酯化合物和热或光自由基聚合引发剂的热或光自由基聚合性树脂层的情况下，作为丙烯酸酯化合物，可从关于第1连接层2说明的物质中适宜地选择使用。
(热自由基聚合引发剂)
另外，作为热自由基聚合引发剂，例如可列举出有机过氧化物或偶氮类化合物等，但可优选使用不产生导致气泡的氮的有机过氧化物。
若热自由基聚合引发剂的使用量过少，则导致固化不良，若过多，则导致制品寿命降低，因此相对于100质量份的丙烯酸酯化合物，优选为2~60质量份，更优选为5~40质量份。
(光自由基聚合引发剂)
作为丙烯酸酯化合物用的光自由基聚合引发剂，可使用公知的光自由基聚合引发剂。
若光自由基聚合引发剂的使用量过少，则导致固化不良，若过多，则导致制品寿命降低，因此相对于100质量份的丙烯酸酯化合物，优选为2~60质量份，更优选为5~40质量份。
(第3连接层5)
以上对图1的双层结构的各向异性导电膜进行了说明，但如图5所示，在第1连接层2的另一面可形成第3连接层5。由此，可得到能够更细致地控制层整体的流动性的效果。在这里，作为第3连接层5，可设为与前述第2连接层3相同的构成。即，第3连接层5由热或光阳离子或阴离子聚合性树脂层(优选含有环氧化合物和热或光阳离子或阴离子聚合引发剂的聚合性树脂层)、或热或光自由基聚合性树脂层(优选含有丙烯酸酯化合物和热或光自由基聚合引发剂的聚合性树脂层)构成。这样的第3连接层5可在第1连接层的一面形成第2连接层后、在第1连接层的另一面形成，也可在形成第2连接层前、在第1连接层或作为其前体的光聚合性树脂层的另一面(未形成第2连接层的面)预先形成第3连接层。
<<各向异性导电膜的制备方法>>
对于本发明的各向异性导电膜的制备方法，可列举出进行一步的光聚合反应的制备方法、和进行两步的光聚合反应的制备方法。
<进行一步的光聚合反应的制备方法>
对通过一步来进行光聚合从而制备图1 (图4B)的各向异性导电膜的一例进行说明。该制备例具有以下工序(A)~(C)。
(工序(A))
如图2所示，在根据需要在剥离膜30上形成的光聚合性树脂层31上以单层排列导电粒子4，使得埋入率为80%以上或1%以上且20%以下。作为导电粒子4的排列方法，无特殊限制，可采用日本特许第4789738号的实施例1的对未拉伸聚丙烯膜利用双轴拉伸操作的方法、或日本特开2010-33793号公报的使用模具的方法等。需说明的是，作为排列的程度，考虑连接对象的尺寸、导通可靠性、绝缘性、安装导电粒子捕捉率等，优选平面上相互隔开1~100μm左右进行排列。
埋入率的调整可通过重复挤压橡胶辊等弹性体来进行。
(工序(B))
接着，如图3A所示，对于排列有导电粒子4的光聚合性树脂层31，通过照射紫外线(UV)来进行光聚合反应，形成在表面固定有导电粒子4的第1连接层2。在这种情况下，可从导电粒子一侧照射紫外线(UV)，也可从相反一侧进行照射，但在从导电粒子一侧照射紫外线(UV)的情况下，如图3B所示，可使位于导电粒子4与第1连接层2的最外表面之间的第1连接层的区域2X的固化率比位于相互毗邻的导电粒子4间的第1连接层的区域2Y的固化率低。由此，也可同时具备粒子的背面侧的固化性确实地降低从而使得接合时的压入容易，且防止粒子流动的效果。
(工序(C))
接着，如图4A所示，在第1连接层2的导电粒子4一侧表面形成由热或光阳离子、阴离子或自由基聚合性树脂层构成的第2连接层3。作为具体的一例，将在剥离膜40上通过常规方法形成的第2连接层3放置在第1连接层2的导电粒子4一侧表面，以不产生过大的热聚合的程度进行热压接。然后，通过去除剥离膜30和40从而可得到图4B的各向异性导电膜。
需说明的是，图5的各向异性导电膜100可通过在工序(C)之后实施以下工序(Z)来得到。
(工序(Z))
在第1连接层的导电粒子一侧的相反面，优选与第2连接层同样地形成由热或光阳离子、阴离子或自由基聚合性树脂层构成的第3连接层。由此可得到图5的各向异性导电膜。
另外，图5的各向异性导电膜100也可不进行工序(Z)，而通过在工序(A)之前实施以下工序(a)来得到。
(工序(a))
该工序为在光聚合性树脂层的一面形成由热或光阳离子、阴离子或自由基聚合性树脂层构成的第3连接层的工序。通过紧接着该工序(a)实施工序(A)、(B)和(C)从而可得到图5的各向异性导电膜100。但是，在工序(A)中，在光聚合性树脂层的另一面以单层排列导电粒子，使得埋入率为80%以上或1%以上且20%以下。
(进行两步的光聚合反应的制备方法)
接着，对通过两步来进行光聚合从而制备图1 (图4B)的各向异性导电膜的一例进行说明。该制备例具有以下工序(AA)~(DD)。
(工序(AA))
如图6所示，在根据需要在剥离膜30上形成的光聚合性树脂层31上以单层排列导电粒子4，使得埋入率为80%以上或1%以上且20%以下。作为导电粒子4的排列方法，无特殊限制，可采用日本特许第4789738号的实施例1的对未拉伸聚丙烯膜利用双轴拉伸操作的方法、或日本特开2010-33793号公报的使用模具的方法等。需说明的是，作为排列的程度，考虑连接对象的尺寸、导通可靠性、绝缘性、安装导电粒子捕捉率等，优选平面上相互隔开1~100μm左右进行排列。
(工序(BB))
接着，如图7A所示，对于排列有导电粒子4的光聚合性树脂层31，通过照射紫外线(UV)来进行光聚合反应，形成在表面临时固定有导电粒子4的临时第1连接层20。在这种情况下，可从导电粒子一侧照射紫外线(UV)，也可从相反一侧进行照射，但在从导电粒子一侧照射紫外线(UV)的情况下，如图7B所示，可使位于导电粒子4与临时第1连接层20的最外表面之间的第1连接层的区域2X的固化率比位于相互毗邻的导电粒子4间的第1连接层的区域2Y的固化率低。
(工序(CC))
接着，如图8A所示，在临时第1连接层20的导电粒子4一侧表面形成由热阳离子、阴离子或自由基聚合性树脂层构成的第2连接层3。作为具体的一例，将在剥离膜40上通过常规方法形成的第2连接层3放置在第1连接层2的导电粒子4一侧表面，以不产生过大的热聚合的程度进行热压接。然后，通过去除剥离膜30和40从而可得到图8B的临时各向异性导电膜50。
(工序DD)
接着，如图9A所示，通过从与第2连接层3相反的一侧对临时第1连接层20照射紫外线来进行光聚合反应，将临时第1连接层20正式固化从而形成第1连接层2。由此，可得到图9B的各向异性导电膜1。该工序中的紫外线的照射优选相对于临时第1连接层从垂直方向进行。另外，优选经由掩模进行照射、或根据照射部位对照射光量设定差额，使得第1连接层的区域2X与2Y的固化率差不消失。
需说明的是，在通过两步来进行光聚合的情况下，图5的各向异性导电膜100可通过在工序(DD)之后实施以下工序(Z)来得到。
(工序(Z))
在第1连接层的导电粒子一侧的相反面优选与第2连接层同样地形成由热或光阳离子、阴离子或自由基聚合性树脂层构成的第3连接层。由此可得到图5的各向异性导电膜。
另外，图5的各向异性导电膜100也可不进行工序(Z)，而通过在工序(AA)之前实施以下工序(a)来得到。
(工序(a))
该工序为在光聚合性树脂层的一面形成由热或光阳离子、阴离子或自由基聚合性树脂层构成的第3连接层的工序。通过紧接着该工序(a)实施工序(AA)~(DD)从而可得到图5的各向异性导电膜100。但是，在工序(AA)中，在光聚合性树脂层的另一面以单层排列导电粒子，使得埋入率为80%以上或1%以上且20%以下。在这种情况下，作为形成第2连接层时使用的聚合引发剂，优选应用热聚合引发剂。在光聚合引发剂的情况下，在工序方面有对作为各向异性导电膜的制品寿命、连接和连接结构体的稳定性造成不良影响之虞。
<<连接结构体>>
这样得到的各向异性导电膜可在将IC芯片、IC模块等第1电子零件与柔性基板、玻璃基板等第2电子零件进行各向异性导电连接时优选应用。这样得到的连接结构体也是本发明的一部分。需说明的是，从提高导通可靠性的观点出发，优选将各向异性导电膜的第1连接层一侧配置在柔性基板等第2电子零件一侧，将第2连接层一侧配置在IC芯片等第1电子零件一侧。
实施例
以下通过实施例来具体地说明本发明。
实施例1~6、比较例1
在依据日本特许第4789738号的实施例1的操作进行导电粒子的排列的同时，按照表1所示的配方(质量份)制备第1连接层和第2连接层层合而成的双层结构的各向异性导电膜。
(第1连接层)
具体而言，首先用醋酸乙酯或甲苯将丙烯酸酯化合物和光自由基聚合引发剂等制备混合液，使得固体成分为50质量%。将该混合液涂布在厚度为50μm的聚对苯二甲酸乙二醇酯膜上，使得干燥厚度为5μm，在80℃的烘箱中干燥5分钟，由此形成作为第1连接层的前体层的光自由基聚合性树脂层。
接着，对于得到的光自由基聚合性树脂层，将平均粒径为4μm的导电粒子(镀Ni/Au树脂粒子，AUL704，积水化学工业(株))相互隔开4μm，通过调整利用橡胶辊的重复挤压次数，由此以使导电粒子相对于第1连接层的埋入率为粒径的表1所示的百分率的方式单层排列。进而，从该导电粒子一侧对光自由基聚合性树脂层照射波长为365nm、累积光量为4000mJ/cm2的紫外线，由此形成在表面固定有导电粒子的第1连接层。
(第2连接层)
用醋酸乙酯或甲苯将热固性树脂和潜伏性固化剂等制备混合液，使得固体成分为50质量%。将该混合液涂布在厚度为50μm的聚对苯二甲酸乙二醇酯膜上，使得干燥厚度为12μm，在80℃的烘箱中干燥5分钟，由此形成第2连接层。
(各向异性导电膜)
将这样得到的第1连接层与第2连接层以导电粒子为内侧的方式层合，由此得到各向异性导电膜。
(连接结构样品体)
使用得到的各向异性导电膜，以180℃、80MPa、5秒的条件将0.5×1.8×20.0mm的大小的IC芯片(凸点尺寸为30×85μm，凸点高度为15μm，凸点间距为50μm)安装在0.5×50×30mm的大小的Corning Inc. (コーニング社)制的玻璃配线基板(1737F)上，从而得到连接结构样品体。
(试验评价)
对于得到的连接结构样品体，如以下说明所述，试验评价各向异性导电膜的“安装导电粒子捕捉率”、“导通可靠性”、“连结粒子个数”和“绝缘性”。将得到的结果示出于表1中。
需说明的是，在评价“绝缘性”的情况下，使用以180℃、80MPa、5秒的条件将0.5×1.5×13mm的大小的IC芯片(镀金凸点尺寸为25×140μm，凸点高度为15μm，凸点间间隙为7.5μm)安装在0.5×50×30mm的大小的Corning Inc. (コーニング社)制的玻璃配线基板(1737F)上而得到的连接结构样品体。
“安装导电粒子捕捉率”
依据以下数学式求得“加热·加压后(实际安装后)的连接结构样品体的凸点上实际捕捉的粒子量”相对于“加热·加压前的连接结构样品体的凸点上存在的理论粒子量”的比例。
安装导电粒子捕捉率(%)={[加热加压后的凸点上的粒子数]/[加热加压前的凸点上的粒子数]}×100
“导通可靠性”
使用数字万用表(Agilent Technologies Japan, Ltd. (アジレント·テクノロジー(株)))测定将连接结构样品体在85℃、85%RH的高温高湿环境下放置500小时后的导通电阻。在实际使用方面希望为4Ω以下。
“连结粒子个数”
用倍率为50倍的电子显微镜观察得到的连接结构样品体的10mm见方的区域，将2个以上的导电粒子呈线状或块状连结而成的连结体计为一个连结粒子，数出这样的连结粒子的个数。例如，在2个导电粒子连结而成的连结粒子有2个、4个连结粒子连结而成的连结粒子有1个的情况下，连结粒子数为3个。若连结个数增大，则构成连结粒子的导电粒子数也有增大的倾向，即变得容易损害占据凸点间间隙的导电粒子的独立性，因此短路的发生概率有增大的倾向。
“绝缘性(短路的发生率)”
求得7.5μm间隙的梳齿TEG图案的短路发生率。在实际使用方面希望为100ppm以下。
[表1]
由表1可知，对于实施例1~6的各向异性导电膜，由于导电粒子相对于第1连接层的埋入率为80%以上，所以连结粒子个数也为10个以下，安装导电粒子捕捉率、导通可靠性、短路的发生率的各评价项目在实际使用方面均显示优选的结果。
与之相对的是，对于比较例1的各向异性导电膜，由于导电粒子相对于第1连接层的埋入率为低于80%的75%，所以连结粒子数增大，短路发生率增大为50ppm。
实施例7
在形成第1连接层时以累积光量为2000mJ/cm2照射紫外线，除此之外，与实施例1相同地制备各向异性导电膜。从该各向异性导电膜的第1连接层一侧进一步以累积光量为2000mJ/cm2照射波长为365nm的紫外线，由此得到从第1连接层的两面照射了紫外线的实施例7的各向异性导电膜。使用该各向异性导电膜，与实施例1的各向异性导电膜相同地制备连接结构样品体并进行评价，得到大致同等的在实际使用方面不存在问题的结果，但安装导电粒子捕捉率有进一步得到改善的倾向。
实施例8~12、比较例2~3
通过调整利用橡胶辊的重复挤压次数，将导电粒子以使导电粒子相对于第1连接层的埋入率为粒径的表2所示的百分率的方式单层排列，除此之外，重复实施例1的操作，由此取得各向异性导电膜，进而得到连接结构样品体。
(试验评价)
对于得到的连接结构样品体，与实施例1相同地试验评价各向异性导电膜的“安装导电粒子捕捉率”、“导通可靠性”和“绝缘性(短路发生率)”，进而如以下说明所述，试验评价“第1连接层一侧的“粘合力””和“粘接强度(芯片剪切力)”。将得到的结果示出于表2中。
[表2]
由表2可知，对于实施例8~12的各向异性导电膜，由于导电粒子相对于第1连接层的埋入率为1%以上且20%以下，所以粘合力、粘接强度、安装导电粒子捕捉率、导通可靠性、绝缘性(短路发生率)的各评价项目在实际使用方面均显示优选的结果。
与之相对的是，对于比较例2的各向异性导电膜，由于导电粒子相对于第1连接层的埋入率超过20%，所以粘合力和粘接强度比实施例8~12的各向异性导电膜差。另外，短路发生率也增加约2.5倍。对于比较例3的各向异性导电膜，由于导电粒子相对于第1连接层的埋入率低于1%，所以安装导电粒子捕捉率比实施例8~12的各向异性导电膜降低，另外作为绝缘性的评价指标的短路发生率也增加约7.5倍。
实施例13
在形成第1连接层时以累积光量2000mJ/cm2照射紫外线，除此之外，与实施例8相同地制备各向异性导电膜。从该各向异性导电膜的第1连接层一侧进一步以累积光量2000mJ/cm2照射波长为365nm的紫外线，由此得到从第1连接层的两面照射了紫外线的实施例13的各向异性导电膜。使用该各向异性导电膜，与实施例8的各向异性导电膜相同地制备连接结构样品体并进行评价，得到大致同等的在实际使用方面不存在问题的结果，但安装导电粒子捕捉率有进一步得到改善的倾向。
产业上的可利用性
本发明的各向异性导电膜具有将由光聚合树脂层构成的第1连接层与由热或光阳离子或阴离子聚合性树脂层、或热或光自由基聚合性树脂层构成的第2连接层层合而成的双层结构，并且在第1连接层的第2连接层一侧表面以单层排列各向异性导电连接用的导电粒子，使得相对于第1连接层的埋入率为80%以上。因此，可将导电粒子良好地固定在第1连接层上，从而显示良好的安装导电粒子捕捉率、导通可靠性、连结粒子个数、绝缘性。另外，在本发明的各向异性导电膜的另外的方案中，各向异性导电连接用的导电粒子以相对于第1连接层的埋入率为1%以上且20%以下的方式单层排列。因此，第1连接层显示良好的粘合性和粘接强度，从而显示良好的导通可靠性、绝缘性(短路发生率)、安装导电粒子捕捉率。因此，这些本发明的各向异性导电膜对于IC芯片等电子零件向配线基板的各向异性导电连接是有用的。这样的电子零件的配线的狭小化不断进展，本发明特别是在有助于这样的技术进步的情况下展现该效果。
符号说明
1、100 各向异性导电膜
2、 第1连接层
2X、2Y 第1连接层的区域
3 第2连接层
4 导电粒子
5 第3连接层
30、40 剥离膜
20 临时第1连接层
31 光聚合性树脂层
50 临时各向异性导电膜
La 导电粒子的粒径
Lb 导电粒子在第1连接层中埋入的深度

Claims (14)

1.各向异性导电膜，其具有第1连接层和在其一面形成的第2连接层，其特征在于：
第1连接层为光聚合树脂层，其中，第1连接层为使含有丙烯酸酯化合物和光自由基聚合引发剂的光自由基聚合性树脂层进行光自由基聚合而成的光自由基聚合树脂层，第1连接层进一步含有环氧化合物和热或光阳离子或阴离子聚合引发剂，第1连接层中的丙烯酸酯化合物的含量为2~70质量%，
第2连接层为热或光阳离子、阴离子或自由基聚合性树脂层，
在第1连接层的第2连接层一侧表面，各向异性导电连接用的导电粒子以单层排列，且导电粒子相对于第1连接层的埋入率为80%以上或1%以上且20%以下，第1连接层中导电粒子的粒子量是每1平方mm为50~50000个。
2.权利要求1所述的各向异性导电膜，其中，第2连接层为含有环氧化合物和热或光阳离子或阴离子聚合引发剂的热或光阳离子或阴离子聚合性树脂层、或含有丙烯酸酯化合物和热或光自由基聚合引发剂的热或光自由基聚合性树脂层。
3.权利要求2所述的各向异性导电膜，其中，第2连接层为含有环氧化合物和热或光阳离子或阴离子聚合引发剂的热或光阳离子或阴离子聚合性树脂层，进一步含有丙烯酸酯化合物和热或光自由基聚合引发剂。
4.权利要求1~3中任一项所述的各向异性导电膜，其中，在第1连接层中，位于导电粒子与第1连接层的最外表面之间的区域的第1连接层的固化率比位于相互毗邻的导电粒子间的区域的第1连接层的固化率低。
5.权利要求1~3中任一项所述的各向异性导电膜，其中，第1连接层的最低熔融粘度比第2连接层的最低熔融粘度高。
6.制备方法，其为权利要求1所述的各向异性导电膜的制备方法，其具有以下工序(A)~(C)：
工序(A)
在光聚合性树脂层上以单层排列导电粒子，使得导电粒子相对于第1连接层的埋入率为80%以上或1%以上且20%以下的工序；
工序(B)
通过对排列有导电粒子的光聚合性树脂层照射紫外线来进行光聚合反应，形成在表面固定有导电粒子的第1连接层的工序；和
工序(C)
在第1连接层的导电粒子一侧表面形成由热或光阳离子、阴离子或自由基聚合性树脂层构成的第2连接层的工序。
7.权利要求6所述的制备方法，其中，从光聚合性树脂层的排列有导电粒子的一侧进行工序(B)的紫外线照射。
8.制备方法，其为权利要求1所述的各向异性导电膜的制备方法，其具有以下工序(AA)~(DD)：
工序(AA)
在光聚合性树脂层上以单层排列导电粒子，使得导电粒子相对于第1连接层的埋入率为80%以上或1%以上且20%以下的工序；
工序(BB)
通过对排列有导电粒子的光聚合性树脂层照射紫外线来进行光聚合反应，形成在表面临时固定有导电粒子的临时第1连接层的工序；
工序(CC)
在临时第1连接层的导电粒子一侧表面形成由热阳离子、阴离子或自由基聚合性树脂层构成的第2连接层的工序；和
工序(DD)
通过从与第2连接层相反的一侧对临时第1连接层照射紫外线来进行光聚合反应，使临时第1连接层正式固化从而形成第1连接层的工序。
9.权利要求8所述的制备方法，其中，从光聚合性树脂层的排列有导电粒子的一侧进行工序(BB)的紫外线照射。
10.制备方法，其在权利要求6所述的制备方法中，在工序(C)之后具有以下工序(Z)：
工序(Z)
在第1连接层的导电粒子一侧的相反面形成由热或光阳离子、阴离子或自由基聚合性树脂层构成的第3连接层的工序。
11.制备方法，其在权利要求6所述的制备方法中，在工序(A)之前具有以下工序(a)：
工序(a)
在光聚合性树脂层的一面形成由热或光阳离子、阴离子或自由基聚合性树脂层构成的第3连接层的工序；
且在工序(A)中，在光聚合性树脂层的另一面以80%以上或1%以上且20%以下的埋入率单层排列导电粒子。
12.制备方法，其在权利要求8所述的制备方法中，在工序(DD)之后具有以下工序(Z)：
工序(Z)
在第1连接层的导电粒子一侧的相反面形成由热或光阳离子、阴离子或自由基聚合性树脂层构成的第3连接层的工序。
13.制备方法，其在权利要求8所述的制备方法中，在工序(AA)之前具有以下工序(a)：
工序(a)
在光聚合性树脂层的一面形成由热或光阳离子、阴离子或自由基聚合性树脂层构成的第3连接层的工序；
在工序(AA)中，在光聚合性树脂层的另一面以80%以上或1%以上且20%以下的埋入率单层排列导电粒子。
14.连接结构体，其是用权利要求1~5中任一项所述的各向异性导电膜将第1电子零件与第2电子零件各向异性导电连接而成的。
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TWI664262B (zh) 2019-07-01

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