CN101946371B - 连接膜、以及接合体及其制造方法 - Google Patents

连接膜、以及接合体及其制造方法 Download PDF

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Publication number
CN101946371B
CN101946371B CN2009801051493A CN200980105149A CN101946371B CN 101946371 B CN101946371 B CN 101946371B CN 2009801051493 A CN2009801051493 A CN 2009801051493A CN 200980105149 A CN200980105149 A CN 200980105149A CN 101946371 B CN101946371 B CN 101946371B
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layer
circuit element
film
organic resin
junctional membrane
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CN101946371A (zh
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阿久津恭志
石松朋之
宫内幸一
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Dexerials Corp
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Sony Chemical and Information Device Corp
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Abstract

本发明的目的在于提供一种在导电性粒子的补充效率及导通可靠性两方面均优异的连接膜，以及接合体及其制造方法。所述连接膜是将第1电路元件和第2电路元件以电形式连接在一起的连接膜，所述第2电路元件在面向第1电路元件的一面形成含有氮原子的膜；所述连接膜具备位于所述第1电路元件一侧的第1层和位于第2电路元件一侧的第2层，所述第1层含有阳离子系固化剂及环氧树脂；所述第2层含有自由基系固化剂、丙烯酸树脂及环氧化合物；所述第1和第2层中的任意一层为含有导电性粒子的含导电性粒子有机树脂层，所述第1和第2层中的另一层为没有导电性的绝缘性有机树脂层；所述含有导电性粒子有机树脂层的最低熔融粘度是所述绝缘性有机树脂层的最低熔融粘度的10倍以上。

Description

连接膜、以及接合体及其制造方法
技术领域
本发明涉及连接膜、以及接合体及其制造方法，尤其涉及一种能够将IC芯片、液晶显示器(LCD)中的液晶面板(LCD面板)等电路元件以电及机械的形式连接的连接膜，以及具有连接膜的接合体及其制造方法。 
背景技术
一直以来，作为连接电路元件的方法，常使用将分散有导电性粒子的热固性树脂涂布于分离膜上的带状的连接材料(例如，各向异性导电膜(ACF：Anisotropic Conductive Film))。 
这种各向异性导电膜(连接膜)，例如以将柔性电路板(FPC)或IC芯片的端子，与形成于LCD面板的玻璃基板上的ITO(Indium Tin Oxide)电极进行连接的情况为代表，用于粘结各种端子之间的同时以电形式进行连接的情况。 
作为所述连接膜，含有阳离子固化剂及环氧树脂的阳离子固化类连接膜已经实用化，并实现了低温固化性、降低被附着体的卷曲。 
但是，锍盐等的阳离子固化剂，因为其固化活性很高，因此即使是微量的杂质等也容易阻碍固化反应，出现固化不良等问题。 
尤其，因形成于IC芯片背面的聚酰亚胺制成的钝化膜所引起的固化不良经常发生。这是由于在通过阳离子固化类连接膜连接IC芯片时，在IC芯片上贴附阳离子固化类连接膜，固化反应一开始，产生的阳离子(H+)就会因钝化膜的聚酰亚胺原料而失活。产生的阳离子(H+)因钝化膜的聚酰亚胺原料而失活的原因，可以认为是由于阳离子(H+)与聚酰亚胺中的氮(N)原子发生反应而被捕获(发生R3N→R3N+H的反应，生成铵盐)。 
进而，即使在使用由粘结剂粘合聚酰亚胺和铜箔而成的TAB进行连接的情况，由于所述粘结剂由聚酰胺制成，因此会有引起阻碍固化的问题。 
此外，作为所述连接膜，含有自由基固化剂(有机过氧化物)及丙烯酸树脂的自由基固化类连接膜在线路板(PWB)侧的连接方面大多已经实用化，并实现了低温固化性。但是，自由基固化类连接膜，由于固化过程中不产生氢氧基，从而与具有极性的被附着体的相互作用减弱，出现粘结强度减弱、产生固化不良等问题。尤其，自由基固化类连接膜对LCD面板的玻璃面的贴附力差，在LCD面板侧易发生界面分离问题。 
虽然含有环氧树脂的自由基固化类连接膜也已经被公开(例如，专利文献1)，但是该情况对玻璃的贴附力也不够充分。 
因此，自由基固化类连接膜不适于LCD面板侧的连接，也缺少实际成绩。 
此外，作为连接膜的材料通常使用的橡胶类材料，易引起阻碍固化的问题。 
此外，也有提出将自由基固化剂(低温固化)和咪唑类固化剂(高温固化)混合成2元固化类的连接膜(例如，专利文献2)。但是，混合固化机理不同的成分而制成的连接膜，在固化时会发生层分离，因此易出现内部裂纹，连接可靠性差。并且，需要将固化分2阶段进行，不适合短时间连接。 
此外，也有提出将自由基固化剂和阳离子固化剂混合成2元固化类的连接膜(例如，专利文献3)、或在粘结剂中含有热固性组合物和光固化性组合物的连接膜(例如，专利文献4)、或具有含阳离子光固化剂层和含自由基光固化剂层的2层结构的连接膜(例如，专利文献5)，但是，这些均无法改善由形成于IC芯片背面的聚酰亚胺制成的钝化膜所引起的固化不良。因此，希望能开发出不产生由聚酰亚 胺制成的钝化膜所引起的固化不良的连接膜。 
此外，近年来在LCD、PDP、有机EL等显示装置中，从电传导性等角度来看，多在ITO等的基体上沉积Al、Mo、Cr、Ti、Cu、Ni等金属布线。这些金属布线缺乏对光的透过性，因此难以通过光固化将连接膜进行固化而连接电路元件。 
此外，已知在2层结构的连接膜中，使第1层与第2层具有粘度差，提高导电性粒子的补充效率的方法(例如，专利文献6)。但是，在该连接膜中，会出现第1层和第2层的边界附近的结合力减弱，导通可靠性降低的情况。 
此外，已知使用苯氧树脂等含羟基的树脂，提高粘结性的方法(例如，专利文献7)。但是，专利文献7公开的粘结剂，其并不是采用粘度不同的2层结构，与本发明相比，其结构及效果完全不同。 
现有技术文献 
专利文献1：日本特许第3587859号 
专利文献2：日本特开2007-262412号公报 
专利文献3：日本特开2006-127776号公报 
专利文献4：日本特开2005-235956号公报 
专利文献5：国际公开号00/084193号说明书 
专利文献6：日本特开平6-45024号公报 
专利文献7：国际公开号00/046315号说明书 
发明内容
发明要解决的技术问题 
本发明的课题为，解决上述现有的诸多问题，实现以下目的。即，本发明的目的在于提供一种在导电性粒子的补充效率和导通可靠性两方面均优异的连接膜，以及接合体及其制造方法。 
解决技术问题的技术手段 
作为解决上述问题的手段如下所述。即： 
<1>一种连接膜，其是将第1电路元件和第2电路元件以电形式连接的连接膜，所述第2电路元件在面向第1电路元件的一面形成含有氮原子的膜，其特征在于，所述连接膜具有位于所述第1电路元件侧的第1层和位于所述第2电路元件侧的第2层；所述第1层含有阳离子固化剂和环氧树脂；所述第2层含有自由基固化剂、丙烯酸树脂和环氧化合物；所述第1和第2层的任意一层为含有导电性粒子的含导电性粒子有机树脂层；所述第1和第2层的另一层为没有导电性的绝缘性有机树脂层；所述含导电性粒子有机树脂层的最低熔融粘度为所述绝缘性有机树脂层的最低熔融粘度的10倍以上。 
在该<1>中所述的连接膜中，因为在第1电路元件侧设置有含有阳离子固化剂及环氧树脂的第1层，在第2电路元件侧设置有含有自由基固化剂及丙烯酸树脂的第2层，所述第2电路元件在面向第1电路元件的一面形成含有氮原子的膜，因此能够提高对电路元件的粘结强度。 
并且，因为含导电性粒子有机树脂层的最低熔融粘度为绝缘性有机树脂层的最低熔融粘度的10倍以上，因此能够提高导电性粒子的补充效率。从而能够应对微间距(Fine Pitch)连接。 
在此，具有粘度差的2层结构的连接膜，在压接时各层的相互混合状态难以保持，有相互分离、层间的结合力变弱的倾向。对此，在本发明中，第2层中含有的环氧化合物与第1层中含有的环氧树脂发生反应，因此能够提高第1层和第2层之间的结合力。 
<2>上述<1>中所述的连接膜，其环氧化合物的分子量为900以上50000以下；环氧当量为450以上，5000以下。 
<3>上述<1>或<2>中所述的连接膜，其第2层含有含羟基丙烯酸酯。 
<4>一种接合体，其特征在于，其具备第1电路元件、第2电路元件以及上述<1>到<3>任意一项所述的连接膜，所述第2电路元件 在面向所述第1电路元件的一面形成含有氮原子的膜。 
该<4>中所述的接合体，因为在第1电路元件侧设置有含有阳离子固化剂及环氧树脂的第1层，在第2电路元件侧设置有含有自由基固化剂及丙烯酸树脂的第2层，所述第2电路元件在与所述第1电路元件相对的一面形成含有氮原子的膜，因此能够提高对电路元件的粘结强度。 
并且，在粘结时，第2层中含有的环氧化合物与第1层中含有的环氧树脂发生反应，因此能够提高第1层和第2层之间的结合力。 
进而，因为含导电性粒子有机树脂层的最低熔融粘度为绝缘性有机树脂层的最低熔融粘度的10倍以上，因此能够提高导电性粒子的补充效率。 
<5>接合体的制造方法，其特征在于，其包括通过上述<1>到<3>任意一项所述的连接膜，将第1及第2电路元件边加热边压接连接的连接工序。 
该<5>中所述的接合体的制造方法，在连接工序中，通过上述<1>到<3>任意一项所述的连接膜，第1及第2电路元件可以边加热边压接连接，因此能够制造在导电性粒子的补充效率及导通可靠性两方面均优异的连接膜。 
<6>上述<5>所述的接合体的制造方法，第1电路元件为LCD面板；第2电路元件为IC及TAB中的任一种，具有聚酰亚胺膜；在连接工序中，将第1层进行预贴附使其连接在所述LCD面板上，将所述聚酰亚胺进行预设置使其连接在第2层上，使用热压从所述第2电路元件侧进行压接连接。 
发明效果 
根据本发明，能够解决上述现有的诸多问题，实现上述目的，能够提供在导电性粒子的补充效率及导通可靠性两方面均优异的连接膜，以及接合体及其制造方法。 
附图说明
图1为本发明接合体的概略图。 
图2为本发明连接膜的概略图。 
图3为粘结强度的评价方法的概略图。 
标记说明： 
10：LCD面板(第1电路元件)、11：IC芯片(第2电路元件)、11a：端子、12：连接膜、12a：导电性粒子、20：分离层(separator)、21：含导电性粒子有机树脂层、22：绝缘性有机树脂层、100：接合体。 
具体实施方式
接合体 
本发明的接合体具有第1电路元件、第2电路元件及连接膜；进一步地，还具有根据需要进行适当选择的其他元件。 
例如，如图1所示，接合体100具有作为第1电路元件的LCD面板10、作为第2电路元件的IC芯片11以及连接膜12。通过导通IC芯片11的端子11a、连接膜12的导电性粒子12a和LCD面板10的端子(没有图示)，从而将LCD面板10和IC芯片11以电形式进行连接。 
<第1电路元件> 
所述第1电路元件没有特别限制，可以根据目的进行适当选择，例如玻璃制的LCD基板(LCD面板)、玻璃制的PDP基板(PDP面板)、玻璃制的有机EL基板(有机EL面板)等。 
并且，第1电路元件具有例如由铝制成的金属布线。像这样，如果第1电路元件具有铝等不透光的材料制成的布线，则难以使连接膜中含有的树脂进行光固化，因此连接膜中含有的树脂更优选为热固性树脂。 
<第2电路元件> 
所述第2电路元件，只要其是在面向第1电路元件的一面形成含有氮原子的膜，没有特别限制，可以根据目的进行适当选择，例如形成含有聚酰亚胺的钝化膜的IC芯片、形成含有Si3N4的钝化膜的IC芯片、搭载有IC芯片的TAB卷带等。 
并且，第2电路元件有由不透光的材料制成的情况。像这样，如果第2电路元件由不透光的材料制成，则难以使连接膜中含有的树脂进行光固化，因此，连接膜中含有的树脂更优选为热固性树脂。 
<连接膜> 
所述连接膜具有第1层和第2层，进一步地，还具有根据需要进行适当选择的其他层。并且，所述第1及第2层的任一层为含有导电性粒子的含导电性粒子有机树脂层，所述第1及第2层的另一层为没有导电性的绝缘性有机树脂层。 
例如，如图2所示，连接膜12具有分离层(separator)20、在分离层(separator)20上形成的作为第2层的绝缘性有机树脂层22、以及在绝缘性有机树脂层22上形成的作为第1层的含导电性粒子有机树脂层21。 
该连接膜12，例如将含导电性粒子有机树脂层21贴附到LC面板10(图1)侧。然后，剥离分离层(separator)20，从绝缘性有机树脂层22侧压接IC芯片11(图1)，形成接合体100(图1)。 
<<第1层>> 
所述第1层，其设置在所述第1电路元件侧，只要其含有阳离子固化剂及环氧树脂，没有特别限制，可以根据目的进行适当选择。 
所述第1层优选含有导电性粒子的含导电性粒子有机树脂层。这时，必须使下述第2层为没有导电性的绝缘性有机树脂层。 
<<<阳离子固化剂>>> 
所述阳离子固化剂，没有特别限制，可以根据目的进行适当选择，例如可以是锍盐、鎓盐等，其中，优选的是芳香族锍盐。 
<<<环氧树脂>>> 
所述环氧树脂，没有特别限制，可以根据目的进行适当选择，例如可以是双酚A型环氧树脂、双酚F型环氧树脂、线型酚醛环氧树脂、或它们的改性环氧树脂等热固性环氧树脂。其可以单独使用1种，也可以2种以上并用。 
<<<导电性粒子>>> 
所述导电性粒子，没有特别限制，可以使用现有的用于各向异性导电粘结剂(连接膜)的导电性粒子，例如，可以使用粒子直径为1～50μm的金属粒子或金属包覆树脂粒子。 
所述金属粒子，例如有镍、钴、铜等。为防止其表面氧化，还可以使用表面涂覆了金、钯的粒子。进一步地，还可以使用表面设有金属突起或有机物制的绝缘皮膜的粒子。 
所述金属包覆树脂粒子，例如用镍、钴、铜等的1种以上进行电镀的圆球状粒子。同样地，还可以使用在最外表面涂覆了金、钯的粒子。进一步地，还可以使用表面设有金属突起或有机物制的绝缘皮膜的粒子。 
<<第2层>> 
所述第2层设置在所述第2电路元件侧，只要其含有自由基固化剂、丙烯酸树脂及环氧化合物，没有特别限制，可以根据目的进行适当选择。 
所述第2层，从对极性电路元件的贴附性的角度来看，优选为含有含羟基丙烯酸酯。 
并且，所述第2层优选为没有导电性的绝缘性有机树脂层，但是也可以是含有所述导电性粒子的含导电性粒子有机树脂层。这时，必须使第1层为绝缘性有机树脂层。 
<<<自由基固化剂>>> 
所述自由基固化剂没有特别限制，可以根据目的进行适当选择， 例如可以是有机过氧化物。 
<<<丙烯酸树脂>>> 
所述丙烯酸树脂没有特别限制，可以根据目的进行适当选择，例如甲基丙烯酸酯、乙基丙烯酸酯、异丙基丙烯酸酯、异丁基丙烯酸酯、环氧基丙烯酸酯、乙二醇二丙烯酸酯、二乙二醇二丙烯酸酯、三羟甲基丙烷三丙烯酸酯、二羟甲基三环癸烷二丙烯酸酯、四亚甲基二醇四丙烯酸酯、2-羟基-1，3-二丙烯酰氧基丙烷、2，2-双[4-(丙烯酰氧基甲氧基)苯基]丙烷、2，2-双[4-(丙烯酰氧基乙氧基)苯基]丙烷、二环戊烯基丙烯酸酯、三环癸基丙烯酸酯、三(丙烯酰氧基乙基)异氰尿酸酯、聚氨酯丙烯酸酯等丙烯酸树脂。其可以单独使用1种，也可以2种以上并用。 
并且，可以将所述丙烯酸酯制成丙烯酸甲酯，其可以单独使用1种，也可以2种以上并用。 
<<<环氧化合物>>> 
所述环氧化合物没有特别限制，可以根据目的进行适当选择，例如与所述环氧树脂相同。 
第2层中含有的环氧化合物，在压接时，与第1层中含有的环氧树脂反应。因此，在第2层中的第1层侧的部分，形成同时发生由丙烯酸树脂引起的自由基固化和由环氧化合物引起的阳离子固化这两种固化的混合层，通过该混合层，能够显著提高第1层和第2层间的结合力。 
所述环氧化合物，其分子量优选为900以上50000以下，更优选的是5000以上40000以下，特别优选的是10000以上30000以下。 
所述环氧化合物的分子量小于900时，未反应的环氧化合物没有内包含在固化了的第2层的网格(network)中，因此会出现第2层侧的粘结强度降低的情况。所述环氧化合物的分子量超过50000时，则粘度增加且粒子捕捉率降低。 
所述环氧化合物，其环氧当量优选为450以上5000以下，更优选的是1000以上4500以下，特别优选的是2000以上4000以下。 
所述环氧化合物的环氧当量小于450时，由于是分子量小的化合物，因此没有内包含在第2层的网格内，并且，由于残留有未反应的环氧基还会引起膜寿命的降低；当超过5000时，则环氧基的数量过少，与第1层的环氧树脂的反应也减少，不能够充分提高层间的结合力。 
<<<含羟基丙烯酸酯>>> 
所述含羟基丙烯酸酯，只要其分子内具有1个以上的羟基，没有特别限制，可以根据目的进行适当选择。 
所述含羟基丙烯酸酯的酸值，优选为1mgKOH/g以上360mgKOH/g以下，更优选的是10mgKOH/g以上300mgKOH/g以下，特别优选的是50mgKOH/g以上250mgKOH/g以下。 
含羟基丙烯酸酯的酸值小于1mgKOH/g时，粘结强度会降低；超过360mgKOH/g时，可能会腐蚀电极而不优选。 
<<最低熔融粘度比>> 
所述含导电性粒子有机树脂层的最低熔融粘度优选为所述绝缘性有机树脂层的最低熔融粘度的10倍以上，更优选的是13倍以上。 
所述含导电性粒子有机树脂层的最低熔融粘度小于所述绝缘性有机树脂层的最低熔融粘度10倍时，不能充分提高导电性粒子的补充效率。 
并且，从导电性的角度来看，所述含导电性粒子有机树脂层的最低熔融粘度优选在所述绝缘性有机树脂层的最低熔融粘度的1000倍以下。 
<<其他层>> 
所述其他层没有特别限制，可以根据目的进行适当选择，例如可以是分离层。 
所述分离层，关于其形状、结构、大小、厚度、材料(材质)等没有特别限制，可以根据目的进行适当选择，但是优选的是分离性良好或耐热性高的分离层，例如，合适的有涂布有硅树脂等分离剂的透明的分离PET(聚对苯二甲酸乙二醇酯)膜等。此外，还可以使用PTFE(聚四氟乙烯)膜。 
<其他成分> 
所述其他成分没有特别限制，可以根据目的进行适当选择，例如，可以是硅烷偶联剂、表面活性剂等。 
接合体的制造方法 
本发明的接合体的制造方法至少包括连接工序，还包括根据需要进行适当选择的其他工序。 
<连接工序> 
所述连接工序是通过本发明的连接膜，将第1及第2电路元件边加热边压接连接的工序。 
所述加热由总热量决定，在连接时间10秒以下完成连接的情况下，在加热温度120℃～220℃下进行。 
所述压接根据第2电路元件的种类不同而不同，当为TAB卷带时压力为2～6MPa；当为IC芯片时压力为20～120MPa，分别进行3～10秒时间。 
并且，还可以通过超声波和热进行连接。 
在此，当第1电路元件为LCD面板、第2电路元件为IC芯片及TAB的任一种且具有聚酰亚胺膜时，在连接工序中，优选的是，将第1层进行预贴附使其连接在LCD面板上，将聚酰亚胺膜进行预设置使其连接在第2层上，然后使用热压从第2电路元件侧进行压接连接。 
如上所述由于从第2电路元件侧进行压接，因此第2电路元件与热压机相接触，由于第2层的树脂被加热，从而使其熔融粘度降低而 易于流动，因此能够有效地捕捉第1层的导电性粒子。 
下面，列举实施例及比较例对本发明进行更具体的说明，但本发明并不限于下述实施例。 
制造例1：阳离子固化类电极粘结用膜C1 
将导电性粒子(商品名：AUL704、积水化学工业公司制)分散至由50份苯氧树脂(商品名：YP-50、东都化成公司制)、35份环氧树脂(商品名：jER828、Japan Epoxy Resins(ジヤパンエポキシレジン)公司制)、1份硅烷偶联剂(商品名：KBM-403，信越硅树脂公司制)、4份固化剂(商品名：SI-60L、三新化学工业公司制)、及10份二氧化硅微粒(商品名：AEROSIL RY200、日本aerosil公司制)制成的粘结剂中，直至粒子密度为30000个/mm2，制成厚度10μm的阳离子固化类电极粘结用膜C1。 
具体地说，首先，将上述原料制成含有固形物50％的乙酸乙酯、甲苯混合溶液。然后，将该混合溶液涂布到厚度50μm的PET膜上，然后在80℃的烘箱中干燥5分钟，得到阳离子固化类电极粘结用膜C1。 
并且，使用流变仪(商品名：RS 150、HAAKE公司制)测定最低熔融粘度。测定在升温速度10℃/min的条件下进行。 
制造例2：阳离子固化类电极粘结用膜C2 
除了在制造例1中将苯氧树脂(商品名：YP-50、东都化成公司制)的添加量从50份变为60份、不添加二氧化硅微粒(商品名：AEROSIL RY200、日本aerosil公司制)以外，与制造例1相同，制成阳离子固化类电极粘结用膜C2，并测定了最低熔融粘度。 
制造例3：阳离子固化类电极粘结用膜C3 
除了在制造例1中将环氧树脂(商品名：jER828、Japan Epoxy Resins公司制)的添加量从35份变为30份、添加5份丙烯酸树脂(商品名：EB600、daicel-cytec公司制)以外，与制造例1相同，制成阳 离子固化类电极粘结用膜C3，并测定了最低熔融粘度。 
制造例4：阳离子固化类电极粘结用膜C4 
除了在制造例1中不添加二氧化硅微粒(商品名：AEROSIL RY200、日本aerosil公司制)以外，与制造例1相同，制成阳离子类电极粘结用膜C4，并测定了最低熔融粘度。 
阳离子固化类电极粘结用膜C1～C4的组成及最低熔融粘度，如下表1所示。 
表1 
Figure BPA00001201197700131
制造例5：自由基固化类电极粘结用膜R1 
制成由50份苯氧树脂(商品名：YP-50、东都化成公司制)、35份丙烯酸树脂(商品名：EB-600、daicel-cytec公司制)、10份环氧化合物(商品名：jER1001、Japan Epoxy Resins公司制)、1份硅烷偶联剂(商品名：KBM-503，信越硅树脂公司制)、及4份固化剂(NYPER BW、日本油脂公司制)制成的厚度10μm的自由基固化类电极粘结用膜R1。 
具体地说，首先，将上述原料制成含有固形物50％的乙酸乙酯、甲苯混合溶液。然后，将该混合溶液涂布到厚度50μm的PET膜上， 然后在80℃的烘箱中干燥5分钟，得到自由基固化类电极粘结用膜R1。 
并且，使用流变仪(商品名：RS 150、HAAKE公司制)测定最低熔融粘度。测定在升温速度10℃/min的条件下进行。 
制造例6：自由基固化类电极粘结用膜R2 
除了在制造例5中加入10份环氧化合物(商品名：jER1010、Japan Epoxy Resins公司制)，来代替10份环氧化合物(商品名：jER1001、Japan Epoxy Resins公司制)之外，与制造例5相同，制成自由基固化类电极粘结用膜R2，并测定了最低熔融粘度。 
制造例7：自由基固化类电极粘结用膜R3 
除了在制造例5中加入10份环氧化合物(商品名：jER4110、Japan Epoxy Resins公司制)，来代替10份环氧化合物(商品名：jER1001、Japan Epoxy Resins公司制)之外，与制造例5相同，制成自由基固化类电极粘结用膜R3，并测定了最低熔融粘度。 
制造例8：自由基固化类电极粘结用膜R4 
除了在制造例7中将丙烯酸树脂(商品名：EB-600、daicel-cytec公司制)的添加量从35份变为30份、并加入5份含羟基丙烯酸酯(商品名：Nk-ester CB-1、新中村化学公司制)以外，与制造例7相同，制成自由基固化类电极粘结用膜R4，并测定了最低熔融粘度。 
制造例9：自由基固化类电极粘结用膜R5 
除了在制造例5中加入10份环氧化合物(商品名：jER828、Japan Epoxy Resins公司制)，来代替10份环氧化合物(商品名：jER1001、Japan Epoxy Resins公司制)以外，与制造例5相同，制成自由基固化类电极粘结用膜R5，并测定了最低熔融粘度。 
制造例10：自由基固化类电极粘结用膜R6 
除了在制造例5中加入10份环氧化合物(商品名：YR55、东都化成公司制)，来代替10份环氧化合物(商品名：jER1001、Japan Epoxy  Resins公司制)以外，与制造例5相同，制成了自由基固化类电极粘结用R6，并测定了最低熔融粘度。 
制造例11：自由基固化类电极粘结用膜R7 
除了在制造例5中将苯氧树脂(商品名：YP-50、东都化成公司制)的添加量从50份变为60份、不加入10份环氧化合物(商品名：jER1001、Japan Epoxy Resins公司制)以外，与制造例5相同，制成自由基固化类电极粘结用膜R7，并测定了最低熔融粘度。 
制造例12：自由基固化类电极粘结用膜R8 
除了在制造例8中将丙烯酸树脂(商品名：EB-600、daicel-cytec公司制)的添加量从30份变为35份、将含羟基丙烯酸酯(商品名：Nk-ester CB-1、新中村化学公司制)的添加量从5份变为10份、不加入10份环氧化合物(商品名：jER4110、Japan Epoxy Resins公司制)以外，与制造例8相同，制成自由基固化类电极粘结用膜R8，并测定了最低熔融粘度。 
并且，含羟基丙烯酸酯(商品名：Nk-ester CB-1、新中村化学公司制)的酸值为197mgKOH/g。 
制造例13：自由基固化类电极粘结用膜R9 
除了在制造例12中加入10份含羟基丙烯酸酯(商品名：β-CEA、daicel-cytec公司制)，来代替10份含羟基丙烯酸酯(商品名：Nk-ester CB-1、新中村化学公司制)以外，与制造例12相同，制成自由基固化类电极粘结用膜R9，并测定了最低熔融粘度。 
并且，含羟基丙烯酸酯(商品名：β-CEA、daicel-cytec公司制)的酸值为365mgKOH/g。 
制造例14：自由基固化类电极粘结用膜R10 
除了在制造例12中将苯氧树脂(商品名：YP-50、东都化成公司制)的添加量从50份变为55份、并加入5份磷酸丙烯酸酯(商品名：LIGHT-ESTER P-1M、共荣社化学公司制)来代替10份含羟基丙烯 酸酯(商品名：Nk-ester CB-1、新中村化学公司制)以外，与制造例12相同，制成自由基固化类电极粘结用膜R10，并测定了最低熔融粘度。 
制造例15：自由基固化类电极粘结用膜R11 
除了在制造例12中加入10份聚氨酯丙烯酸酯(商品名：U-2PPA、新中村化学公司制)来代替10份含羟基丙烯酸酯(商品名：Nk-ester CB-1、新中村化学公司制)以外，与制造例12相同，制成自由基固化类电极粘结用膜R11，并测定了最低熔融粘度。 
自由基固化类电极粘结用膜R1～R11的组成、及最低熔融粘度如下表2所示。并且，部分材料的环氧当量及分子量如下表3所示。 
Figure BPA00001201197700171
表3 
    环氧当量   分子量
  YP55   10000～20000   50000～60000
  jER828   184～194   370
  jER1001   450～500   900
  jER1010   3000～5000   5500
  jER4110   3500～4000   约5万
  EB-600   -   600
实施例1 
将制造例1制成的阳离子固化类电极粘结用膜C1和制造例5制成的自由基固化类电极粘结用膜R1层压制成2层结构的电极粘结用膜，通过该2层结构的电极粘结用膜，将IC芯片(尺寸：1.8mm×20.0mm；厚度：0.5mm；金凸块尺寸：30μm×85μm；凸块高度：15μm；凸块间距：50μm)和与IC芯片的花纹相对应的铝花纹玻璃基板(商品名：1737F、康宁(Corning)公司制，尺寸：50mm×30mm×0.5mm)连接起来，制成接合体。 
并且，在IC芯片侧贴有自由基固化类电极粘结用膜R1，在铝花纹玻璃基板侧贴有阳离子固化类电极粘结用膜C1。此外，作为IC芯片的钝化膜可以使用聚酰亚胺。通过在180℃、80MPa、5秒条件下压IC芯片进行IC芯片和铝花纹玻璃基板之间的连接。 
实施例2 
除了在实施例1中用制造例6制成的自由基固化类电极粘结用膜R2代替自由基固化类电极粘结用膜R1以外，与实施例1相同，制成接合体。 
实施例3 
除了在实施例1中用制造例7制成的自由基固化类电极粘结用膜R3代替自由基固化类电极粘结用膜R1以外，与实施例1相同，制成接合体。 
实施例4 
除了在实施例1中用制造例8制成的自由基固化类电极粘结用膜R4代替自由基固化类电极粘结用膜R1以外，与实施例1相同，制成接合体。 
实施例5 
除了在实施例1中用制造例9制成的自由基固化类电极粘结用膜R5代替自由基固化类电极粘结用膜R1以外，与实施例1相同，制成接合体。 
实施例6 
除了在实施例1中用制造例10制成的自由基固化类电极粘结用膜R6代替自由基固化类电极粘结用膜R1以外，与实施例1相同，制成接合体。 
比较例1 
除了在实施例1中用制造例2制成的阳离子固化类电极粘结用膜C2代替阳离子固化类电极粘结用膜C1、用制造例11制成的自由基固化类电极粘结用膜R7代替自由基固化类电极粘结用膜R1以外，与实施例1相同，制成接合体。 
比较例2 
除了在比较例1中用制造例3制成的阳离子固化类电极粘结用膜C3代替阳离子固化类电极粘结用膜C2以外，与比较例1相同，制成接合体。 
比较例3 
除了在比较例1中用制造例6制成的自由基固化类电极粘结用膜R2代替自由基固化类电极粘结用膜R7以外，与比较例1相同，制成接合体。 
接合体的评价 
对上述实施例1～6、比较例1～3制成的接合体，用如下方法进行评价。 
<最低熔融粘度比> 
计算得到含导电性粒子有机树脂层(ACF)的最低熔融粘度相对于绝缘性有机树脂层(NCF)的最低熔融粘度的比。 
并且，在上述实施例、比较例中，阳离子固化类电极粘结用膜为含导电性粒子有机树脂层；自由基固化类电极粘结用膜为绝缘性有机树脂层。 
<粒子补充效率的评价> 
在各接合体中，根据下述公式计算得到接合前凸块上的粒子个数(接合前粒子数)。 
接合前粒子数＝导电性粒子的粒子密度(个/mm2)×凸块的面积(mm2) 
此外，用金相显微镜进行计数从而测定了接合后凸块上的导电性粒子个数(接合后粒子数) 
并且，根据下述公式计算得到导电性粒子的补充效率(粒子补充效率)。 
粒子补充效率＝(接合后粒子数/接合前粒子数)×100％ 
<芯片剪切强度的测定> 
对制成的各接合体，用芯片剪切力测试机(商品名：Daga2400，Dage公司制)进行芯片剪切强度的测定。 
<热循环试验> 
将各接合体按照-40℃下30分钟、100℃下30分钟的条件进行热循环，每隔100循环取出各接合体测定连接电阻。以连接电阻超过50Ω的循环数作为出现不良的循环数。 
<粘结强度> 
将0.7mm厚的玻璃上贴有ITO膜的ITO玻璃和间距50μm的FPC(柔性印刷布线板)，通过与实施例1～6、比较例1～3相同的阳离子 固化类电极粘结用膜及自由基固化类电极粘结用膜，在180℃、4MPa、5秒钟的条件下，加热、加压压接使其接合。 
用万能拉力试验机(Tensilon)(orientec(オリエンテツク)公司制)，按图3所示方法测定该接合体的粘结强度。在图3中，测定方法为90°Peel；测定速度为50mm/min；图3中的箭头方向为Y方向；30表示玻璃；31表示FPC或TAB；32表示ACF。 
各接合体的评价结果如下表4所示。 
表4 
Figure BPA00001201197700211
从表4可知，具备本发明结构的实施例1～6的接合体在导电性粒子的补充效率高的同时，结合强度高，导通可靠性也优异。 
与此相反，自由基固化类电极粘结用膜(第2层)不含有环氧化合物的比较例1、2的接合体，在芯片剪切强度低的同时，出现不良的循环数小，不能得到充分的粘结强度。因此，可能会损害导通可靠性。 
并且，能够看出在含导电性粒子有机树脂层的最低熔融粘度小于 绝缘性有机树脂层的最低熔融粘度10倍的比较例1、3的接合体中，粒子补充效率低、难以应对微间距连接。 
比较例1因为在阳离子固化类电极粘结用膜C2(ACF)的最低熔融粘度(500Pa·s)和自由基固化类电极粘结用膜R7(NCF)的最低熔融粘度(500Pa·s)之间没有粘度差，因此粒子补充效率低，无法应对微间距连接。但是，因为在阳离子固化类电极粘结用膜C2(ACF)的最低熔融粘度(500Pa·s)和自由基固化类电极粘结用膜R7(NCF)的最低熔融粘度(500Pa·s)之间没有粘度差，易形成混合层，提高粘结强度。 
还可知比较例2的接合体，在阳离子固化类电极粘结用膜(第1层)中加入了丙烯酸树脂，但粘结强度低，为了解决本发明的问题，自由基固化类电极粘结用膜(第2层)中必须含有环氧树脂。 
将实施例4与实施例1进行比较可知，加入了含羟基丙烯酸酯的实施例4中，粘结强度进一步提高。 
此外，还可知在环氧化合物的分子量小的实施例5及环氧当量大的实施例6中，虽然可以认为其对现有技术进行了改善，但是与实施例1～4相比，芯片剪切强度低、出现不良的循环数也小。 
参考例1 
<接合体的评价> 
除了在比较例1中，用制造例12制成的自由基固化类电极粘结用膜R8代替自由基固化类电极粘结用膜R7以外，与比较例1相同，制成接合体。 
在测定该接合体的导通电阻的同时，用与上述实施例、比较例相同的方法测定粘结强度。 
<腐蚀性评价> 
在1mm厚的玻璃上具有布线间距15μm的ITO布线的梳齿型评价元件上，贴附自由基固化类电极粘结用膜R8，作为用于评价腐蚀 性的样本。 
在40℃、90％RH的环境下，外加40V直流电压到上述用于评价腐蚀性的样本的布线间，根据出现腐蚀的时间按以下3个阶段进行评价。 
○：即使超过48小时也不出现腐蚀。 
△：在24～48小时出现腐蚀。 
×：在经过24小时之前出现腐蚀。 
参考例2 
除了在参考例1中用制造例4制成的阳离子固化类电极粘结用膜C4代替阳离子固化类电极粘结用膜C2、用制造例13制成的自由基固化类电极粘结用膜R9代替自由基固化类电极粘结用膜R8以外，与参考例1相同，实施对导通电阻、粘结强度、腐蚀性的评价。 
参考例3 
除了在参考例1中用制造例11制成的自由基固化类电极粘结用膜R7代替自由基固化类电极粘结用膜R8以外，与参考例1相同，实施对导通电阻、粘结强度、腐蚀性的评价。 
参考例4 
除了在参考例3中用制造例14制成的自由基固化类电极粘结用膜R10代替自由基固化类电极粘结用膜R7以外，与参考例3相同，实施对导通电阻、粘结强度、腐蚀性的评价。 
参考例5 
除了在参考例2中用制造例15制成的自由基固化类电极粘结用膜R11代替自由基固化类电极粘结用膜R9以外，与参考例2相同，实施对导通电阻、粘结强度、腐蚀性的评价。 
参考例1～5的评价结果如下表5所示。 
表5 
Figure DEST_PATH_GPA00001201197000041
在参考例1、2中，由于使用含有含羟基丙烯酸酯的自由基固化类电极粘结用膜，因此显示出很好的粘结强度和低的导通电阻。尤其是，酸值低的参考例1腐蚀性低，优选作为连接膜使用。 
相对于此，在参考例3中，因为在自由基固化类电极板中没有使用含羟基丙烯酸酯，因此不能获得很好的粘结强度。 
此外，在参考例4、5中，由于使用了磷酸丙烯酸酯、聚氨酯丙烯酸酯，因此粘结强度提高，但其阻碍阳离子固化类电极板的反应，引起未固化状态，因此导通电阻增加。 
产业上的应用可能性 
本发明的连接膜、以及接合体及其制造方法，作为在导电性粒子的补充效率及导通可靠性两方面均优异的连接膜、以及接合体及其制造方法，能够适合于应用。 

Claims (6)

1.一种连接膜，其是将第1电路元件和第2电路元件以电形式连接的连接膜，所述第2电路元件在面向第1电路元件的一面形成含有氮原子的膜，其特征在于，
所述连接膜具有位于所述第1电路元件侧的第1层和位于所述第2电路元件侧的第2层；
所述第1层含有阳离子固化剂和环氧树脂；所述第2层含有自由基固化剂、丙烯酸树脂和环氧化合物；
所述第1和第2层的任意一层为含导电性粒子有机树脂层；
所述第1和第2层的另一层为没有导电性的绝缘性有机树脂层；
所述含导电性粒子有机树脂层的最低熔融粘度为所述绝缘性有机树脂层的最低熔融粘度的10倍以上。
2.根据权利要求1所述的连接膜，其特征在于，环氧化合物的分子量为900以上，50000以下；环氧当量为450以上、5000以下。
3.根据权利要求1所述的连接膜，其特征在于，第2层含有含羟基丙烯酸酯。
4.一种接合体，其特征在于，其具备第1电路元件、第2电路元件和连接膜；所述第2电路元件在面向所述第1电路元件的一面形成含有氮原子的膜；所述连接膜以电形式连接所述第1电路元件和所述第2电路元件，其具备位于所述第1电路元件侧的第1层和位于第2电路元件侧的第2层；所述第1层含有阳离子固化剂和环氧树脂，所述第2层含有自由基固化剂、丙烯酸树脂和环氧化合物，所述第1和第2层的任一层为含导电性粒子有机树脂层，所述第1和第2层的另一层为没有导电性的绝缘性有机树脂层，所述含导电性粒子有机树脂层的最低熔融粘度为所述绝缘性有机树脂层的最低熔融粘度的10倍以上。
5.一种接合体的制造方法，其特征在于，其包括通过连接膜，将第1及第2电路元件边加热边压接连接的连接工序；所述连接膜以电形式连接所述第1电路元件和所述第2电路元件，所述第2电路元件在面向所述第1电路元件的一面形成含有氮原子的膜，所述连接膜具备位于所述第1电路元件侧的第1层和位于第2电路元件侧的第2层；所述第1层含有阳离子固化剂和环氧树脂，所述第2层含有自由基固化剂、丙烯酸树脂和环氧化合物，所述第1和第2层的任一层为含导电性粒子有机树脂层，所述第1和第2层的另一层为没有导电性的绝缘性有机树脂层，所述含导电性粒子有机树脂层的最低熔融粘度为所述绝缘性有机树脂层的最低熔融粘度的10倍以上。
6.根据权利要求5所述的接合体的制造方法，其特征在于，第1电路元件为LCD面板；第2电路元件为IC和TAB中的任一种，具有聚酰亚胺膜；
在连接工序中，将第1层进行预贴附使其连接在所述LCD面板上，将所述聚酰亚胺膜进行预设置使其连接在第2层上，使用热压从所述第2电路元件侧进行压接连接。
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