CN104540869A - 电子部件用固化性组合物、连接结构体及连接结构体的制造方法 - Google Patents

电子部件用固化性组合物、连接结构体及连接结构体的制造方法 Download PDF

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Publication number
CN104540869A
CN104540869A CN201480002105.9A CN201480002105A CN104540869A CN 104540869 A CN104540869 A CN 104540869A CN 201480002105 A CN201480002105 A CN 201480002105A CN 104540869 A CN104540869 A CN 104540869A
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electrode
mentioned
electronic component
solidification compound
electroconductive particle
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CN104540869B (zh
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石泽英亮
久保田敬士
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Sekisui Chemical Co Ltd
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Sekisui Chemical Co Ltd
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    • H01L24/81—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a bump connector
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Abstract

提供一种电子部件用固化性组合物，其可以快速地进行固化，并且，在连接有铜电极的情况下，也可以提高导通性。本发明所述的电子部件用固化性组合物用于铜电极的连接。本发明所述的电子部件用固化性组合物含有热固化性化合物、潜伏性固化剂、和具有芳香族骨架的咪唑化合物。

Description

电子部件用固化性组合物、连接结构体及连接结构体的制造方法
技术领域
本发明涉及一种用于铜电极的连接的电子部件用固化性组合物。本发明还涉及一种使用有上述电子部件用固化性组合物的连接结构体及连接结构体的制造方法。
背景技术
热固化性树脂组合物广泛地用于电子、建筑及车辆等各种用途。另外，为了对各种连接对象部件的电极间进行电连接，有时在上述热固化性树脂组合物中配合导电性粒子。含有导电性粒子的热固化性树脂组合物被称为各向异性导电材料。
上述各向异性导电材料用于IC芯片与挠性印刷电路基板之间的连接、及IC芯片与具有ITO电极的电路基板之间的连接等。例如，将各向异性导电材料配置在IC芯片的电极和电路基板的电极之间后，通过进行加热及加压，可以利用导电性粒子对这些电极进行电连接。
作为上述热固化性树脂组合物的一例，下述的专利文献1中公开有一种组合物，其含有(a)环氧树脂和(b)固化促进剂。专利文献1的实施例中，使用咪唑类作为上述(b)固化促进剂。专利文献1中，提出了将上述组合物用作半导体密封用膜状粘接剂。
现有技术文献
专利文献
专利文献1：日本特开2009-256588号公报
发明内容
发明要解决的问题
近年来，为了有效地对电子部件的电极间等进行连接，要求缩短组合物的固化需要的加热时间。通过缩短加热时间，可以抑制得到的电子部件的热劣化。
专利文献1中记载有：在半导体装置中密封时使用组合物的情况下，操作性优异，在加热至300℃以上的情况下，也可以充分地抑制空隙的产生，同时，可以制造连接可靠性和绝缘可靠性充分优异的半导体装置。但是，有时专利文献1中记载的那样的现有固化性组合物未充分、快速地热固化。另外，对铜电极的表面进行通常的耐热预焊剂处理。为了对这种铜电极进行电连接，在使用现有的固化性组合物的情况下，有时导通性变低。
本发明的目的在于，提供一种电子部件用固化性组合物，以及提供一种使用有该电子部件用固化性组合物的连接结构体及连接结构体的制造方法，所述电子部件用固化性组合物可以快速地固化，即使在进一步连接铜电极的情况下，也可以提高导通性。
解决问题的方法
根据本发明的宽广方面，提供一种电子部件用固化性组合物，其用于铜电极的连接，所述固化性组合物含有热固化性化合物、潜伏性固化剂、具有芳香族骨架的咪唑化合物。
在本发明所述电子部件用固化性组合物的某一特定方面，所述潜伏性固化剂为微胶囊型咪唑固化剂。
在本发明所述电子部件用固化性组合物的某一特定方面，该电子部件用固化性组合物含有导电性粒子。
在本发明所述电子部件用固化性组合物的某一特定方面，所述导电性粒子是导电性的外表面为焊料的导电性粒子。
在本发明所述电子部件用固化性组合物的某一特定方面，所述固化性组合物为糊。
根据本发明的宽广方面，提供一种连接结构体，其具备：表面具有第1电极的第1连接对象部件、表面具有第2电极的第2连接对象部件、将所述第1连接对象部件和所述第2连接对象部件连接起来的连接部，所述连接部通过使上述的电子部件用固化性组合物固化而形成，所述第1电极及所述第2电极中的至少之一为铜电极，将所述第1电极和所述第2电极电连接。
在本发明所述连接结构体的某一特定方面，所述电子部件用固化性组合物含有导电性粒子，所述第1电极和所述第2电极通过所述导电性粒子进行电连接。
根据本发明的宽广方面，提供一种连接结构体的制造方法，其包含：在表面具有第1电极的第1连接对象部件和在表面具有第2电极的第2连接对象部件之间设置上所述的电子部件用固化性组合物的工序；通过使所述电子部件用固化性组合物固化，形成将所述第1连接对象部件和所述第2连接对象部件连接起来的连接部，得到所述第1电极和所述第2电极实现了电连接的连接结构体的工序，所述第1电极及所述第2电极中的至少之一为铜电极。
在本发明所述连接结构体的制造方法的某一特定方面，所述电子部件用固化性组合物含有导电性粒子，得到所述第1电极和所述第2电极通过所述导电性粒子进行了电连接的连接结构体。
发明的效果
由于本发明所述的电子部件用固化性组合物含有热固化性化合物、潜伏性固化剂和具有芳香族骨架的咪唑化合物，因此，可以快速地固化。进而，在使用本发明所述的电子部件用固化性组合物连接铜电极的情况下，可以提高导通性。
附图说明
图1是示意性地示出使用有本发明的一实施方式中涉及的电子部件用固化性组合物的连接结构体的剖面图；
图2是示意性地示出图1所示的连接结构体的变形例的剖面图；
图3是示意性地示出可以在本发明的一个实施方式中涉及的电子部件用固化性组合物中使用的导电性粒子的剖面图；
图4是表示导电性粒子的变形例的剖面图；
图5是表示导电性粒子的其它变形例的剖面图。
标记说明
1、11…连接结构体
2，12…第1连接对象部件
2a，12a…第1电极
3、13…连接部
4、14…第2连接对象部件
4a、14a…第2电极
5…导电性粒子
21…导电性粒子
21a…表面
22…树脂粒子
22a…表面
23…导电层
24…第1导电层
24a…表面
25…焊料层
25a…熔融的焊料层部分
31…导电性粒子
32…焊料层
41…焊料粒子
具体实施方式
下面，对本发明的详细情况进行说明。
(电子部件用固化性组合物)
本发明所述的电子部件用固化性组合物(以下，有时简称为固化性组合物)含有热固化性化合物、潜伏性固化剂和具有芳香族骨架的咪唑化合物。上述固化性组合物用于铜电极的连接。上述固化性组合物用于电子部件。上述固化性组合物优选用于电子部件的连接。优选上述固化性组合物为电子部件用连接材料。优选上述固化性组合物为电子部件用电路连接材料。
本发明所述的电子部件用固化性组合物具有上述的组成，因此，能够快速地固化。而且，本发明所述的电子部件用固化性组合物具有上述组成，因此，在对铜电极进行连接时，可以提高导通性。
另外，对铜电极的表面进行通常的耐热预焊剂处理。在本发明中，即使对这种进行了耐热塑料处理的铜电极进行连接，也可以提高导通性。上述具有芳香族骨架的咪唑化合物大大有助于铜电极导通性的提高。另一方面，在单独使用具有芳香族骨架的咪唑化合物而不使用潜伏性固化剂的情况下，不能使上述热固化性化合物充分地固化，或组合物的保存稳定性变低，或组合物的固化速度变慢。在本发明中，主要利用上述潜伏性固化剂使上述热固化性化合物快速地固化，主要利用上述具有芳香族骨架的咪唑化合物提高铜电极的导通性。因此，在本发明中，在铜电极的连接中，对潜伏性固化剂和具有芳香族骨架的咪唑化合物进行组合具有巨大意义。
而且，在本发明中，可以提高固化物的耐湿热性。另外，也可以提高固化物的耐热冲击性。
以下，对本发明所述的电子部件用固化性组合物中所含的各成分的详细情况进行说明。
[热固化性化合物]
作为上述热固化性化合物，可列举：氧杂环丁烷化合物、环氧化合物、环硫化物化合物、(甲基)丙烯酸化合物、苯酚化合物、氨基化合物、不饱和聚酯化合物、聚氨酯化合物、硅酮化合物及聚酰亚胺化合物等。上述热固化性化合物可以单独使用1种，也可以组合使用2种以上。
环氧化合物具有固化物的粘接力高、固化物的耐水性及耐热性也优异的性质。因此，上述热固化性化合物优选为环氧化合物。
作为上述环氧化合物，可列举：双酚型环氧化合物、苯酚酚醛清漆型环氧化合物、联苯酚醛清漆型环氧化合物、联苯酚型环氧化合物、间苯二酚型环氧化合物、萘型环氧化合物、芴型环氧化合物、苯酚芳烷基型环氧化合物、萘酚芳烷基型环氧化合物、二环戊二烯型环氧化合物、蒽型环氧化合物、具有金刚烷骨架的环氧化合物、具有三环癸烷骨架的环氧化合物及骨架中具有三嗪核的环氧化合物等。作为上述双酚型环氧化合物，可列举：双酚A型环氧化合物、双酚F型环氧化合物及双酚S型环氧化合物等。
上述环氧化合物可以具有环氧基及自由基聚合性基团。上述自由基聚合性基团是指可以利用自由基进行加成聚合的基团。作为上述自由基聚合性基团，可列举含有不饱和双键的基团等。作为上述自由基聚合性基团的具体例，可列举：烯丙基、异丙烯基、马来酰基、苯乙烯基、乙烯基苄基、(甲基)丙烯酰基及乙烯基等。需要说明的是，(甲基)丙烯酰基是指丙烯酰基和甲基丙烯酰基。
从更进一步提高组合物的速固化性及固化物的耐湿热性的观点出发，上述自由基聚合性基团优选具有乙烯基，更优选为(甲基)丙烯酰基。在上述自由基聚合性基团为(甲基)丙烯酰基的情况下，上述自由基聚合性基团具有乙烯基。
从更进一步提高组合物的速固化性的观点出发，上述环氧化合物优选在两末端具有环氧基。从更进一步提高固化物的耐湿热性的观点出发，上述环氧化合物优选在侧链上具有乙烯基，优选具有(甲基)丙烯酰基，优选在侧链上具有(甲基)丙烯酰基。
从更进一步提高组合物的速固化性及固化物的耐湿热性的观点出发，上述环氧化合物的重均分子量优选为500以上，更优选为1000以上，优选为150000以下，更优选为50000以下，进一步优选为15000以下。
上述环氧化合物的重均分子量表示利用凝胶渗透色谱法(GPC)测定的、以聚苯乙烯计的重均分子量。
上述环氧化合物更优选使用了二醇化合物和具有2个环氧基的化合物的反应物。上述环氧化合物优选通过使二醇化合物和具有2个环氧基的化合物之间的反应物与具有乙烯基的化合物或具有环氧基的化合物进行反应而得到。
上述环氧化合物优选在侧链上具有1个以上的乙烯基，更优选在侧链上总计具有2个以上的乙烯基。乙烯基的数量越多，越可以更加缩短加热时间，进而可以更进一步提高固化物的粘接性及耐湿热性。
上述环氧化合物优选是具有2个以上的酚性羟基的化合物与具有2个以上的环氧基的化合物之间的反应物。
作为具有2个以上的上述酚性羟基的化合物，可列举双酚化合物、间苯二酚及萘酚等。作为上述双酚化合物，可列举：双酚F、双酚A、双酚S、双酚SA及双酚E等。
作为上述具有2个以上的环氧基的环氧化合物，可列举脂肪族环氧化合物及芳香族环氧化合物等。作为上述脂肪族环氧化合物，可列举：在碳原子数为3～12的烷基链的两末端具有缩水甘油醚基的化合物、以及具有碳原子为数2～4的聚醚骨架、且具有2～10个该聚醚骨架连续键合而成的结构单元的聚醚型环氧化合物。
上述环氧化合物优选通过使具有自由基聚合性基团的化合物与下述反应物(以下，有时记载为反应物X)反应而得到，所述反应物是双酚F或间苯二酚与1,6-己二醇二缩水甘油醚或间苯二酚二缩水甘油醚之间的反应物。在该反应中，进行反应使得自由基聚合性基团残留。使用这种化合物合成的环氧化合物可以更加快速地固化，进而可以更进一步提高固化物的粘接性及耐湿热性。上述具有自由基聚合性基团的化合物优选为(甲基)丙烯酸或(甲基)丙烯酰氧基乙基异氰酸酯。
作为上述反应物X，可列举：双酚F与1,6-己二醇二缩水甘油醚反应得到的第1反应物、间苯二酚与1,6-己二醇二缩水甘油醚反应得到的第2反应物、间苯二酚与间苯二酚二缩水甘油醚反应得到的第3反应物、及双酚F与间苯二酚二缩水甘油醚反应得到的第4反应物。
上述第1反应物在主链上具有来自双酚F的骨架和来自1,6-己二醇二缩水甘油醚的骨架键合而成的结构单元，且在两末端具有来自1,6-己二醇二缩水甘油醚的环氧基。上述第2反应物在主链上具有来自间苯二酚的结构单元和来自1,6-己二醇二缩水甘油醚的结构单元，且在两末端具有来自1,6-己二醇二缩水甘油醚的环氧基。上述第3反应物在主链上具有来自间苯二酚的骨架和来自间苯二酚二缩水甘油醚的骨架，且在两末端具有来自间苯二酚二缩水甘油醚的环氧基。上述第4反应物在主链上具有来自双酚F的骨架和来自间苯二酚二缩水甘油醚的骨架，且在两末端具有来自间苯二酚二缩水甘油醚的环氧基。
从容易合成、能够使环氧化合物更加快速地固化、进而更进一步提高固化物的粘接性及耐湿性的观点出发，上述第1反应物、第2反应物、第3反应物、第4反应物中，优选上述第1反应物、上述第2反应物或上述第3反应物。上述反应物X优选为上述第1反应物，也优选为上述第2反应物，进一步优选为上述第3的反应物。
[潜伏性固化剂]
作为上述潜伏性固化剂，可列举：潜伏性咪唑固化剂、潜伏性胺固化剂、潜伏性苯酚固化剂、三氟化硼-胺络合物及有机酸酰肼等。上述潜伏性固化剂可以具有芳香族骨架，也可以不具有芳香族骨架。上述潜伏性固化剂可以单独使用1种，也可以组合使用2种以上。
作为上述潜伏性咪唑固化剂的市售品，可列举：日本曹达社制造的笼形咪唑化合物“TEP-2MZ”、“TEP-2E4MZ”及“TEP-1B2MZ”、以及四国化成工业社制的“CUREDUCT P-0505”等。
作为上述潜伏性胺固化剂，可列举：二氰二酰胺、改性胺化合物及胺加合物化合物等。
作为上述改性胺化合物的市售品，可列举T&KTOKA社制的“FujicureFXR-1020”、“Fujicure FXR-1030”及“Fujicure FXR-1081”等。作为上述胺加合物化合物，可列举味之素Finetech社制的“Amicure PN-23”、“AmicurePN-H”、“Amicure PN-31”、“Amicure PN-40”、“Amicure PN-50”、“AmicurePN-F”、“Amicure PN-23J”、“Amicure PN-31J”、“Amicure PN-40J”、“Amicure PN-40”、“Amicure MY-24”、“Amicure MY-H”及“Amicure 25”等。
作为上述有机酸酰肼的市售品，可列举味之素Finetech社制的“AmicureVDH”、“Amicure VDH-J”、“Amicure UDH”及“Amicure UDH-J”等。
从更进一步提高组合物的速固化性的观点出发，上述潜伏性固化剂优选为潜伏性咪唑固化剂，更优选为微胶囊型咪唑固化剂。从更进一步提高组合物的保存稳定性的观点出发，上述潜伏性固化剂更优选为微胶囊型潜伏性固化剂，更优选为微胶囊型咪唑固化剂。
作为上述微胶囊型咪唑固化剂的市售品，可列举旭化成E-materials社制的“Novacure HX3941HP”、“Novacure HX3921HP”、“Novacure HX3721”、“Novacure HX3722”、“Novacure HX3748”、“Novacure HX3088”、“NovacureHX3741”、“Novacure HX3742”及“Novacure HX3613”等。
相对于上述热固化性化合物100重量份，上述潜伏性固化剂的含量优选为1重量份以上，更优选为5重量份以上，优选为65重量份以下，更优选为55重量份以下。上述潜伏性固化剂的含量为上述下限以上及上述上限以下时，组合物的速固化性及铜电极间的导通性均衡地升高。
[具有芳香族骨架的咪唑化合物]
上述具有芳香族骨架的咪唑化合物不是潜伏性固化剂。作为上述具有芳香族骨架的咪唑化合物，不包括潜伏性固化剂。上述固化性组合物中所含的潜伏性固化剂与上述固化性组合物中所含的具有芳香族骨架的咪唑化合物不同。上述具有芳香族骨架的咪唑化合物可以单独使用1种，也可以组合使用2种以上。
作为上述芳香族骨架，可列举芳基骨架、萘骨架及蒽骨架等。从有效地提高铜电极间的导通性的观点出发，上述芳香族骨架优选为芳基骨架，更优选为苯基骨架。
作为上述具有芳香族骨架的咪唑化合物，可列举：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、1-苄基-2-甲基咪唑、1-氰基乙基-2-苯基咪唑、1-氰基乙基-2-苯基咪唑鎓偏苯三酸盐、2-苯基-4-甲基-5-二羟基甲基咪唑、2-苯基-4，5-二羟基甲基咪唑、及2-苯基-4-甲基-5-羟基甲基咪唑等。
上述具有芳香族骨架的咪唑化合物的含量相对于上述热固化性化合物100重量份，优选为0.1重量份以上，更优选为0.5重量份以上，优选为10重量份以下，更优选为5重量份以下。上述具有芳香族骨架的咪唑化合物的含量为上述下限以上及上述上限以下时，组合物的速固化性及铜电极间的导通性均衡地升高。
[其它成分]
上述固化性组合物根据需要可以进一步含有焊剂、粘接力调整剂、无机填充剂、溶剂、贮藏稳定剂、离子捕捉剂或硅烷偶联剂等。
上述固化性化合物优选含有焊剂。通过焊剂的使用，铜电极的导通性更加提高。作为上述焊剂，可以使用公知的焊剂。上述焊剂可以单独使用1种，也可以组合使用2种以上。
上述焊剂没有特别限定。作为该焊剂，可以使用焊料接合等中一般所使用的焊剂。作为上述焊剂，可列举例如：氯化锌、氯化锌和无机卤化物的混合物、氯化锌和无机酸的混合物、熔融盐、磷酸、磷酸的衍生物、有机卤化物、肼、有机酸及松脂等。
作为上述熔融盐，可列举氯化胺等。作为上述有机酸，可列举乳酸、柠檬酸、硬脂酸及谷氨酸等。作为上述松脂，可列举活性化松脂及非活性化松脂等。上述焊剂优选为松脂。通过松脂的使用，电极间的连接电阻更变得更低。
上述松脂为以松香酸为主成分的松香类。上述焊剂优选为松香类，更优选为松香酸。通过使用该优选的焊剂，电极间的连接电阻更进一步变低。另外，上述焊剂优选为具有羧基的有机酸。作为具有羧基的化合物，可列举：烷基链上键合有羧基的化合物、芳香环上键合有羧基的化合物等。就这些具有羧基的化合物而言，也可以在烷基链或芳香环上进一步键合羟基。烷基链或芳香环上键合的羧基的数优选为1～3个，更优选为1或2个。烷基链上键合有羧基的化合物中烷基链的碳原子数优选为3以上，优选为8以下，更优选为6以下。作为烷基链上键合有羧基的化合物的具体例，可列举己烷酸(碳原子数5、羧基1个)及戊二酸(碳原子数4、羧基2个)等。作为具有羧基和羟基的化合物的具体例，可列举苹果酸及柠檬酸等。作为芳香环上键合有羧基的化合物的具体例，可列举：苯甲酸、邻苯二甲酸、苯甲酸酐及邻苯二甲酸酐等。
相对于上述热固化性化合物100重量份，上述焊剂的含量优选为0.5重量份以上，更优选为1重量份以上，优选为10重量份以下，更优选为5重量份以下。上述焊剂的含量为上述下限以上及上限以下时，更加有效地显现焊剂的添加效果。因此，组合物中的焊剂效果得到提高，例如铜电极的导通性更加得到提高。
(含有导电性粒子的电子部件用固化性组合物)
在上述固化性组合物含有导电性粒子的情况下，可以将上述固化性组合物用作导电材料。上述导电材料优选为各向异性导电材料。
上述导电性粒子对连接对象部件的电极间进行电连接。具体而言，上述导电性粒子对例如电路基板和半导体芯片的电极间进行电连接。上述导电性粒子只要是具有导电性的粒子，就没有特别限定。上述导电性粒子只要在导电性的表面具有导电部即可。
作为上述导电性粒子，可列举例如：将除有机粒子、金属粒子之外的无机粒子、有机无机杂化粒子或金属粒子等的表面用导电层(金属层)包覆的导电性粒子、或实质上仅由金属构成的金属粒子等。
图3用剖面图示出可以在本发明的一个实施方式中涉及的电子部件用固化性组合物中使用的导电性粒子。
图3示出的导电性粒子21具有树脂粒子22(基材粒子)和配置于树脂粒子22的表面22a上的导电层23。导电层23对树脂粒子22的表面22a进行包覆。导电性粒子21是利用导电层23对树脂粒子22的表面22a进行包覆而成的包覆粒子。因此，导电性粒子21在表面21a上具有导电层23。除树脂粒子22之外，还可以使用金属粒子等。
导电层23具有配置于树脂粒子22的表面22a上的第1导电层24和配置于该第1导电层24的表面24a上的焊料层25(焊料、第2导电层)。导电层23的外侧表面层为焊料层25。因此，导电性粒子21具有焊料层25作为导电层23的一部分，并具有在树脂粒子22和焊料层25之间且不同于焊料层25的第1导电层24作为导电层23的一部分。这样，导电层23可以具有多层结构，也可以具有2层以上的叠层结构。
如上所述，导电层23具有2层结构。如图4所示的变形例那样，导电性粒子31作为单层的导电层，可以具有焊料层32。导电性粒子中导电层的至少外侧表面层(表面)只要为焊料层(焊料)即可。但是，导电性粒子的制作容易，因此，在导电性粒子21和导电性粒子31中，优选导电性粒子21。另外，如图5所示的变形例那样，可以使用芯中不具有基材粒子的焊料粒子的导电性粒子41而不使用芯-壳粒子。导电性粒子41的中心部也由焊料形成。
导电性粒子21、31、41可以在上述导电材料中使用。
上述导电部没有特别限定。作为构成上述导电部的金属，可列举金、银、铜、镍、钯及锡等。作为上述导电层，可列举含有金层、银层、铜层、镍层、钯层或锡的导电层等。
从增大电极与导电性粒子的接触面积、更进一步提高电极间的导通可靠性的观点出发，优选上述导电性粒子具有树脂粒子和配置于该树脂粒子表面上的导电层(第1导电层)。从更进一步提高电极间的导通可靠性的观点出发，优选上述导电性粒子是至少导电性的外侧表面为低熔点金属层的导电性粒子。从更进一步提高耐湿热性及导通性的观点出发，更优选上述导电性粒子具有基材粒子和配置于该基材粒子的表面上的导电层、该导电层的至少外侧表面为低熔点金属层。更优选上述导电性粒子具有树脂粒子和配置于该树脂粒子表面上的导电层，且该导电层的至少外侧表面为低熔点金属层。
上述低熔点金属层为含有低熔点金属的层。该低熔点金属表示熔点为450℃以下的金属。低熔点金属的熔点优选为300℃以下，更优选为160℃以下。另外，上述低熔点金属优选含有锡。低熔点金属中所含的金属100重量％中，锡的含量优选为30重量％以上，更优选为40重量％以上，进一步优选为70重量％以上，特别优选为90重量％以上。上述低熔点金属中锡的含量为上述下限以上时，低熔点金属与电极的连接可靠性更加得到提高。需要说明的是，上述锡的含量可以使用高频感应偶合等离子体发光分光分析装置(堀场制作所社制造“ICP-AES”)、或荧光X射线分析装置(岛津制作所社制造“EDX-800HS”)等进行测定。从更进一步提高耐湿热性及导通性的观点出发，优选上述导电性粒子为导电性的外侧的表面为焊料的导电性粒子。
在导电部的外侧表面为低熔点金属层的情况下，低熔点金属层熔融而与电极接合，低熔点金属层使电极间导通。例如，低熔点金属层与电极容易进行面接触而不是点接触，因此连接电阻变低。另外，通过使用至少导电性的外侧表面为低熔点金属层的导电性粒子，低熔点金属层与电极之间的接合强度升高，结果，低熔点金属层与电极的剥离更加难以产生，导通可靠性有效地得到提高。
上述构成低熔点金属层的低熔点金属没有特别限定。上述低熔点金属优选为锡、或含有锡的合金。该合金可列举：锡-银合金、锡-铜合金、锡-银-铜合金、锡-铋合金、锡-锌合金、锡-铟合金等。其中，由于相对于电极的润湿性优异，因此，优选上述低熔点金属为锡、锡-银合金、锡-银-铜合金、锡-铋合金、锡-铟合金。更优选为锡-铋合金、锡-铟合金。
另外，上述低熔点金属优选为焊料。构成上述焊料的材料没有特别限定，基于JIS Z3001：焊接用语，优选为液相线为450℃以下的填焊金属。作为上述焊料的组分，可列举含有例如锌、金、铅、铜、锡、铋、铟等的金属组分。其中，优选低熔点且无铅的锡-铟系(117℃共晶)、或锡-铋系(139℃共晶)。即，优选上述焊料为含有锡和铟的焊料、或含有锡和铋的焊料，且优选不含有铅。
为了更进一步提高上述低熔点金属与电极的接合强度，上述低熔点金属可以含有镍、铜、锑、铝、锌、铁、金、钛、磷、锗、碲、钴、铋、锰、铬、钼、钯等金属。从更进一步提高低熔点金属与电极的接合强度的观点出发，优选上述低熔点金属含有镍、铜、锑、铝或锌。从更进一步提高低熔点金属与电极的接合强度的观点出发，用于提高接合强度的这些金属的含量在低熔点金属100重量％中，优选为0.0001重量％以上，优选为1重量％以下。
上述导电性粒子具有树脂粒子和配置于该树脂粒子的表面上的导电层，该导电层的外侧表面为低熔点金属层，优选具有在上述树脂粒子与上述低熔点金属层(焊料层等)之间的、且与上述低熔点金属层不同的第2导电层。该情况下，上述低熔点金属层为上述导电层整体的一部分，上述第2导电层为上述导电层整体的一部分。
优选与上述低熔点金属层不同的上述第2导电层含有金属。构成该第2导电层的金属没有特别限定。作为该金属，可列举例如：金、银、铜、铂、钯、锌、铅、铝、钴、铟、镍、铬、钛、锑、铋、锗及镉、以及它们的合金等。另外，作为上述金属，可以使用锡掺杂氧化铟(ITO)。上述金属可以单独使用1种，也可以组合使用2种以上。
上述第2导电层优选为镍层、钯层、铜层或金层，更优选为镍层或金层，进一步优选为铜层。导电性粒子优选具有镍层、钯层、铜层或金层，更优选具有镍层或金层，进一步优选具有铜层。通过将具有这些优选的导电层的导电性粒子用于电极间的连接，电极间的连接电阻变得更低。另外，低熔点金属层可以更容易地形成于这些优选的导电层的表面。需要说明的是，上述第2导电层可以为焊料层等低熔点金属层。导电性粒子可以具有多层的低熔点金属层。
上述低熔点金属层的厚度优选为0.1μm以上，更优选为0.5μm以上，进一步优选为1μm以上，优选为50μm以下，更优选为10μm以下，进一步优选为5μm以下，特别优选为3μm以下。上述低熔点金属层的厚度为上述下限以上时，导电性充分地得到提高。上述低熔点金属层的厚度为上述上限以下时，树脂粒子与低熔点金属层的热膨胀率之差变小，难以产生低熔点金属层的剥离。
在导电层为低熔点金属层以外的导电层的情况、或导电层具有多层结构的情况下，导电层的整体厚度优选为0.1μm以上，更优选为0.5μm以上，进一步优选为1μm以上，优选为50μm以下，更优选为10μm以下，进一步优选为5μm以下，特别优选为3μm以下。
上述导电性粒子的平均粒径优选为100μm以下，更优选为20μm以下，更加优选小于20μm，进一步优选为15μm以下，特别优选为10μm以下。导电性粒子的平均粒径优选为0.5μm以上，更优选为1μm以上。从更进一步提高受到热史时的连接结构体的连接可靠性的观点出发，导电性粒子的平均粒径特别优选为1μm以上、10μm以下，最优选为1μm以上、4μm以下。优选导电性粒子的平均粒径为3μm以下。
导电性粒子的平均粒径为适于上述导电材料中的导电性粒子的大小、且可以更加缩小电极间的间隔，因此，导电性粒子的平均粒径特别优选为1μm以上且100μm以下。
上述导电性粒子的“平均粒径”表示数均粒径。导电性粒子的平均粒径通过用电子显微镜或光学显微镜对任意的50个导电性粒子进行观察，并算出平均值而求出。
上述导电性粒子的表面可以利用绝缘性粒子等绝缘性材料、焊剂等进行绝缘处理。优选绝缘性材料、焊剂等通过进行连接时的热进行软化、流动而从连接部排除。由此，抑制电极间的短路。
上述导电性粒子的含量没有特别限定。上述固化性组合物100重量％中，上述导电性粒子的含量优选为0.1重量％以上，更优选为0.5重量％以上，优选为40重量％以下，更优选为20重量％以下，进一步优选为15重量％以下。上述导电性粒子的含量为上述下限以上及上述上限以下时，可以将导电性粒子容易地配置在应该连接的上下的电极间。而且，不能连接的邻接的电极间隔着多个导电性粒子而难以电连接。即，可以防止相邻的电极间的短路。
(电子部件用固化性组合物的用途)
上述固化性组合物可以为了对各种连接对象部件进行粘接而使用。但是，上述固化性组合物用于铜电极的连接。上述固化性组合物可以为膜，也可以为糊。优选上述固化性组合物为糊。上述固化性组合物为糊时，初期的连接电阻变得更低。进而，也可以有效地较低地对暴露于冲击或高温高湿后的连接电阻进行维持。
上述固化性组合物为含有导电性粒子的导电材料时，该导电材料可以作为导电糊、或导电膜等使用。上述导电材料作为导电膜使用时，可以将不含有导电性粒子的膜叠层在含有导电性粒子的该导电膜上。需要说明的是，膜包括片材。优选上述固化性组合物为糊状的导电糊。优选上述导电糊为各向异性导电糊。优选上述导电膜为各向异性导电膜。
上述固化性组合物优选使用于得到连接结构体，所述连接结构体具备：表面具有第1电极的电极第1连接对象部件、表面具有第2电极的第2连接对象部件、对上述第1连接对象部件和上述第2连接对象部件进行连接的连接部。上述连接部通过使上述固化性组合物固化而形成。上述连接结构体中，上述第1电极及上述第2电极中的至少一种为铜电极。对上述第1电极和上述第2电极进行电连接。更优选上述第1电极及上述第2电极的两者为铜电极。
优选上述电子部件用固化性组合物含有导电性粒子，并通过上述导电性粒子得到使上述第1电极与上述第2电极电连接的连接结构体。
本发明所述的连接结构体的制造方法包括：将上述电子部件用固化性组合物配置于表面具有第1电极的第1连接对象部件和表面具有第2电极的第2连接对象部件之间的工序；通过使上述电子部件用固化性组合物固化，形成使上述第1连接对象部件和上述第2连接对象部件连接的连接部，并得到使上述第1电极和上述第2电极电连接的连接结构体的工序。上述第1电极及上述第2电极中的至少一种为铜电极。
本发明所述的连接结构体的制造方法中，优选上述电子部件用固化性组合物含有导电性粒子，通过上述导电性粒子得到使上述第1电极和上述第2电极电连接的连接结构体。
图1中，用剖面图示意性地示出使用有本发明的一个实施方式中涉及的固化性组合物的连接结构体的一个例子。
图1所示的连接结构体1具备：第1连接对象部件2、第2连接对象部件4、对第1连接对象部件2和第2连接对象部件4进行连接的连接部3。连接部3为固化物层，通过使含有导电性粒子5的电子部件用固化性组合物(导电材料)固化而形成。
第1连接对象部件2在表面(上面)具有多个第1电极2a。第2连接对象部件4在表面(下面)具有多个第2电极4a。第1电极2a和第2电极4a中的至少一种为铜电极。通过1个或多个导电性粒子5使第1电极2a与第2电极4a进行电连接。因此，第1连接对象部件2、第2连接对象部件4通过导电性粒子5而电连接。
通常，第1电极2a、第2电极4a间的连接如下进行：通过对第1连接对象部件2和第2连接对象部件4隔着上述固化性组合物进行叠合使得第1电极2a、第2电极4a彼此对置，然后，在使上述固化性组合物固化时加压。一般而言，通过加压，导电性粒子5被压缩。
上述第1连接对象部件、第2连接对象部件没有特别限定。作为上述第1连接对象部件、第2连接对象部件，具体而言，可列举半导体芯片、电容器及二极管等电子部件、以及印刷基板、挠性印刷基板、玻璃环氧基板及玻璃基板等电路基板等电子部件等。
需要说明的是，上述固化性组合物可以含有导电性粒子。在该情况下，可以使第1连接对象部件、第2连接对象部件的电极间不通过导电性粒子电连接，例如，使电极彼此接触而使电极间电连接。
图2中，用剖面图示意性地示出图1所示的连接结构体的变形例。
图2所示的连接结构体11具备：第1连接对象部件12、第2连接对象部件14、对第1连接对象部件12和第2连接对象部件14进行连接的连接部13。连接部13为固化物层，通过使不含有导电性粒子的电子部件用固化性组合物(导电材料)固化而形成。
第1连接对象部件12在表面(上面)具有多个第1电极12a。第2连接对象部件14在表面(下面)具有多个第2电极14a。第1电极12a和第2电极14a中的至少一种为铜电极。第1电极12a和第2电极14a例如为凸块电极。通过第1电极12a和第2电极14a相互连接进行电连接而不经由导电性粒子进行电连接。因此，第1连接对象部件12、第2连接对象部件14发生电连接。
在上述固化性组合物为导电材料的情况下，该导电材料可以用于例如挠性印刷基板和玻璃基板的连接(FOG(Film on Glass))、半导体芯片和挠性印刷基板的连接(COF(Chip on Film))、半导体芯片和玻璃基板的连接(COG(Chip onGlass))、或挠性印刷基板和玻璃环氧基板的连接(FOB(Film on Board))等。其中，上述导电材料适于FOG用途或COG用途，更适于COG用途。上述固化性组合物优选为用于挠性印刷基板和玻璃基板的连接、或半导体芯片和挠性印刷基板的连接的导电材料，更优选为用于半导体芯片和挠性印刷基板的连接的导电材料。
以下，列举实施例及比较例，对本发明具体地进行说明。本发明并不仅限定于以下的实施例。
准备以下的配合成分。
(热固化性化合物)
热固化性化合物1(含环氧基的聚合物、日油社制造“MARPROOFG-01100”、重均分子量：12000、Tg：47℃、环氧当量：170g/eq)
热固化性化合物2(间苯二酚型环氧化合物、Nagase chemteX社制造“EX-201”)
热固化性化合物3(三嗪三缩水甘油醚、日产化学社制“TEPIC-SS”)
(潜伏性固化剂)
潜伏性固化剂1(笼形咪唑化合物、日本曹达社制“TEP-2MZ”)
潜伏性固化剂2(环氧基-咪唑加合物、四国化成工业社制造“CUREDUCTP-0505”)
潜伏性固化剂3((微胶囊型潜伏性固化剂)、旭化成E-materials社制社制造“Novacure HX3921HP”)
潜伏性固化剂4((微胶囊型潜伏性固化剂)、旭化成E-materials社制社制造“Novacure HX3941HP”)
(具有芳香族骨架的咪唑化合物)
含芳香族骨架的咪唑化合物1(四国化成工业社制造“2-苯基咪唑”)
含芳香族骨架的咪唑化合物2(四国化成工业社制造“2-苯基-4-甲基咪唑”)
含芳香族骨架的咪唑化合物3(和光纯药工业社制造“苯并咪唑”)
含芳香族骨架的咪唑化合物4(和光纯药工业社制造“2-甲基苯并咪唑”)
(其它咪唑化合物)
其它咪唑化合物(不是潜伏性固化剂的、不具有芳香族骨架的、四国化成工业社制“2-甲基咪唑”)
(导电性粒子)
导电性粒子1：SnBi焊料粒子(福田金属社制“Sn58Bi-20”、平均粒径4.5μm)
导电性粒子2：(树脂芯焊料包覆粒子、按照下述步骤制作)
对二乙烯基苯树脂粒子(积水化学工业社制造“Micropearl SP-207”、平均粒径7μm、软化点330℃、10％K值(23℃)4GPa)进行无电解镀镍，在树脂粒子的表面上形成厚度0.1μm的基底镀镍层。接着，对形成有基底镀镍层的树脂粒子进行电解镀铜，形成厚度1μm的铜层。进一步，使用含有锡及铋的电解电镀液进行电解电镀，形成厚度1μm的焊料层。这样，在树脂粒子的表面上形成厚度1μm的铜层，制作在该铜层的表面形成有厚度1μm的焊料层(锡:铋＝43重量％:57重量％)的导电性粒子(平均粒径14μm、CV值22％、树脂芯焊料包覆粒子)。
导电性粒子3：二乙烯基苯树脂粒子的Au电镀粒子(积水化学工业社制“Au-210”、平均粒径10μm)
(其它)
填料(纳米二氧化硅、株式会社德山制造“MT-10”)
增粘剂(信越化学工业社制造“KBE-403”)
焊剂(和光纯药工业社制造“Glutaric acid”)
苯氧基树脂(新日铁住金化学社制造“YP-50S”)
(实施例1～21及比较例1～3)
对下述的表1～3所示的成分以下述的表1～3所示的配合量进行配合，使用行星式搅拌机，以2000rpm搅拌5分钟，由此得到各向异性导电糊。
(实施例22)
将苯氧基树脂(新日铁住金化学社制“YP-50S”)10重量份溶解在甲基乙基酮(MEK)中使得固态成分为50重量％，得到溶解液。将除去下述的表3所示的苯氧基树脂的成分按照下述的表3所示的配合量与上述溶解液的总量进行配合，使用行星式搅拌机以2000rpm搅拌5分钟后，使用棒涂机涂敷于脱模PET(聚对苯二甲酸乙二醇酯)膜上，使得干燥后的厚度成为30μm。通过在室温下进行真空干燥而除去MEK，由此得到各向异性导电膜。
(评价)
(1)～(3)的评价项目中使用的连接结构体(FOB)的制作：
按照L/S为100μm/100μm的电极图案，准备上面具有70根铜电极的玻璃环氧基板(FR-4基板)。另外，按照L/S为100μm/100μm的电极图案，准备下面具有70根铜电极的挠性印刷基板。对FR-4基板和挠性印刷基板的图案进行设计使得其可以通过叠合而形成雏菊链。
在上述玻璃环氧基板的上面对得到的各向异性导电糊进行涂敷使得其厚度成为200μm，形成各向异性导电糊层。接着，将上述挠性印刷基板叠层于各向异性导电糊层上使得电极彼此对置。然后，一边调整加热压接头的温度使得各向异性导电糊层的温度成为170℃(本压接温度)，一边将加压压接头载置在挠性印刷基板的上面，直至施加1MPa的压力且在170℃下完成固化为止使各向异性导电糊层进行固化，得到连接结构体(FOB)。
(1)固化速度
在得到上述连接结构体时，对通过加热直至各向异性导电糊层固化为止的时间进行测定。具体而言，按照得到上述连接结构体的步骤将各向异性导电糊涂布于上述玻璃环氧基板上之后，对在170℃电热板上各向异性导电糊层的表面的粘性(用安田精机制作所制的球粘性试验机、助跑道：100mm、测定部：100mm、倾斜角度30°、球φ1/16在测定部不停止的程度的粘合性)消失为止的凝胶化时间。按照下述的基准判定固化速度。
[固化速度的判定基准]
○：直至表面的粘性消失为止的凝胶化时间小于3秒
×：直至表面的粘性消失的凝胶化时间为3秒以上
(2)导通性
使用得到的连接结构体，利用4端子法对20处的连接电阻进行评价。按照下述的基准判定导通性。
[导通性的判定基准]
○○：连接电阻的平均值为8.0Ω以下
○：连接电阻的平均值超过8.0Ω、且为10.0Ω以下
△：连接电阻的平均值超过10.0Ω、且为15.0Ω以下
×：连接电阻的平均值超过15.0Ω
(3)耐热冲击性
分别准备10个得到的连接结构体，在－30℃下保持5分钟，接着，升温至80℃并保持5分钟后，降温至－30℃，将该过程设为1次循环，实施每1循环设为1小时的冷热循环试验。在500循环后，分别取出10个连接结构体。
对进行了500次循环的冷热循环试验后的10个连接结构体，计数产生上下的电极间的导通不良的个数。按照下述的基准对耐热冲击性进行判定。
[耐热冲击性的判定基准]
○○：全部10个连接结构体，从冷热循环试验前的连接电阻的连接电阻上升率为5％以下
○：全部10个的连接结构体，从冷热循环试验前的连接电阻的连接电阻上升率超过5％且为10％以下
×：10个连接结构体中，从冷热循环试验前的连接电阻的连接电阻上升率超过10％的连接结构体为1个以上
(4)耐湿热性
通过偏压试验评价耐湿热性。具体而言，准备在上面具有L/S为100μm/100μm的70根梳形铜电极图案的玻璃环氧基板(FR-4基板)。另外，准备在下面具有L/S为100μm/100μm的70根梳形铜电极图案的挠性印刷基板。用与(1)～(3)的评价项目中使用的连接结构体的制作方法相同的方法得到连接结构体。对FR-4基板和挠性印刷基板的图案进行涉及使得可以通过叠合而形成梳形图案。按照下述的基准对耐湿热性进行判定。
[耐湿热性的判定基准]
○○：电阻值为108Ω以上
○：电阻值为5×107Ω以上且小于108Ω
△：电阻值为107Ω以上且小于5×107Ω
×：电阻值小于107Ω
(5)保存稳定性
将各向异性导电糊在23℃下静置48小时，使用E型粘度计TV-33(东机产业社制)对静置前后的粘度变化进行测定。由静置前后的粘度变化按照下述的基准对保存稳定性进行判定。
[保存稳定性的判定基准]
○○：静置48小时后的粘度/初期粘度小于1.2
○：静置48小时后的粘度/初期粘度为1.2以上且小于1.5
×：静置48小时后的粘度/初期粘度为1.5以上
(6)保存稳定性
将各向异性导电糊在40℃下静置48小时，使用E型粘度计TV-33(东机产业社制)对静置前后的粘度变化进行测定。由静置前后的粘度变化按照下述的基准对保存稳定性进行判定。
[保存稳定性的判定基准]
○○：静置48小时后的粘度/初期粘度小于1.2
○：静置48小时后的粘度/初期粘度为1.2以上且小于1.35
△：静置48小时后的粘度/初期粘度为1.35以上且小于1.5
×：静置48小时后的粘度/初期粘度为1.5以上
将结果示于下述的表1～3。
[表1]
[表2]
[表3]
对使用了上面具有铜电极的玻璃环氧基板(连接对象部件)和下面具有铜电极的挠性印刷基板(连接对象部件)的连接结构体的评价结果进行表示。确认到：在这些2个连接对象部件中的仅一个的电极为铜电极，而剩余电极为铝电极的情况下，可得到与表1～3所示的评价结果的倾向相同的评价结果。需要说明的是，在这些2个连接对象部件的电极的两者为铝电极的情况下，实施例和比较例的评价结果的差异小。即，在2个连接对象部件的电极中的至少一个电极为铜电极的情况下，与2个连接对象部件的电极的两者电极为铝电极的情况相比，实施例与比较例的评价结果的差异大。由此可知：通过在铜电极的连接中使用本发明所述的电子部件用固化性组合物，可有效地发挥本发明的效果。
另外，实施例16～21中，潜伏性固化剂为微胶囊型咪唑固化剂，因此，比较高的温度(40℃)下的保存稳定性很优异。

Claims (9)

1.一种电子部件用固化性组合物，其用于铜电极的连接，
所述固化性组合物含有热固化性化合物、潜伏性固化剂、具有芳香族骨架的咪唑化合物。
2.如权利要求1所述的电子部件用固化性组合物，其中，
所述潜伏性固化剂为微胶囊型咪唑固化剂。
3.如权利要求1或2所述的电子部件用固化性组合物，其含有导电性粒子。
4.如权利要求3所述的电子部件用固化性组合物，其中，
所述导电性粒子是导电性的外表面为焊料的导电性粒子。
5.如权利要求1～4中任一项所述的电子部件用固化性组合物，其中，
该电子部件用固化性组合物为糊。
6.一种连接结构体，其具备：
表面具有第1电极的第1连接对象部件、
表面具有第2电极的第2连接对象部件、
将所述第1连接对象部件和所述第2连接对象部件连接起来的连接部，
所述连接部通过使权利要求1～5中任一项所述的电子部件用固化性组合物固化而形成，
所述第1电极及所述第2电极中的至少之一为铜电极，
将所述第1电极和所述第2电极电连接。
7.如权利要求6所述的连接结构体，其中，
所述电子部件用固化性组合物含有导电性粒子，
所述第1电极和所述第2电极通过所述导电性粒子进行电连接。
8.一种连接结构体的制造方法，该方法包括：
在表面具有第1电极的第1连接对象部件和在表面具有第2电极的第2连接对象部件之间设置权利要求1～5中任一项所述的电子部件用固化性组合物的工序；
通过使所述电子部件用固化性组合物固化，形成将所述第1连接对象部件和所述第2连接对象部件连接起来的连接部，得到所述第1电极和所述第2电极实现了电连接的连接结构体的工序，
所述第1电极及所述第2电极中的至少之一为铜电极。
9.如权利要求8所述的连接结构体的制造方法，其中，
所述电子部件用固化性组合物含有导电性粒子，
得到所述第1电极和所述第2电极通过所述导电性粒子进行了电连接的连接结构体。
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