CN105594064A - 电连接材料 - Google Patents

电连接材料 Download PDF

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Publication number
CN105594064A
CN105594064A CN201480054982.0A CN201480054982A CN105594064A CN 105594064 A CN105594064 A CN 105594064A CN 201480054982 A CN201480054982 A CN 201480054982A CN 105594064 A CN105594064 A CN 105594064A
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layer
conducting particles
resin composition
electrical connection
free radical
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CN201480054982.0A
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CN105594064B (zh
Inventor
阿久津恭志
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Dexerials Corp
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Dexerials Corp
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    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/46—Polymerisation initiated by wave energy or particle radiation
    • C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
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    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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    • H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
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Abstract

本发明涉及各向异性导电膜等电连接材料，所述材料抑制在各向异性导电连接部等电连接部产生翘曲，而且不使通过各向异性导电连接等电连接而得到的连接体的导电可靠性降低，所述材料具有用第1绝缘性热固型树脂组合物层和第2绝缘性热固型树脂组合物层夹持含有导电粒子的层的结构。该含有导电粒子的层是通过光照射使含有丙烯酸酯系自由基聚合性化合物、光自由基聚合引发剂、环氧系非自由基聚合性化合物和导电粒子的含有导电粒子的树脂组合物层光自由基聚合而乙阶化。第1绝缘性热固型树脂组合物层和第2绝缘性热固型树脂组合物层各自含有环氧系非自由基聚合性化合物和热阳离子聚合引发剂或热阴离子聚合引发剂。

Description

电连接材料
技术领域
本发明涉及各向异性导电膜等电连接材料、其制备方法及连接体。
背景技术
在将IC芯片等电气部件安装于基板等时，将由导电粒子和作为其分散介质的粘合剂树脂组合物构成的各向异性导电膜广泛用作电连接材料。由于对这样的各向异性导电膜要求高的粘接强度，所以广泛使用可实现比丙烯酸酯系粘接剂组合物高的粘接强度的环氧系粘接剂组合物作为粘合剂树脂组合物。通常，这样的环氧系粘接剂组合物是在环氧系化合物中掺混阴离子系固化剂或阳离子系固化剂而得到。
但是，在将环氧系粘接剂组合物用作粘合剂树脂组合物的各向异性导电膜的情况下，由于环氧系粘接剂组合物的固化物无法充分地缓和因该环氧系粘接剂组合物的固化收缩而在各向异性导电连接部产生的应力，所以有会在各向异性导电连接部产生翘曲这样的问题。因此，提出了在使用阳离子系固化剂的环氧系粘接剂组合物中掺混提供与它们相比应力松弛能力较优异的固化物的丙烯酸酯系自由基聚合性组合物，使得不降低环氧系粘接剂组合物的高粘接强度而赋予应力松弛能力(专利文献1)。
现有技术文献
专利文献
专利文献1：日本特开2006-127776号公报。
发明内容
发明所要解决的课题
但是，在专利文献1的各向异性导电膜的情况下，虽然可在某种程度上减少各向异性导电连接部的翘曲的产生，但在高温高湿下保管使用各向异性导电膜形成的连接体的情况下，有导通电阻增大，导通可靠性降低这样的问题。
本发明的目的在于解决以上目前的技术问题，提供抑制在各向异性导电连接部等电连接部产生翘曲，而且不降低通过各向异性导电连接等电连接而得到的连接体的导通可靠性的各向异性导电膜等电连接材料。
解决课题的手段
本发明人发现，通过将各向异性导电膜等电连接材料制成用绝缘性热固型树脂组合物层夹持含有导电粒子的层的结构，并且作为该含有导电粒子的层，采用使以下树脂组合物层光固化而乙阶化的层，所述树脂组合物层是在含有导电粒子的丙烯酸酯系自由基聚合性组合物中不与环氧化合物用固化剂并用而掺混环氧系非自由基聚合性化合物而成，由此可达成上述目的，从而完成本发明。
即，本发明提供电连接材料，其为用第1绝缘性热固型树脂组合物层和第2绝缘性热固型树脂组合物层夹持含有导电粒子的层而得的电连接材料，优选为各向异性导电膜，其特征在于：
含有导电粒子的层是通过光照射使含有丙烯酸酯系自由基聚合性化合物、光自由基聚合引发剂、环氧系非自由基聚合性化合物和导电粒子的含有导电粒子的树脂组合物层光自由基聚合而乙阶化，
第1绝缘性热固型树脂组合物层和第2绝缘性热固型树脂组合物层各自含有环氧系非自由基聚合性化合物和热阳离子聚合引发剂或热阴离子聚合引发剂。
本发明还提供制备方法，其为上述本发明的电连接材料、优选各向异性导电膜的制备方法，其具有：
将含有丙烯酸酯系自由基聚合性化合物、光自由基聚合引发剂、环氧系非自由基聚合性化合物和导电粒子的含有导电粒子的树脂组合物成膜，对得到的膜照射光进行光自由基聚合而乙阶化，由此形成含有导电粒子的层的工序；和
在含有导电粒子的层的一面层合含有环氧系非自由基聚合性化合物和热阳离子聚合引发剂或热阴离子聚合引发剂的第1绝缘性热固型树脂组合物层，并在另一面层合含有环氧系非自由基聚合性化合物和热阳离子聚合引发剂或热阴离子聚合引发剂的第2绝缘性热固型树脂组合物层的工序。
此外，本发明提供连接体，其为通过上述本发明的电连接材料、优选各向异性导电膜将第1电气部件的端子与第2电气部件的端子通过热压接电连接、优选各向异性导电连接而成。
发明的效果
本发明的各向异性导电膜等电连接材料具有用第1绝缘性热固型树脂组合物层和第2绝缘性热固型树脂组合物层夹持含有导电粒子的层的结构。因此，例如若将第1绝缘性热固型树脂组合物层和第2绝缘性热固型树脂组合物层的固化收缩率彼此调和为相同水平，则可抑制使用各向异性导电膜等电连接材料制备的连接体的翘曲的产生。
另外，含有导电粒子的层是通过光照射使含有丙烯酸酯系自由基聚合性化合物、光自由基聚合引发剂、环氧系非自由基聚合性化合物和导电粒子的含有导电粒子的树脂组合物层光自由基聚合而乙阶化。因此，在进行各向异性导电连接等电连接时，导电粒子变得难以从需要连接的端子间(连接部)流动，从而可有助于提高导通可靠性。而且，可使各向异性导电膜等电连接材料整体展现应力松弛能力，也可有助于抑制使用各向异性导电膜等电连接材料制备的连接体的翘曲的产生。
此外，在此含有导电粒子的层中不含有使环氧系非自由基聚合性化合物聚合的聚合引发剂。因此，使得在乙阶化的含有导电粒子的层中含有未聚合的环氧系非自由基聚合性化合物，若使用液态的环氧化合物，则可在进行各向异性导电连接等电连接时确保压入导电粒子所需要的流动性。
另外，含有导电粒子的层中含有的环氧系非自由基聚合性化合物可通过热阳离子聚合或热阴离子聚合来进行阳离子聚合或阴离子聚合，所述热阳离子聚合或热阴离子聚合通过各向异性导电连接等电连接时的热压接而在第1和第2绝缘性热固型树脂组合物层中产生。由此，可使含有导电粒子的层充分地固化，可抑制使用各向异性导电膜等电连接材料制备的连接体的导通可靠性的降低。这样本申请发明的电连接材料作为各向异性导电膜有用，并且作为各向异性导电糊剂、通常的导电膜或导电糊剂也有用。
附图说明
图1是作为本发明的电连接材料的优选的一个方式的各向异性导电膜的截面图。
具体实施方式
以下以作为本发明的电连接材料的优选的一个方式的各向异性导电膜为例，详细地说明本发明。
<各向异性导电膜>
如图1所示，本发明的各向异性导电膜10具有用第1绝缘性热固型树脂组合物层2和第2绝缘性热固型树脂组合物层3夹持含有导电粒子的层1的结构。
(含有导电粒子的层1)
此含有导电粒子的层1是通过光照射使含有丙烯酸酯系自由基聚合性化合物、光自由基聚合引发剂、环氧系非自由基聚合性化合物和导电粒子的含有导电粒子的树脂组合物层光自由基聚合而乙阶化而得。在这里，“乙阶”指固化型树脂组合物为半固化的状态，且通过加热而流动或软化的状态。
作为含有导电粒子的层1的光自由基聚合前的前体，含有导电粒子的树脂组合物层含有丙烯酸酯系自由基聚合性化合物、光自由基聚合引发剂、环氧系非自由基聚合性化合物和导电粒子，但不含有使环氧系非自由基聚合性化合物聚合的聚合引发剂。其原因在于：通过在含有导电粒子的层1的两面层合的第1绝缘性热固型树脂组合物层2和第2绝缘性热固型树脂组合物层3的聚合，使环氧系非自由基聚合性化合物聚合。
在含有导电粒子的层1中，通过光照射产生的光自由基聚合中丙烯酸酯系自由基聚合性化合物的反应率优选为70%以上。若反应率为70%以上，则可充分地得到抑制连接时的粒子流动这样的效果。反应率的测定可通过FT-IR等公知的方法来进行。需说明的是，此反应率为100%的情况也是本申请发明的范围，但由于含有导电粒子的层1含有未聚合的环氧系非自由基聚合性化合物，所以作为含有导电粒子的层1整体可以说并不是真正固化状态，而是乙阶状态。
需说明的是，光照射条件(光源、光波长、光强度、光量、温度等)可适宜设定。
作为丙烯酸酯系自由基聚合性化合物，可列举出单官能或多官能(甲基)丙烯酸酯(在这里，(甲基)丙烯酸酯为包含丙烯酸酯和甲基丙烯酸酯的术语)化合物。作为单官能(甲基)丙烯酸酯化合物，可列举出(甲基)丙烯酸甲酯，(甲基)丙烯酸乙酯，(甲基)丙烯酸正丙酯或(甲基)丙烯酸异丙酯，(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸仲丁酯或(甲基)丙烯酸叔丁酯，(甲基)丙烯酸-2-乙基己酯，(甲基)丙烯酸苄酯，丙烯酸二环戊基酯化合物等。作为多官能(甲基)丙烯酸酯化合物，可示例出二(甲基)丙烯酸乙二醇酯、二(甲基)丙烯酸二甘醇酯、二(甲基)丙烯酸-1,6-己二醇酯、二(甲基)丙烯酸丙二醇酯、二(甲基)丙烯酸二丙二醇酯、二(甲基)丙烯酸-1,2-环己二醇酯、二(甲基)丙烯酸新戊二醇酯、二甲基丙烯酸双环戊二烯酯等2官能(甲基)丙烯酸酯化合物，或三(甲基)丙烯酸甘油酯、三羟甲基丙烷三(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、三(2-丙烯酰氧基乙基)异氰尿酸酯等3官能(甲基)丙烯酸酯化合物。另外，也可使用进行了环氧改性、氨基甲酸酯改性、环氧乙烷改性、环氧丙烷改性的化合物。其中，从固化后的连接稳定性的方面出发，可优选使用双酚A型环氧丙烯酸酯。
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选择来使用。例如，可列举出苯乙酮系光聚合引发剂、苯偶酰缩酮系光聚合引发剂、α-烷基氨基苯酮系光聚合引发剂、磷系光聚合引发剂等。具体而言，作为苯乙酮系光聚合引发剂，可列举出2-羟基-2-环己基苯乙酮(IRGACURE184，BASFJapan(Ltd.)(BASFジャパン(株)))、α-羟基-α,α’-二甲基苯乙酮(DAROCUR1173，BASFJapan(Ltd.))、2,2-二甲氧基-2-苯基苯乙酮(IRGACURE651，BASFJapan(Ltd.))、4-(2-羟基乙氧基)苯基(2-羟基-2-丙基)酮(IRGACURE2959，BASFJapan(Ltd.))、2-羟基-1-{4-[2-羟基-2-甲基-丙酰基]-苄基}苯基}-2-甲基-丙烷-1-酮(IRGACURE127，BASFJapan(Ltd.))等。作为苯偶酰缩酮系光聚合引发剂，可列举出二苯甲酮、芴酮、二苯并环庚酮、4-氨基二苯甲酮、4,4’-二氨基二苯甲酮、4-羟基二苯甲酮、4-氯二苯甲酮、4,4’-二氯二苯甲酮等。另外，作为α-烷基氨基苯酮系光聚合引发剂，可使用2-苄基-2-二甲基氨基-1-(4-吗啉代苯基)-丁酮-1(IRGACURE369，BASFJapan(Ltd.))。作为磷系光聚合引发剂，可列举出双(2,4,6-三甲基苯甲酰基)-苯基氧化膦(IRGACURE819，BASFJapan(Ltd.))、(2,4,6-三甲基苯甲酰基)-二苯基氧化膦(DAROCURETPO，BASFJapan(Ltd.))等。
相对于100质量份的丙烯酸酯系自由基聚合性化合物，光自由基聚合引发剂的掺混量优选为0.1~40质量份，更优选为0.5~30质量份。若为此范围，则可充分地进行光自由基聚合，抑制含有导电粒子的层1的机械强度的降低。
作为丙烯酸酯系自由基聚合性化合物与光自由基聚合引发剂的优选的组合，可列举出双酚A型环氧丙烯酸酯与α-烷基氨基苯酮系光聚合引发剂的组合。
作为环氧系非自由基聚合性化合物，可列举出以下化合物，所述化合物可为液态或固态，环氧当量通常为100~4000左右，在分子内不存在自由基聚合性的不饱和键，并且具有2个以上的环氧基。例如，可优选使用双酚A型环氧化合物、苯酚酚醛清漆型环氧化合物、甲酚酚醛清漆型环氧化合物、酯型环氧化合物、脂环型环氧化合物等。另外，在这些化合物中可含有单体或低聚物。
相对于100质量份的丙烯酸酯系自由基聚合性化合物，环氧系非自由基聚合性化合物的掺混量优选为3~250质量份，更优选为10~150质量份。若为此范围，则可提高粘接力，抑制过度的翘曲的变化。
需说明的是，在含有导电粒子的层1中，除了丙烯酸酯系自由基聚合性化合物和环氧系非自由基聚合性化合物以外，可含有苯氧树脂、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、聚烯烃树脂等作为成膜用树脂。相对于总和为100质量份的丙烯酸酯系自由基聚合性化合物和环氧系非自由基聚合性化合物，这样的成膜用树脂成分的掺混量优选为10~200质量份，更优选为20~150质量份。若为此范围，则可提高固化前的操作性，抑制也会导致翘曲的固化后的残余应力。
作为导电粒子，可采用公知的构成各向异性导电膜的导电粒子。例如，可列举出镍等金属粒子、在树脂芯核的表面形成有镍等金属镀膜的被覆金属的树脂粒子等。可根据需要形成绝缘薄膜。
作为这样的导电粒子的平均粒径，从导通保持性的方面出发，优选为1~20μm，更优选为2~10μm。
相对于总和为100质量份的丙烯酸酯系自由基聚合性化合物、环氧系非自由基聚合性化合物和根据需要掺混的成膜用树脂，导电粒子的掺混量优选为2~200质量份，更优选为5~150质量份。若为此范围，则可提高导通可靠性，抑制粘接性的过度降低或连接后的短路的产生。
从确保导通和防止短路的方面出发，含有导电粒子的层1的导电粒子密度优选为1000~150000个/mm2，更优选为2000~100000个/mm2。
需说明的是，作为含有导电粒子的层1中导电粒子的存在形态，可制成在含有导电粒子的树脂组合物中均匀地混合并成膜的形态，或使用公知的方法(例如转印模)制成以单层规则排列的形态。
含有导电粒子的层1的层厚度优选为1~20μm，更优选为2~10μm，进一步更优选为3~8μm。若为此范围，则不使粒子捕捉效率过于降低，也可抑制导通电阻的过度上升。
(第1绝缘性热固型树脂组合物层2和第2绝缘性热固型树脂组合物层3)
这些树脂组合物层各自独立地含有环氧系非自由基聚合性化合物和热阳离子聚合引发剂或热阴离子聚合引发剂。
作为环氧系非自由基聚合性化合物，可列举出以下化合物，所述化合物可为液态或固态，环氧当量通常为100~4000左右，在分子内不存在自由基聚合性的不饱和键，并且具有2个以上的环氧基。例如，可优选使用双酚A型环氧化合物、苯酚酚醛清漆型环氧化合物、甲酚酚醛清漆型环氧化合物、酯型环氧化合物、脂环型环氧化合物等。另外，在这些化合物中可含有单体或低聚物。作为特别优选的环氧系非自由基聚合性化合物，从固化后的连接稳定性的方面出发，为双酚A型环氧化合物。
作为热阳离子聚合引发剂，可使用引发环氧化合物的阳离子聚合的公知的热阳离子聚合引发剂，例如可使用公知的碘鎓盐、锍盐、鏻盐、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。作为热阳离子系聚合引发剂的优选的实例，可列举出二苯基碘鎓六氟锑酸盐、二苯基碘鎓六氟磷酸盐、二苯基碘鎓六氟硼酸盐、三苯基锍六氟锑酸盐、三苯基锍六氟磷酸盐、三苯基锍六氟硼酸盐。具体而言，可列举出(株)ADEKA制的SP-150、SP-170、CP-66、CP-77，日本曹达(株)制的CI-2855、CI-2639，三新化学工业(株)制的San-Aid(サンエイド)SI-60、SI-80，UnionCarbideCorporation(ユニオンカーバイド社)制的CYRACURE-UVI-6990、UVI-6974等。
若热阳离子聚合引发剂的掺混量过少，则有热阳离子聚合未充分地进行的趋势，若过多，则可能导致刚性降低，因此相对于100质量份的环氧系非自由基聚合性化合物，优选为0.1~40质量份，更优选为0.5~30质量份。
作为热阴离子聚合引发剂，可使用引发环氧化合物的阴离子聚合的公知的热阴离子聚合引发剂，例如可列举出脂族胺系化合物、芳族胺系化合物、仲胺或叔胺系化合物、咪唑系化合物、多硫醇系化合物、三氟化硼-胺络合物、双氰胺、有机酰肼等，可优选使用对温度显示良好的潜伏性的胶囊化咪唑系化合物。具体而言，可列举出AsahiKaseiE-materialsCorporation(旭化成イーマテリアルズ(株))制NOVACURE(ノバキュア)HX3941HP等。
若热阴离子聚合引发剂的掺混量过少，则有热阴离子聚合未充分地进行的趋势，若过多，则可能导致刚性降低，因此相对于100质量份的环氧系非自由基聚合性化合物，优选为0.1~200质量份，更优选为0.5~150质量份。
为了进一步抑制使用本发明的各向异性导电膜制备的连接体的翘曲的产生，优选第1绝缘性热固型树脂组合物层2与第2绝缘性热固型树脂组合物层3之间的固化收缩率差优选为10%以下。需说明的是，固化收缩率可依据JISK6901来测定。各层各自的固化收缩率优选为10%以内，更优选为5%以内，进一步更优选为3%以内。
第1绝缘性热固型树脂组合物层2和第2绝缘性热固型树脂组合物层3的层厚度各自优选为0.1~30μm，更优选为1~20μm。若为此范围，则不使粒子捕捉效率过于降低，也可抑制导通电阻的过度上升。
以上以各向异性导电膜为例说明本发明的电连接材料，但除了各向异性导电膜以外，本发明的电连接材料可采用各向异性导电糊剂、导电糊剂、导电膜等方式。
<电连接材料(优选各向异性导电膜)的制备方法>
本发明的各向异性导电膜等电连接材料可通过具有以下说明的工序1和工序2的制备方法来制备。
(工序1)
首先，将含有丙烯酸酯系自由基聚合性化合物、光自由基聚合引发剂、环氧系非自由基聚合性化合物和导电粒子的含有导电粒子的树脂组合物成膜，对得到的膜照射光进行光自由基聚合而乙阶化，由此形成含有导电粒子的层。
含有导电粒子的树脂组合物可通过以下方法来制备：通过公知的方法(例如行星混合机等)，将丙烯酸酯系自由基聚合性化合物、光自由基聚合引发剂、环氧系非自由基聚合性化合物、导电粒子和根据需要进行掺混的成膜成分等其它的成分同时均匀地混合。其成膜也可通过公知的方法(例如刮刀法等)来进行。在此情况下，在剥离处理基质片材(例如进行了剥离处理的聚酯片材)上将含有导电粒子的树脂组合物成膜，根据需要进行干燥，由此形成未固化状态的含有导电粒子的树脂组合物层。对于这样形成的含有导电粒子的树脂组合物层，照射紫外线等光，使丙烯酸酯系自由基聚合性化合物光自由基聚合，优选使得丙烯酸酯系自由基聚合性化合物的反应率为70%以上、优选90%以上。由此，形成乙阶化的含有导电粒子的层。
(工序2)
接着，在含有导电粒子的层的一面层合含有环氧系非自由基聚合性化合物和热阳离子聚合引发剂或热阴离子聚合引发剂的第1绝缘性热固型树脂组合物层，并在另一面层合含有环氧系非自由基聚合性化合物和热阳离子聚合引发剂或热阴离子聚合引发剂的第2绝缘性热固型树脂组合物层。由此，得到本发明的各向异性导电膜等电连接材料。
第1绝缘性热固型树脂组合物层和第2绝缘性热固型树脂组合物层可如下制备。首先，通过公知的方法(例如行星混合机等)将环氧系非自由基聚合性化合物、热阳离子聚合引发剂或热阴离子聚合引发剂和根据需要进行掺混的成膜成分等其它的成分同时均匀地混合，由此各自制备绝缘性热固型树脂组合物。通过公知的方法(例如刮刀法等)，将此树脂组合物在剥离处理基质片材上成膜，根据需要进行干燥，由此制备未固化状态的第1绝缘性热固型树脂组合物层和第2绝缘性热固型树脂组合物层。
接着，在之前形成的含有导电粒子的层上重叠第1绝缘性热固型树脂组合物层并进行压接。接着，剥下含有导电粒子的层侧的剥离基质片材，重叠第2绝缘性热固型树脂组合物层，将得到的层合物压接，由此得到本发明的各向异性导电膜等电连接材料。需说明的是，通过用第1绝缘性热固型树脂组合物层和第2绝缘性热固型树脂组合物层夹持从剥离处理基质片材剥下的含有导电粒子的层，并将得到的层合物压接，也可得到本发明的各向异性导电膜等电连接材料。
<连接体>
本发明的各向异性导电膜等电连接材料可在第1电气部件(例如IC芯片)的端子(例如凸点)与第2电气部件(例如布线基板)的端子(例如凸点、焊盘)之间配置，从第1或第2电气部件侧通过热压接来进行电连接、优选各向异性导电连接，由此提供连接体。
实施例
以下通过实施例具体地说明本发明。
实施例1~7、比较例1~4
(第1绝缘性热固型树脂组合物层的形成)
依据表1所示的配方(单位：质量份)，使用甲苯制备固体成分为50%的第1绝缘性热固型树脂组合物混合液，将此混合液涂布于剥离PET基质片材上，使得干燥厚度为8μm，于80℃干燥5分钟，由此形成第1绝缘性热固型树脂组合物层。
(第2绝缘性热固型树脂组合物层的形成)
依据表1所示的配方(单位：质量份)，使用甲苯制备固体成分为50%的第2绝缘性树脂组合物混合液，将此混合液涂布于剥离PET基质片材上，使得干燥厚度为8μm，于80℃干燥5分钟，由此形成第2绝缘性热固型树脂组合物层。
(含有导电粒子的层的形成)
依据表1所示的配方(单位：质量份)，使用甲苯制备固体成分为50%的含有导电粒子的树脂组合物混合液，将此混合液涂布于剥离PET基质片材上，使得干燥厚度为6μm，于80℃干燥5分钟，接着，照射紫外线使得为表1的累积光量以进行光自由基聚合，由此形成含有导电粒子的层。使用FT-IR(FT/IR-4100，日本分光(株))测定此含有导电粒子的层中丙烯酸酯系自由基聚合性化合物的反应率，将得到的结果示出于表1中。
(各向异性导电膜的制备)
在第1绝缘性热固型树脂组合物层上重叠含有导电粒子的层并进行层合后，剥下含有导电粒子的层侧的剥离PET基质片材，露出含有导电粒子的层。在此露出的含有导电粒子的层上重叠第2绝缘性热固型树脂组合物层，从剥离PET基质片材上方，以40℃、0.1Pa的条件进行层合，由此得到各向异性导电膜。
<连接体的评价>
(连接体的制备)
使用在各实施例和比较例中制备的各向异性导电膜，通过热压接将IC芯片的凸点与玻璃基板的ITO图案电极之间各向异性导电连接。需说明的是，在进行各向异性连接时将第一绝缘性树脂组合物层配置于IC芯片侧。
热压接条件：180℃，80MPa，5秒
IC芯片的尺寸：1.5mm×20mm，0.5mmt
IC芯片的凸点：镀金凸点，30μm×85μm，凸点高度为15μm，凸点间距为50μm
设置有厚度为200nm的ITO图案电极的玻璃基板的尺寸：50mm×30mm，0.3mmt(1737F，CorningIncorporated(コーニング社))。
(性能评价)
对于得到的连接体，如以下说明那样，对“初期导通电阻”、“高温高湿负荷试验后的导通电阻(导通可靠性)”、“连接体的翘曲”进行测定。将得到的结果示出于表1中。
“初期导通电阻”
使用市售的电阻测定仪测定刚制备之后的连接体的初期导通电阻。在实际使用上希望为10Ω以下。
“高温高湿负荷试验后的导通电阻(导通可靠性)”
使用市售的电阻测定仪测定将连接体在维持于85℃、85%Rh的室中放置1000小时后的连接体的导通电阻。在实际使用上希望为15Ω以下。
“连接体的翘曲”
对于连接体的翘曲，使用市售的三维形状测定系统(KeyenceCorporation((株)キーエンス))测定相当于IC芯片背面的宽度为20mm的未安装IC芯片的一侧的玻璃基板表面。希望翘曲为10μm以内。
[表1]
。
<考察>
实施例1~7的各向异性导电膜的导通可靠性优异，并且翘曲也少。需说明的是，根据因丙烯酸酯的掺混量较少而刚性较低的实施例4的各向异性导电膜和因反应率较低而刚性较低的实施例6的各向异性导电膜的结果可知，各向异性导电膜的刚性较低的连接体难以翘曲。反之，可知在刚性较高的实施例5或实施例7的各向异性导电膜的情况下变得容易翘曲。
与之相对的是，在比较例1、2、4的情况下，由于未进行针对含有导电粒子的层的光照射，所以导通可靠性有问题。在比较例3的情况下，虽然也进行了针对含有导电粒子的层的光照射，但由于不含有光自由基聚合引发剂，所以导通可靠性有问题。另外，由于含有热自由基聚合引发剂，所以在进行各向异性导电连接时会立即固化，并大幅地翘曲。
产业上的可利用性
根据本发明的各向异性导电膜等电连接材料，抑制在各向异性导电连接部等电连接部产生翘曲，而且不降低通过各向异性导电连接等电连接而得到的连接体的导通可靠性。因此，本发明的各向异性导电膜在将IC芯片等电气部件倒装安装于布线基板等其它的电机部件时有用。
符号说明
1含有导电粒子的层
2第1绝缘性热固型树脂组合物层
3第2绝缘性热固型树脂组合物层

Claims (8)

1.电连接材料，其为用第1绝缘性热固型树脂组合物层和第2绝缘性热固型树脂组合物层夹持含有导电粒子的层而得的电连接材料，其特征在于：
含有导电粒子的层是通过光照射使含有丙烯酸酯系自由基聚合性化合物、光自由基聚合引发剂、环氧系非自由基聚合性化合物和导电粒子的含有导电粒子的树脂组合物层光自由基聚合而乙阶化，
第1绝缘性热固型树脂组合物层和第2绝缘性热固型树脂组合物层各自含有环氧系非自由基聚合性化合物和热阳离子聚合引发剂或热阴离子聚合引发剂。
2.权利要求1的电连接材料，其中，在含有导电粒子的层中，丙烯酸酯系自由基聚合性化合物的反应率为70%以上。
3.权利要求1或2的电连接材料，其中，丙烯酸酯系自由基聚合性化合物为双酚A型环氧丙烯酸酯，光自由基聚合引发剂为α-烷基氨基苯酮系光聚合引发剂。
4.权利要求1~3中任一项的电连接材料，其中，环氧系非自由基聚合性化合物为双酚A型环氧化合物，热阳离子聚合引发剂为芳族锍盐。
5.权利要求1~4中任一项的电连接材料，其中，第1绝缘性热固型树脂组合物层与第2绝缘性热固型树脂组合物层之间的固化收缩率差为10%以下。
6.制备方法，其为权利要求1的电连接材料的制备方法，其具有：
将含有丙烯酸酯系自由基聚合性化合物、光自由基聚合引发剂、环氧系非自由基聚合性化合物和导电粒子的含有导电粒子的树脂组合物成膜，对得到的膜照射光进行光自由基聚合而乙阶化，由此形成含有导电粒子的层的工序；和
在含有导电粒子的层的一面层合含有环氧系非自由基聚合性化合物和热阳离子聚合引发剂或热阴离子聚合引发剂的第1绝缘性热固型树脂组合物层，并在另一面层合含有环氧系非自由基聚合性化合物和热阳离子聚合引发剂或热阴离子聚合引发剂的第2绝缘性热固型树脂组合物层的工序。
7.权利要求6的制备方法，其中，对于含有导电粒子的树脂组合物的膜，照射光使得丙烯酸酯系自由基聚合性化合物的反应率为70%以上。
8.连接体，其为通过权利要求1~5中任一项的电连接材料将第1电气部件的端子与第2电气部件的端子通过热压接电连接而成。
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