CN103459453A - 各向异性导电膜 - Google Patents

各向异性导电膜 Download PDF

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Publication number
CN103459453A
CN103459453A CN2012800183637A CN201280018363A CN103459453A CN 103459453 A CN103459453 A CN 103459453A CN 2012800183637 A CN2012800183637 A CN 2012800183637A CN 201280018363 A CN201280018363 A CN 201280018363A CN 103459453 A CN103459453 A CN 103459453A
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Prior art keywords
epoxy resin
anisotropic conductive
conductive film
electronic unit
terminal
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CN2012800183637A
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CN103459453B (zh
Inventor
出口真吾
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Dexerials Corp
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Dexerials Corp
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R4/00—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation
    • H01R4/04—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation using electrically conductive adhesives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
    • C08G59/687—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used containing sulfur
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/24—Electrically-conducting paints
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    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/10—Adhesives in the form of films or foils without carriers
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    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02—Electrically-conducting adhesives
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    • C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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Abstract

在包含环氧树脂、环氧树脂用固化剂和膜形成用树脂的热固型环氧树脂组合物中分散导电性颗粒而成的各向异性导电膜中，作为其环氧树脂，使用以质量比9:1~2:8的比例含有β-烷基缩水甘油基型环氧树脂和缩水甘油基醚型环氧树脂的环氧树脂。作为β-烷基缩水甘油基型环氧树脂，优选为间苯二酚二（β-甲基缩水甘油基）醚，作为缩水甘油基醚型环氧树脂，优选为氧化烯改性缩水甘油基醚型环氧树脂。

Description

各向异性导电膜
技术领域
本发明涉及在热固型环氧树脂组合物中分散有导电性颗粒的各向异性导电膜。
背景技术
将IC芯片连接于布线基板时，广泛使用了以材料成本较低的、通用的缩水甘油基醚型环氧树脂作为主要固化成分的各向异性导电膜（ACF），但对于这种各向异性导电膜，要求连接可靠性良好是理所当然的，从防止因热而导致IC芯片的性能劣化、降低各向异性导电连接成本的观点出发，要求低温快速固化性，进而从昂贵的IC芯片、布线基板的有效利用的观点出发，还要求显示良好的可修复性（リペア性）以及材料成本低。
另外，通用的缩水甘油基醚型环氧树脂在环氧树脂材料之中是能够期待一定程度的连接可靠性、且材料成本较低的环氧树脂，但反应性不能说充分，因此不得不将其固化温度设定为约170℃以上，难以说低温快速固化性是充分的，且交联密度过高，因此存在不会显示充分可修复性的问题。
因此，作为解决这些课题的探讨，尝试了作为固化剂使用与现有通常的阴离子系固化剂相比能够期待迅速的固化反应的阳离子系固化剂（专利文献1）；使用反应性更高的脂环式环氧树脂来代替缩水甘油基醚型环氧树脂（专利文献2）。
现有技术文献
专利文献
专利文献1：日本特开2009-275102号公报
专利文献2：日本特开2007-238751号公报。
发明内容
发明要解决的课题
然而，使用阳离子系固化剂时，能够实现低温快速固化性的改善，但依然存在可修复性不充分的问题。另外，与缩水甘油基醚型环氧树脂相比，在使用阳离子系固化剂的基础上使用脂环式环氧树脂时，低温快速固化性进一步被改善，但材料成本高，另外，存在可修复性依然不充分、作为各向异性导电膜的保存稳定性降低的问题。进而，由于与缩水甘油基醚型环氧树脂相比更具有疏水性，因此存在对被粘接体的粘接力在进行了高温高湿条件下的熟化处理（エージング処理）后降低、连接可靠性也随之降低的倾向。
本发明是要解决以上现有技术课题而进行的，其目的在于提供如下各向异性导电膜，其在使用阳离子系固化剂的环氧树脂基质的各向异性导电膜中不使用脂环式环氧树脂，即使使用材料成本较低的通用缩水甘油基醚型环氧树脂或其衍生物，低温快速固化性和可修复性两者也均优异，进而连接可靠性和保存稳定性也优异。
解决问题的技术手段
本发明人等尝试了对于在含有阳离子系固化剂作为固化剂的热固型环氧树脂组合物中分散导电性颗粒而成的各向异性导电膜，尤其是为了改善其低温快速固化性，作为构成热固型环氧树脂组合物的环氧树脂，除了通用的缩水甘油基醚型环氧树脂之外，还组合使用环氧环的β位具有能够通过立***阻来阻碍环氧树脂的阴离子聚合的烷基的β-烷基缩水甘油基型环氧树脂时，结果发现与阴离子聚合体系的情况不同，阳离子聚合体系出乎意料地改善了低温快速固化性，更令人惊讶的是，可修复性也得到改善，连接可靠性和保存稳定性也优异，从而完成了本发明。
即，本发明提供各向异性导电膜，其为在包含环氧树脂、作为环氧树脂用固化剂的阳离子系固化剂和膜形成用树脂的热固型环氧树脂组合物中分散有导电性颗粒的各向异性导电膜，
该环氧树脂以质量比9:1~2:8的比例含有β-烷基缩水甘油基型环氧树脂和缩水甘油基醚型环氧树脂。
另外，本发明提供制造方法，其为利用各向异性导电膜将第一电子部件的端子与第二电子部件的端子进行了各向异性导电连接的连接结构体的制造方法，该制造方法具备如下工序：
在第一电子部件的端子上临时粘贴前述本发明的各向异性导电膜的工序；
在进行了临时粘贴的各向异性导电膜上将第二电子部件以其端子与第一电子部件的相应端子相对的方式进行临时设置的工序；以及
将第二电子部件边用加热焊接机加热边向第一电子部件按压，将第一电子部件的端子与第二电子部件的端子各向异性导电连接的工序。
另外，本发明提供连接结构体，其是利用前述本发明的各向异性导电膜将第一电子部件的端子与第二电子部件的端子进行各向异性导电连接而成的。
发明效果
使用阳离子系固化剂的本发明的环氧树脂基质的各向异性导电膜中，作为成为导电性颗粒的分散介质的、构成热固型环氧树脂组合物的环氧树脂，以特定比例组合使用β-烷基缩水甘油基型环氧树脂和缩水甘油基醚型环氧树脂。β-烷基缩水甘油基型环氧树脂由于具有可以认为能够使阳离子种稳定化的叔碳，结果可以改善各向异性导电膜的低温快速固化性，而且还可以同时改善可修复性、连接可靠性和保存稳定性，所述叔碳是通过接受源自阳离子系聚合引发剂的阳离子种的攻击、使环氧环开环而形成的。
附图说明
图1是连接结构体的制造工序说明图。
图2是接着图1的连接结构体的制造工序说明图。
图3是接着图2的连接结构体的制造工序说明图。
图4是连接结构体的概略剖面图。
具体实施方式
本发明是在包含环氧树脂、环氧树脂用固化剂和膜形成用树脂的热固型环氧树脂组合物中分散有导电性颗粒的各向异性导电膜。
构成本发明的各向异性导电膜的热固型环氧树脂组合物成为导电性颗粒的分散介质，作为整体而形成膜，针对被粘接体在固化前发挥粘合力、在固化后发挥粘接力，如上所述，其含有环氧树脂、环氧树脂用固化剂和膜形成用树脂。
本发明中，热固型环氧树脂组合物所含有的环氧树脂为热固化成分，含有β-烷基缩水甘油基型环氧树脂和缩水甘油基醚型环氧树脂。由此，各向异性导电膜，与不使用β-甲基缩水甘油基型环氧树脂而使用由通用的缩水甘油基醚型环氧树脂构成的热固型环氧树脂组合物的各向异性导电膜相比，不仅能够改善低温快速固化性，还能够改善可修复性，进而能够实现良好的连接可靠性和保存稳定性。
β-烷基缩水甘油基型环氧树脂是指用以下的通式（1）表示的化合物。
式（1）中，Y为甲基、乙基、丙基、异丙基、丁基、异丁基、戊基、己基、环己基等烷基，其中，从获取容易性的观点出发，优选为甲基。X为-O-、-NH-或-OCO-基。其中，从合成容易性的观点出发，优选为-O-。另外，n为2以上的数。R为芳香族、脂肪族或脂环式多元醇化合物残基；芳香族、脂肪族或脂环式多胺化合物残基；或者芳香族、脂肪族或脂环式聚羧酸化合物残基。其中，从获取容易性的观点出发，优选为芳香族、脂肪族或脂环式多元醇化合物残基，特别优选为芳香族多元醇化合物残基。此处，式（1）的化合物是使β-烷基环氧氯丙烷与多元醇化合物、多胺化合物或聚羧酸化合物发生脱氯化氢反应而制备的，由于脱氯化氢反应是逐渐进行的，因此β-烷基缩水甘油基型环氧树脂中包含单体类型、预聚物类型（缩合物）。这种预聚物类型的化合物的优选例子示于式（2）。此处，m为1~20的数。
Figure 398033DEST_PATH_IMAGE002
作为这种芳香族、脂肪族或脂环式多元醇化合物，可列举出间苯二酚、4,4'-二羟基联苯、双酚A、双酚F、1,6-己二醇、1,4-丁二醇、环己烷-1,3-二醇等。作为芳香族、脂肪族或脂环式多胺化合物，可列举出邻苯二胺、间苯二胺、对苯二胺、1,6-己二胺、1,4-丁二胺、环己烷-1,3-二胺等。作为芳香族、脂肪族或脂环式聚羧酸化合物，可列举出邻苯二甲酸、间苯二甲酸、对苯二甲酸、己二酸、琥珀酸等。
作为式（1）的β-烷基缩水甘油基型环氧树脂的优选具体例，可列举出间苯二酚二（β-烷基缩水甘油基）醚、双酚A型二（β-烷基缩水甘油基）醚、双酚F型二（β-烷基缩水甘油基）醚等。其中，从能够改善各向异性导电膜的低温快速固化性的观点出发，优选为间苯二酚二（β-烷基缩水甘油基）醚，特别优选为间苯二酚二（β-甲基缩水甘油基）醚。需要说明的是，该间苯二酚二（β-甲基缩水甘油基）醚可以是单体类型，也可以是预聚物类型。
另一方面，作为与β-烷基缩水甘油基型环氧树脂组合使用的缩水甘油基醚型环氧树脂，是缩水甘油基中不存在烷基等取代基的环氧树脂，可以优选地使用通用的缩水甘油基醚型环氧树脂，尤其优选使用氧化烯改性（优选为2摩尔以上的氧化烯改性）缩水甘油基醚型环氧树脂。作为这种缩水甘油基醚型环氧树脂，可列举出双酚A型二缩水甘油基醚及其预聚物（缩合物）、双酚F型二缩水甘油基醚及其预聚物（缩合物）、线型酚醛型二缩水甘油基醚等。其中，从能够对各向异性导电膜赋予良好的粘接强度的观点出发，可以优选地使用环氧乙烷或环氧丙烷改性双酚A型二缩水甘油基醚。
热固型环氧树脂组合物所含有的环氧树脂以质量比9:1~2:8、优选为8:2~4:6的比例含有上述的β-烷基缩水甘油基型环氧树脂和缩水甘油基醚型环氧树脂。与该质量比范围相比β-烷基缩水甘油基型环氧树脂的含量多时，存在各向异性导电膜的连接可靠性降低的倾向，相反变少时，存在其可修复性难以改善的倾向。
本发明中，作为热固型环氧树脂组合物所含有的环氧树脂，可以在不损害本发明的效果的范围内组合使用除了β-烷基缩水甘油基型环氧树脂和缩水甘油基醚型环氧树脂以外的其它环氧树脂，例如3,4-环氧环己基甲基-3,4-环氧环己烷羧酸酯等脂环式环氧树脂。
构成本发明的各向异性导电膜的热固型环氧树脂组合物中，作为环氧树脂用固化剂，使用已知对改善低温快速固化性而言有效的阳离子系固化剂。作为这种阳离子系固化剂，可以使用公知的固化剂，例如可以使用芳基重氮盐系固化剂、芳基碘鎓盐系固化剂、芳基硫鎓盐系固化剂、丙二烯-离子络合物（アレン－イオン錯体）系固化剂、金属（例如，铝、钛、锌、锡等）与乙酰乙酸酯或二酮类的螯合物系固化剂等。尤其是，从低温下的反应性优异、有效期（ポットライフ）长的观点出发，优选使用芳基硫鎓盐系固化剂。
作为本发明中能够适合地使用的芳基硫鎓盐系固化剂，可例示出以下的式（3）~（6）所示结构的固化剂。
Figure 145147DEST_PATH_IMAGE003
式（3）中，Ra为氢原子、COCH3基或COOCH3基，Rb和Rc分别为氢原子、卤素原子或C1~C4的烷基，Rd为氢原子、CH3基、OCH3基或卤素原子，Re为C1~C4的烷基，X为SbF6、AsF6、PF6或BF4。
Figure 540356DEST_PATH_IMAGE004
式（4）中，Rf为氢原子、乙酰基、甲氧基羰基、甲基、环氧基羰基、叔丁氧基羰基、苯甲酰基、苯氧基羰基、苄氧基羰基、9-芴基甲氧基羰基或对甲氧基苄基羰基，Rg和Rh分别为氢原子、卤素原子或C1~C4的烷基，Ri和Rj分别为氢原子、甲基、甲氧基或卤素原子，X为SbF6、AsF6、PF6或BF4。
Figure 823570DEST_PATH_IMAGE005
式（5）中，Rk为乙氧基、苯基、苯氧基、苄氧基、氯甲基、二氯甲基、三氯甲基或三氟甲基，Rl和Rm分别为氢原子、卤素原子或C1~C4的烷基，Rn为氢原子、甲基、甲氧基或卤素原子，Ro为C1~C4的烷基，X为SbF6、AsF6、PF6或BF4。
Figure 646032DEST_PATH_IMAGE006
式（6）中，Rp为氢原子、乙酰基、甲氧基羰基、甲基、环氧基羰基、叔丁氧基羰基、苯甲酰基、苯氧基羰基、苄氧基羰基、9-芴基甲氧基羰基或对甲氧基苄基羰基，Rq和Rr分别为氢原子、卤素原子或C1~C4的烷基，Rs和Rt分别为甲基或乙基，X为SbF6、AsF6、PF6或BF4。
作为本发明中能够使用的市售阳离子系固化剂的具体例，例如可列举出芳基重氮盐[例如，PP-33（（株）ADEKA制）]、芳基碘鎓盐、芳基硫鎓盐[例如，FC-509、FC-540（3M公司制）、UVE1014（G.E.公司制）、UVI-6974、UVI-6970、UVI-6990、UVI-6950（ユニオン?カーバイド公司制）、SP-170、SP-150、CP-66、CP-77等（ADEKA公司制）]、SI-60L、SI-80L、SI-100L、SI-110L（三新化学工业株式会社制）、丙二烯-离子络合物[例如，CG-24-61（BASF公司制）]。
热固型环氧树脂组合物中的阳离子系固化剂的用量过少时，存在产生固化不良的倾向，而过多时存在保存稳定性降低的倾向。另外，通过以该范围进行使用，能够获得耐热性、透明性、耐候性等良好的固化物，因此优选相对于环氧树脂100质量份为1~30质量份、更优选为1~10质量份。
作为含有构成本发明的各向异性导电膜的热固型环氧树脂组合物的膜形成用树脂，可以优选地使用能够适用于公知的各向异性导电膜的膜形成用树脂的热塑性树脂。作为这种膜形成用树脂，优选与热固型环氧树脂组合物的环氧树脂相容的树脂，例如可以使用苯氧基树脂、聚酯树脂、聚氨酯树脂、聚酰胺树脂、聚酰亚胺树脂、聚烯烃树脂等，可以组合使用它们的两种以上。这些之中，从材料成本、成膜性、加工性、连接可靠性等观点出发，可以优选地使用苯氧基树脂。
构成本发明的各向异性导电膜的热固型环氧树脂组合物中的膜形成用树脂的配混量过少时，存在膜形成性降低的倾向，而过多时存在流动性降低的倾向，因此相对于环氧树脂100质量份，优选为40~200质量份，更优选为50~150质量份。
作为构成本发明的各向异性导电膜的导电性颗粒，可以采用公知的各向异性导电膜中使用的导电性颗粒。例如可列举出镍、钴、银、铜、金、钯等金属颗粒、金属被覆树脂颗粒等，可以组合使用它们的两种以上。它们的颗粒形状和粒径可以根据各向异性导电膜的使用环境、使用目的等来适当决定。
关于这种导电性颗粒相对于热固型环氧树脂组合物的配混比例，导电性颗粒过少时，存在难以进行稳定的各向异性导电连接的倾向，而过多时，膜的平面方向容易产生导电性颗粒的导通，因此相对于热固型环氧树脂组合物（即除了导电性颗粒以外的环氧树脂、环氧树脂用固化剂和膜形成用树脂的合计）100质量份，优选为0.1~50质量份、更优选为0.1~30质量份。
构成本发明的各向异性导电膜的热固型环氧树脂组合物中，还可以根据需要含有溶剂、公知的硅烷偶联剂、着色剂、阻燃剂、填充剂、聚丁二烯颗粒等应力缓和剂等添加剂。
本发明的各向异性导电膜可以通过按照常规方法将热固型环氧树脂组合物和导电性颗粒以及其他添加剂均匀地混合而制备各向异性导电膜形成用组合物，并用压延法、流延法等公知的成膜方法将该组合物制成膜，从而制造，所述热固型环氧树脂组合物包含：以质量比9:1~2:8的比例含有β-烷基缩水甘油基型环氧树脂和缩水甘油基醚型环氧树脂的环氧树脂、环氧树脂用固化剂以及膜形成用树脂。需要说明的是，也可以将除了导电性颗粒以外的成分预先均匀地混合而制备热固型环氧树脂组合物，按照常规方法向该组合物中均匀地分散导电性颗粒，从而制备各向异性导电膜形成用组合物。
这样操作而得到的各向异性导电膜的厚度可以根据各向异性导电膜的使用形态等来适当决定。
本发明的各向异性导电膜可以在制造将形成于第一电子部件的单面的端子与形成于第二电子部件的单面的端子各向异性导电连接的连接结构体时优选地适用。以下针对具备工序（a）~（c）的、使用本发明的各向异性导电膜的连接结构体的制造方法，分工序进行说明。
＜工序（a）＞
如图1所示，在第一电子部件10的端子11上临时粘贴本发明的各向异性导电膜20。临时粘贴使用后述的加热焊接机40（参照图3），可以通过边将各向异性导电膜20加热至不会热固化但表现出粘合性的温度边按压来进行。各向异性导电膜20中分散有导电性颗粒21。
作为第一电子部件10，可列举出玻璃布线基板、刚性布线基板、挠性布线基板等。作为端子11，可列举出在第一电子部件10的单面由铜、镍、铝、金等金属或铟-钛氧化物等复合氧化物按照常规方法形成的端子。另外，端子11的厚度、布线间距可以根据第一电子部件10的使用目的等来适当决定。
＜工序（b）＞
接着，如图2所示，在进行了临时粘贴的各向异性导电膜20上将第二电子部件30以其端子31与第一电子部件10的相应端子11相对的方式进行临时设置。临时设置使用后述的加热焊接机40（参照图3），可以通过边将各向异性导电膜20加热至不会热固化但表现出粘合性的温度边按压来进行。该临时设置时，在第二电子部件30或各向异性导电膜20产生位置偏移的情况下，根据需要，例如可以用热板将第一电子部件10侧加热而使各向异性导电膜20软化，按照常规方法剥离第二电子部件30，将第一电子部件10或第二电子部件30的表面残留的热固型环氧树脂组合物用丙酮等有机溶剂去除。由此能够实现良好的可修复性。
作为第二电子部件30，可列举出半导体芯片、电容器、LED芯片、挠性布线基板等。作为端子31，可列举出在第二电子部件30的单面由铜、镍、铝、金、焊锡等金属按照常规方法形成的电极（例如凸块）。另外，端子31的厚度、布线间距可以根据第二电子部件30的使用目的等来适当决定。
＜工序（c）＞
接着，如图3所示，将第二电子部件30边用加热焊接机40加热边向第一电子部件10按压。由此，端子11和端子31所夹持的导电性颗粒21被压碎，第一电子部件10的端子11和第二电子部件30的端子31之间实现电导通。由此，如图4所示，能够获得利用各向异性导电膜20将第一电子部件10的端子11与第二电子部件30的端子31进行各向异性导电连接的连接结构体100。
需要说明的是，作为该工序（c）中使用的加热焊接机40，可以使用在制造半导体装置时使用的公知的加热焊接机。另外，作为加热加压条件，可以按照要使用的各向异性导电膜的特性来适当决定。
作为如此操作而得到的连接结构体100的具体例，可列举出半导体装置、液晶显示装置、LED照明装置等。该连接结构体100也是本发明的一个方式。需要说明的是，连接结构体100中，各向异性导电膜20已经被热固化。
实施例
以下，通过实施例来具体说明本发明的各向异性导电膜。
实施例1~12、比较例1~7
＜各向异性导电膜的作成＞
使用搅拌装置以表1和表2的配混比例（质量份基准）将热塑性树脂（苯氧基树脂）、β-甲基缩水甘油基型环氧树脂A、缩水甘油基醚型环氧树脂B、硅烷偶联剂、阳离子系固化剂、应力缓和剂（聚丁二烯颗粒）和导电性颗粒均匀地混合，在剥离膜上以干燥厚度达到20μm的方式进行涂布，在70℃的干燥机中进行干燥，从而制作了各向异性导电膜。
＜各向异性导电膜的评价＞
针对实施例1~12、比较例1~7中得到的各向异性导电膜，按照以下说明的那样，试验评价了使差示扫描量热分析（DSC）（放热起始温度、放热峰温度、放热量减少率）、热压接条件发生变化而制作的连接结构体（覆晶薄膜（COF）基材与玻璃基板的各向异性导电连接体）的连接电阻、粘接强度和可修复性。所得结果示于表1和表2。
（差示扫描量热分析）
1）DSC
使用DSC装置（DSC-60、岛津制作所制）对各向异性导电膜进行热分析，测定放热起始温度（℃）、放热峰温度（℃）。实用上考虑到低温快速固化性和保存性，希望放热起始温度为90~110℃，另外，希望放热峰温度为100~130℃。
2）DSC放热量减少率
针对制造刚完成后、或者以30℃放置1个月、2个月或3个月的各向异性导电膜，使用DSC装置（DSC-60、岛津制作所制）进行热分析，测定总放热量（j/g），算出以30℃放置1个月、2个月或3个月的各向异性导电膜的总放热量相对于制造刚结束后的各向异性导电膜的总放热量的减少率（%）。实用上希望1个月后的减少率（%）为35%以下。
（连接电阻测定）
作为评价用基材，准备了覆晶薄膜（COF）基材（在38μm厚的聚酰亚胺膜表面形成有50μm间距的Cu8μm厚-Sn镀敷电极线的基材）、以及形成有由铟锡复合氧化物（ITO）形成的固体电极（ベタ電極）的玻璃基板。
接着，使用工具宽度（ツール幅）为1.5mm的压接机，在ITO实心玻璃基板的规定位置，将切削成1.5mm的各向异性导电膜隔着缓冲材料为150μm厚的特氟隆（注册商标）制的缓冲材料，以70℃、1MPa、1sec这一条件进行临时粘贴。
接着，使用相同压接机在进行过临时粘贴的各向异性导电膜上以80℃、0.5MPa、0.5sec这一条件临时设置COF基材。
进而，确认COF基材与玻璃基板之间未产生位置偏移后，使用相同压接机以表1或表2所示的条件（150℃、160℃或170℃、4MPa、5秒）进行主压接，制作了连接结构体。
将所得连接结构体在85℃和85%RH的环境下放置500小时。然后针对刚放置500小时后的连接结构体，使用数字万用表（横河电机株式会社制）测定连接电阻值。另外，同样地测定在85℃和85%RH的环境下放置500小时后、进而以30℃保存1个月、保存2个月或保存3个月后的连接结构体的连接电阻值。实用上期望测定值为2Ω以下。
（粘接强度测定）
制作与测定连接电阻值时制作的连接结构体相同的连接结构体，在85℃和85%RH的环境下放置500小时。接着，使用拉伸试验机（AND公司制）将连接结构体的COF基材以拉伸速度50mm/sec向90°方向剥离，测定此时的剥离强度来作为粘接强度。实用上希望为6N/cm以上。
（可修复性试验）
作为评价用基材，准备了覆晶薄膜（COF）基材（在38μm厚的聚酰亚胺膜表面形成有50μm间距的Cu8μm厚-Sn镀敷电极线的基材）、以及形成有由铟锡复合氧化物（ITO）形成的固体电极的玻璃基板。
接着，使用工具宽度为1.5mm的压接机，在ITO实心玻璃基板的规定位置，将切削成1.5mm的各向异性导电膜隔着缓冲材料为150μm厚的特氟隆（注册商标）制的缓冲材料，以70℃、1MPa、1sec这一条件进行临时粘贴。
接着，使用相同压接机在进行过临时粘贴的各向异性导电膜上以80℃、0.5MPa、0.5sec这一条件临时设置COF基材得到层叠体。
将该临时设置有COF基材的层叠体以其玻璃基板侧在温度加热至100℃的热板上载置30秒后，将COF基材从玻璃基板剥下，将COF基材或玻璃基材上残存的各向异性导电膜的热固型环氧树脂组合物用浸渗有丙酮的棉棒擦拭，对到树脂组合物被全部擦掉为止的擦拭次数进行计数。实用上希望为30次以下。
需要说明的是，表1和表2中使用的材料如下所示。  
＊1 苯氧基树脂（JER-4210、三菱化学公司）
＊2使1摩尔的双酚A与2摩尔的β-甲基环氧氯丙烷反应而成的产物
＊3使 1摩尔的间苯二酚与2摩尔的β-甲基环氧氯丙烷反应而成的产物
＊4 jER-828、三菱化学公司
＊5 EP-4100S、ADEKA公司
＊6 平均粒径为0.5μm的聚丁二烯颗粒（RKB、レジナス化成公司）
＊7 KBM-403、信越化学工业株式会社
＊8 芳基硫鎓盐系固化剂（SI-60、三新化学工业株式会社）＋3%稳定剂（对羟基苯基二甲基锍甲基硫酸酯）
＊9 芳基硫鎓盐系固化剂（SI-60、三新化学工业株式会社）＋5%稳定剂（对羟基苯基二甲基锍甲基硫酸酯）
＊10 芳基硫鎓盐系固化剂（SI-60、三新化学工业株式会社）＋8%稳定剂（对羟基苯基二甲基锍甲基硫酸酯）
＊11 芳基硫鎓盐系固化剂（SI-80、三新化学工业株式会社）＋3%稳定剂（对羟基苯基二甲基锍甲基硫酸酯）
＊12 ブライトGNR、日本化学工业株式会社
＊13 CEL2021P、ダイセル公司。
[表1]
Figure 913065DEST_PATH_IMAGE007
[表2]
Figure 580807DEST_PATH_IMAGE008
由表1可知，实施例1~12的各向异性导电膜中，作为环氧树脂，以质量比9:1~2:8的比例含有通常的缩水甘油基醚型环氧树脂和β-烷基缩水甘油基型环氧树脂，因此DSC的放热起始温度、放热峰温度没有问题，而且低温快速固化性得到改善，且可修复性、连接可靠性和保存稳定性也同时得到改善。
与此相对，表2的比较例1的各向异性导电膜中，作为环氧树脂，不使用β-烷基缩水甘油基型环氧树脂，仅使用了通常的缩水甘油基醚型环氧树脂，因此在150℃-4MPa-5秒这一较低温的热压接条件下的初始连接电阻和粘接强度存在问题。另外，在160℃-4MPa-5秒这一热压接条件下的粘接强度和可修复性也存在问题。
另外，比较例2的各向异性导电膜不使用β-烷基缩水甘油基型环氧树脂，与比较例1相比，作为环氧树脂，将通常的缩水甘油基醚型环氧树脂的一半用氧化烯改性缩水甘油基醚型环氧树脂代替，结果，由于只不过是仅使用了缩水甘油基醚型环氧树脂的物质，因此与比较例1同样地在150℃-4MPa-5秒这一较低温的热压接条件下的初始连接电阻和粘接强度存在问题，另外，在160℃-4MPa-5秒这一热压接条件下可修复性也存在问题。
比较例3的各向异性导电膜中，作为环氧树脂，虽然组合使用了β-烷基缩水甘油基型环氧树脂和缩水甘油基醚型环氧树脂，但质量比为1:9的比例，因此在150℃-4MPa-5秒这一较低温的热压接条件下的初始连接电阻和粘接强度存在问题。另外，在160℃-4MPa-5秒这一热压接条件下粘接强度和可修复性也存在问题。
比较例4的各向异性导电膜中，作为环氧树脂，仅使用了β-烷基缩水甘油基型环氧树脂，因此在150℃-4MPa-5秒这一较低温的热压接条件下的可修复性不存在问题，但初始连接电阻和粘接强度存在问题，另外，在160℃-4MPa-5秒这一热压接条件下粘接强度也存在问题。
与比较例2相比，比较例5的各向异性导电膜中，作为环氧树脂，将通常的缩水甘油基醚型环氧树脂和氧化烯改性缩水甘油基醚型环氧树脂的各一部分用脂环式环氧树脂代替，不使用β-烷基缩水甘油基型环氧树脂，因此DSC的反应起始温度低，另外，在150℃和160℃-4MPa-5秒这一较低温和中温的热压接条件下的可修复性存在问题。
与比较例2相比，比较例6和7的各向异性导电膜的阳离子系固化剂中的稳定剂量从3%分别增加至5%和8%，作为环氧树脂，与比较例2同样地不使用β-烷基缩水甘油基型环氧树脂，而使用了通常的缩水甘油基醚型环氧树脂和氧化烯改性缩水甘油基醚型环氧树脂，因此在170℃-4MPa-5秒这一热压接条件下的可修复性存在问题。
产业上的可利用性
使用阳离子系固化剂的本发明的环氧树脂基质的各向异性导电膜中，作为成为导电性颗粒的分散介质的构成热固型环氧树脂组合物的环氧树脂，将β-烷基缩水甘油基型环氧树脂和缩水甘油基醚型环氧树脂以特定比例组合使用，因此低温快速固化性、可修复性、连接可靠性和保存稳定性可以同时得到改善。因此，对于制造半导体装置、LED装置等是有用的。
符号的说明
10 第一电子部件
11、31 端子
20 各向异性导电膜
21 导电性颗粒
30 第二电子部件
40 加热焊接机
100 连接结构体

Claims (7)

1.各向异性导电膜，其为在包含环氧树脂、作为环氧树脂用固化剂的阳离子系固化剂和膜形成用树脂的热固型环氧树脂组合物中分散有导电性颗粒的各向异性导电膜，
该环氧树脂以质量比9:1~2:8的比例含有β-烷基缩水甘油基型环氧树脂和缩水甘油基醚型环氧树脂。
2.根据权利要求1所述的各向异性导电膜，其中，该环氧树脂以质量比8:2~4:6的比例含有β-烷基缩水甘油基型环氧树脂和缩水甘油基醚型环氧树脂。
3.根据权利要求1或2所述的各向异性导电膜，其中，该β-烷基缩水甘油基型环氧树脂为间苯二酚二（β-甲基缩水甘油基）醚。
4.根据权利要求1~3中任一项所述的各向异性导电膜，其中，该缩水甘油基醚型环氧树脂为氧化烯改性缩水甘油基醚型环氧树脂。
5.根据权利要求1~4中任一项所述的各向异性导电膜，其中，阳离子系固化剂为芳基硫鎓盐系固化剂。
6.制造方法，其为利用各向异性导电膜将第一电子部件的端子与第二电子部件的端子进行了各向异性导电连接的连接结构体的制造方法，该制造方法具备如下工序：
在第一电子部件的端子上临时粘贴权利要求1~5中任一项所述的各向异性导电膜的工序；
在进行了临时粘贴的各向异性导电膜上将第二电子部件以其端子与第一电子部件的相应端子相对的方式进行临时设置的工序；以及
将第二电子部件边用加热焊接机加热边向第一电子部件按压，将第一电子部件的端子与第二电子部件的端子各向异性导电连接的工序。
7.连接结构体，其是利用权利要求1~5中任一项所述的各向异性导电膜将第一电子部件的端子与第二电子部件的端子进行各向异性导电连接而成的。
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