CN105778815B - 电路部件的连接结构和电路部件的连接方法 - Google Patents

电路部件的连接结构和电路部件的连接方法 Download PDF

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CN105778815B
CN105778815B CN201610149536.9A CN201610149536A CN105778815B CN 105778815 B CN105778815 B CN 105778815B CN 201610149536 A CN201610149536 A CN 201610149536A CN 105778815 B CN105778815 B CN 105778815B
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circuit
conducting particles
metal level
nucleome
electrode
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CN105778815A (zh
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小岛和良
小林宏治
有福征宏
望月日臣
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Lishennoco Co ltd
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Hitachi Chemical Co Ltd
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    • H—ELECTRICITY
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    • 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
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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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    • H01R12/00—Structural associations of a plurality of mutually-insulated electrical connecting elements, specially adapted for printed circuits, e.g. printed circuit boards [PCB], flat or ribbon cables, or like generally planar structures, e.g. terminal strips, terminal blocks; Coupling devices specially adapted for printed circuits, flat or ribbon cables, or like generally planar structures; Terminals specially adapted for contact with, or insertion into, printed circuits, flat or ribbon cables, or like generally planar structures
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    • H01R12/57—Fixed connections for rigid printed circuits or like structures characterised by the terminals surface mounting terminals
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    • H05K3/323—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by conductive adhesives by applying an anisotropic conductive adhesive layer over an array of pads
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K9/02—Ingredients treated with inorganic substances
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    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
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    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
    • H05K2201/0203—Fillers and particles
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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
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    • H05K2201/10—Details of components or other objects attached to or integrated in a printed circuit board
    • H05K2201/10613—Details of electrical connections of non-printed components, e.g. special leads
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    • H05K3/36—Assembling printed circuits with other printed circuits
    • H05K3/361—Assembling flexible printed circuits with other printed circuits

Abstract

本发明涉及电路部件的连接结构和电路部件的连接方法。所述电路部件的连接结构具备：形成有电路电极且所述电路电极被相对配置的2个电路部件；和介于所述电路部件之间，通过加热加压而将所述电路电极电连接的电路连接部件，所述电路连接部件为电路连接材料的固化物，所述电路连接材料含有粘接剂组合物和导电粒子，所述导电粒子具备由有机高分子化合物形成的核体以及被覆该核体的金属层，所述金属层具有向着导电粒子的外侧突起的突起部，所述金属层由镍或者镍合金构成，所述核体的平均粒径为2.5～3.5μm，所述金属层的厚度为75～100nm，在所述电路连接材料所含有的导电粒子的突起部的内侧部分，金属层陷入核体。

Description

电路部件的连接结构和电路部件的连接方法
本申请是申请日为2008年10月29日，申请号为200880020091.8，发明名称为《电路连接材料及电路部件的连接结构》的中国专利申请的分案申请。
技术领域
本发明涉及一种电路连接材料及电路部件的连接结构。
背景技术
在液晶显示面板和带载封装(以下称为“TCP”)的连接、挠性电路基板(以下称为“FPC”)和TCP的连接、或者FPC和印刷配线板的连接这样的电路部件彼此的连接中，使用粘接剂中分散有导电粒子的电路连接材料(例如各向异性导电性粘接剂)。
并且，最近在基板上安装半导体硅芯片的情况，为了连接电路部件彼此，不使用引线键合而将半导体硅芯片正面朝下直接安装在基板上，进行所谓的倒装芯片安装。在这倒装芯片安装中，电路部件彼此的连接中使用各向异性导电粘接剂等电路连接材料(参照专利文献1～5)。
专利文献1：日本特开昭59-120436号公报
专利文献2：日本特开昭60-191228号公报
专利文献3：日本特开平1-251787号公报
专利文献4：日本特开平7-90237号公报
专利文献5：日本特开2001-189171号公报
专利文献6：日本特开2005-166438号公报
发明内容
发明要解决的问题
可是，近年，伴随着电子设备的小型化、薄型化，形成于电路部件上的电路的高密度化得到发展，存在与邻接的电极的间隔或者电极的幅度变得非常窄的倾向。电路电极的形成是通过在整个基板上形成作为电路的基础的金属，在应该形成电路电极的部分涂布抗蚀剂并固化，除此以外的部分用酸或者碱蚀刻的工序进行的。但是，上述的被高密度化的电路的情况，如果在整个基板上形成的金属的凹凸大，则在凹部与凸部上的蚀刻时间不同，所以不能进行精密的蚀刻，存在邻接电路间短路或者发生断线的问题。因此，希望高密度电路的电极表面上凹凸小，即电极表面平坦。
但是，使用上述以往的电路连接材料连接这样的相对置的平坦的电路电极彼此的情况下，在电路连接材料中所含导电粒子和平坦电极之间就会残留粘接剂树脂，存在对置的电路电极间不能确保充分的电连接以及长期可靠性的问题。
因此，以解决上述问题为目的，提出了将含有如下所述导电粒子的电路连接材料用于对置的电路电极彼此的连接的技术，该导电粒子的表面侧具有多个突起、并且金属层的最外层为金(Au)(参照专利文献6)。
虽然使用此电路连接材料连接的电路连接结构体在对置的电路电极间能够确保充分的电连接以及长期可靠性，但是要求在实现对置的电路电极彼此间更加良好的电连接的同时，进一步提高电路电极间的电特性的长期可靠性。
本发明是鉴于上述情况而进行的，目的是提供一种能够实现对置的电路电极间的良好的电连接的同时，能够充分提高电路电极间的电特性的长期可靠性的电路连接材料，以及使用了该电路连接材料的电路部件的连接结构以及电路部件的连接方法。
解决问题的手段
就用于以往的电路连接材料的、表面具有突起的导电粒子而言，构成导电粒子的金属层的最外层由Au构成。由于Au是比较软的金属，所以电路连接时被施加压力的话突起就会变形，难以得到对于电路电极的长期的连接性。因此，本发明人反复进行深入研究的结果，着眼于构成导电粒子的金属层(金属层为多层的情况下是最外层)的材质，考虑到更换为比Au更硬的金属。于是，本发明人发现在电路连接时发生的、突起部的内侧部分的金属层向核体的陷入会影响对置的电路电极间的电连接，它是由于导电粒子的金属层的硬度和来源于由有机高分子化合物形成的核体的塑料的斥力引起的。即，在使用了本发明的电路连接材料的电路部件的连接中，依靠电路连接时的压力，导电粒子表面的突起部陷入电路电极侧的同时，突起部的内侧部分的金属层也陷入核体侧，通过依靠塑料的斥力此突起被压在电路电极侧，而形成了进一步陷入电路电极的电路连接部。其结果，本发明的电路连接材料，能够发挥对置的电路电极间的良好的连接，并能够提高电路电极间的电特性的长期可靠性。
本发明提供为了将形成有电路电极的2个电路部件电连接成电路电极对置的电路连接材料，电路连接材料含有粘接剂组合物和导电粒子，导电粒子具备由有机高分子化合物形成的核体及被覆该核体的金属层，金属层具有向着导电粒子的外侧突起的突起部，金属层由镍或者镍合金构成，在向导电粒子施加压力的情况下，突起部的内侧部分的金属层会陷入核体。
本发明还提供为了将形成有电路电极的2个电路部件电连接成电路电极对置的电路连接材料，电路连接材料含有粘接剂组合物和导电粒子，导电粒子具备由有机高分子化合物形成的核体及被覆该核体的多个金属层，金属层具有向着导电粒子的外侧突起的突起部，金属层的最外层由镍或者镍合金构成，在向所述导电粒子施加压力的情况下，突起部的内侧部分的金属层会陷入核体。
这样的电路连接材料能够在实现对置的电路路电极间的良好的电连接的同时，能够充分提高电路电极间的电特性的长期可靠性。
在本发明的电路连接材料中，优选上述金属层或者金属层的最外层的维氏硬度为400～1000。由此，更进一步使对置的电路电极间的电连接良好，能够更加提高电路电极间的电特性的长期可靠性。
并且，本发明提供一种电路部件的连接结构，它具备形成有电路电极且电路电极对向配置的2个电路部件、介于电路部件之间且通过加热加压而将电路电极电连接的电路连接部件，电路连接部件是本发明的电路连接材料的固化物，在电路连接材料所含有的导电粒子的突起部的内侧部分，金属层陷入了核体。
此电路部件的连接结构，由于使用上述电路连接材料制作，所以能够得到电路电极间的良好的电连接。于是，夹着导电粒子的对置的电路电极间的良好的电连接状态，通过电路连接材料的固化物而长期保持，由此能够充分提高电特性的长期可靠性。
在上述电路部件的连接结构中，优选2个电路部件的电路电极的至少一方的电路电极的表面由铟锡氧化物(以下称为“ITO”)或者铟锌氧化物(以下称为“IZO”)形成。像这样通过电路电极的表面由ITO或者IZO形成，与由Au、Ag、Sn、Pt族的金属、Al或者Cr形成的电极相比，具有能防止底层金属氧化的优点。
进一步，本发明提供一种电路部件的连接方法，其特征在于，使上述电路连接材料介于形成有电路电极、且电路电极对向配置的2个电路部件之间，加热加压而将电路电极电连接，由此使电路连接材料所含有的导电粒子的突起部的内侧部分的金属层陷入核体。由此可以制作电路电极间的电特性的长期可靠性十分优异的电路部件的连接结构。
发明效果
根据本发明的电路连接材料，能够实现对置的电路电极间的良好的电连接，同时能够充分提高电路电极间的电特性的长期可靠性。并且，根据本发明能够提供电路电极间的电特性的长期可靠性十分优异的电路部件的连接结构及其连接方法。
附图说明
图1是表示本发明的电路部件的连接结构的一实施方式的截面图。
图2是表示构成本发明的电路连接材料的导电粒子的各种形态的截面图。
图3是表示本发明的膜状电路连接材料的一实施方式的截面图。
图4是实施例2中制作的电路部件的连接结构中连接部的截面SEM照片。
符号说明
1是电路部件的连接结构；10是电路连接部件；11是绝缘性物质；12是导电粒子；14是突起(突起部)；21是核体(粒子)；21a是中核部(核体)；21b是突起部；22是金属层；30是第一电路部件；31是电路基板(第一电路基板)；31a是主面；32是电路电极(第一电路电极)；40是第二电路部件；41是电路基板(第二电路基板)；41a是主面；42是电路电极(第二电路电极)；50是膜状电路连接材料；51是粘接剂组合物；H是导电粒子的突起高度；S是邻接的突起间的距离。
具体实施方式
以下，根据需要参照附图，对本发明的适宜的实施方式进行详细说明。另外，附图中，同一要素标注同一符号，省略重复说明。并且，上下左右等的位置关系，只要事先没有说明，就是基于图面所示的位置关系。进一步，附图的尺寸比例不限于图示的比例。
电路部件的连接结构
图1是表示本发明的电路部件的连接结构的一例子的截面示意图。电路部件的连接结构1具备相互对置的第1电路部件30和第2电路部件40，在第1电路部件30和第2电路部件40之间设有连接它们的电路连接部件10。电路连接部件10是将含有粘接剂组合物和表面上具备多个突起14的导电粒子12的电路连接材料固化处理而得到的。从而，电路连接部件10含有绝缘性物质11和导电粒子12。这里，绝缘性物质11由粘接剂组合物的固化物构成。
第1电路部件30具备电路基板(第1电路基板)31和在电路基板31的主面31a上形成的电路电极(第1电路电极)32。第2电路部件40具备电路基板41和在电路基板41的主面41a上形成的电路电极(第2电路电极)42。
在电路基板31、41中，电路电极32、42的表面是平坦的。另外，在本发明中“电路电极的表面平坦”是指电路电极的表面的凹凸在20nm以下。
电路电极32、42的厚度优选50nm以上。在电路电极32、42的厚度不足50nm的情况下，存在电路连接材料中的导电粒子12的表面侧的突起部14在压接时贯穿电路电极32、42而与电路基板31、41接触的可能性。这种情况下，存在电路电极32、42和导电粒子12的接触面积减少而连接电阻上升的倾向。并且，电路电极32、42的厚度从制造成本等的角度考虑，优选1000nm以下，更加优选500nm以下。
作为电路电极32、42的材质，可以举出Au、Ag、Sn、Pt族的金属或者ITO、IZO、Al、Cr。尤其是电路电极32、42的材质为ITO或者IZO的情况下，电连接显著地变得良好，发挥了本发明的效果。并且，电路电极32、42可以全部由上述物质构成，也可以仅表面(最外层)由上述物质构成。
虽然电路基板31、41的材质不作特别的限制，但是通常为有机绝缘性物质、玻璃或者硅。
作为第1电路部件30和第2电路部件40的具体例子，可以举出半导体芯片、电阻芯片、电容器芯片等芯片部件，印刷基板等基板。这些电路部件30、40通常设有多个(根据情况可以是单个)电路电极(电路端子)32、42。并且，作为电路部件的连接结构的形态，还有IC芯片和芯片搭载基板的连接结构、电气电路相互的连接结构的形态。
并且，在第1电路部件30中，也可以在第1电路电极32和电路基板31之间进一步设置绝缘层；在第2电路部件40中，也可以在第2电路电极42和电路基板41之间进一步设置绝缘层。绝缘层只要由绝缘材料构成就不作特别的限制，但是通常由有机绝缘性物质、二氧化硅或者氮化硅构成。
而且，在此电路部件的连接结构1中，对置的电路电极32和电路电极42通过导电粒子12被电连接。即，导电粒子12与电路电极32、42的双方直接接触。具体的，导电粒子12的突起(又称为“突起部”)14贯穿绝缘性物质11而与第1电路电极32、第2电路电极42接触。
因此，电路电极32、42间的连接电阻充分降低，使电路电极32、42间的良好的电连接成为可能。从而，可以使电路电极32、42间的电流的流动畅通，并且可以充分发挥电路所具有的功能。
导电粒子12的多个突起14中的一部分突起，优选陷入电路电极32或者电路电极42中。此时，导电粒子12的突起14和电路电极32、42的接触面积进一步增加，可以进一步降低连接电阻。
在电路部件的连接结构1中，优选第1电路电极32、第2电路电极42的至少一方的表面积在15000μm2以下，同时，处于第1电路电极32和第2电路电极42之间的平均导电粒子数在1个以上。在这里，平均导电粒子数是指平均每电路电极的导电粒子数的平均值。此时，对置的电路电极32、42间的连接电阻能够更加充分降低。
并且，平均导电粒子数在3个以上的情况下，能够进一步实现良好的连接电阻。这是因为对置的电路电极32、42间的连接电阻充分降低。并且在电路电极32、42间的平均导电粒子数在1个以下的情况下，连接电阻变得过高，电子电路有时不能正常工作。
以下，对电路连接部件10进行详细说明。电路连接部件10为膜状，如上所述，是对含有表面侧具有突起部14的导电粒子12和粘接剂组合物的电路连接材料进行固化处理而得到的。
电路连接部件10含有绝缘性物质11和导电粒子12。导电粒子12，对其详细内容在后叙述，但是如图2的(a)、(b)所示，其表面侧具有多个突起部14。而且，在此电路部件的连接结构1中，对置的电路电极32和电路电极42通过导电粒子12电连接。即，导电粒子12与电路电极32、42双方直接接触。具体地，导电粒子12的突起部14贯穿绝缘性物质11，与第1电路电极32、第2电路电极42接触。并且，导电粒子12的突起部14的内侧部分的金属层22陷入核体21a侧，此时，通过核体21a的塑料的斥力突起部14压向电路电极32、42侧，突起部14成为更加陷入电路电极的状态。
因此，导电粒子12和电路电极32、42的接触面积增加，电路电极32、42间的连接电阻被充分降低，使电路电极32、42间的良好的电连接成为可能。从而，能够将电路电极32、42间的电流的流动变得畅通，并且能充分发挥电路所具有的功能。
电路连接材料
导电粒子
导电粒子12由具有导电性的粒子(本体部)和在此粒子的表面上形成的多个突起部14构成。在这里，多个突起部14由具有导电性的金属构成。图2是表示与本发明相关的电路连接材料中含有的导电粒子的各种形态的截面图。
图2的(a)表示的导电粒子12由核体21和在核体21的表面上形成的金属层22构成，所述核体21由有机高分子化合物形成。核体21由中核部21a和在中核部21a的表面上形成的突起部21b构成。金属层22在其表面侧具有多个突起部14。金属层22覆盖着核体21，在与突起部21b对应的位置向导电粒子的外侧突起，其突起着的部分成为突起部14。
核体21与由金属形成的核体相比，成本低，对于热膨胀或者压接接合时的尺寸变化弹性变形范围广，因此作为电路连接材料，更加适合。
作为构成核体21的中核部21a的有机高分子化合物，例如可以举出丙烯酸树脂、苯乙烯树脂、苯鸟粪胺树脂、有机硅树脂、聚丁二烯树脂或者这些的共聚物，也可以使用将这些交联的物质。
核体21的中核部21a的平均粒径优选1～4μm，更优选2～4μm，进一步优选2.5～3.5μm。如果平均粒径不足1μm，就会发生粒子的二次凝集，存在与邻接的电路的绝缘性不充分的倾向。另一方面，如果平均粒径超过4μm，由于电路连接时排除粘接剂组合物的面积变大，所以存在粘接剂组合物的排除不充分的倾向。另外，本说明书中的核体21的平均粒径是指中核部21a的平均粒径，可以通过使用粒度分布测定装置，或者通过电子显微镜观察导电粒子的截面来测定。
作为构成核体21的突起部21b的有机高分子化合物，例如可以举出丙烯酸树脂、苯乙烯树脂、苯鸟粪胺树脂、有机硅树脂、聚丁二烯树脂或者这些的共聚物，也可以使用将这些交联的物质。构成突起部21b的有机高分子化合物可以与构成中核部21a的有机高分子化合物相同或者不同。另外，突起部21b的平均粒径优选50～500nm。
核体21可以通过在中核部21a的表面吸附多个具有比中核部21a小的直径的突起部21b而形成。作为在中核部21a的表面吸附突起部21b的方法，例如可以举出，将双方或者一方的粒子用硅烷、铝、钛等各种偶联剂及粘接剂的稀释溶液处理表面后将两者混合附着的方法。
作为金属层22的材质可以举出Cu、Ni或者Ni合金、Ag或者Ag合金，优选Ni或者Ni合金。并且，在金属层22由多个金属层构成的情况下，金属层22的最外层的材质优选Ni或者Ni合金。作为镍合金例如可以举出Ni-B、Ni-W、Ni-B、Ni-W-Co、Ni-Fe和Ni-Cr。
作为金属层22的硬度，优选维氏硬度为400～1000，更加优选500～800。并且，金属层22由多个金属层构成的情况下，金属层22的最外层的维氏硬度为400～1000，更加优选500～800。金属层的维氏硬度不足400的情况下，电路电极接触时突起的金属层就会变形，对电路电极的陷入就会变弱，存在接触面积减少连接电阻变高的倾向。并且，如果金属层的维氏硬度超过1000，由于连接时的粒子变形导致金属层产生裂痕，变成电路电极彼此的传导通路被切断的状态而存在连接电阻增加的倾向。
金属层22可以通过使用无电解镀法对核体21镀覆这些金属而形成。无电解镀法大致被分为分批方式和连续滴加方式，使用任意方式都能够形成金属层22。
金属层22的厚度(镀层的厚度)优选65～125nm，更加优选75～100nm，进一步优选80～90nm。通过使金属层22的厚度在这样的范围内，能够使电路电极32、42间的连接电阻更加良好。在这里，本说明书中的导电粒子的金属层22的厚度指不包括突起部14的金属层部分的厚度，可以通过电子显微镜测定。
如果金属层22的厚度不足65nm，因为镀层的厚度薄，存在使连接电阻变大的倾向，如果超过125nm，镀覆时在导电粒子间发生凝结，存在在邻接的电路电极间容易发生短路的倾向。
并且，在导电粒子12中，金属层22从核体21上完全剥离了的粒子的混入率，优选在粒子25万个中不足5％，更优选不足1.0％，进一步优选不足0.1％。通过使金属层22从核体21上完全剥离了的粒子的混入率在这样的范围内，能够使电路电极32、42间的传导确切。如果金属层22从核体21上完全剥离了的粒子的混入率在5％以上，由于与导电无关的粒子存在于电极上，存在连接电阻变大的倾向。
本发明中的导电粒子12也有核体21部分性地露出来的情况。从连接可靠性的角度考虑，对核体21的表面积的金属层22的被覆率优选70％以上，更加优选80～100％。通过使金属层22的被覆率在这样的范围内，能够使电路电极32、42间的连接电阻更加良好。如果金属层22的被覆率不足70％，因为导电粒子表面的传导面积会变小所以存在连接电阻变大的倾向。
导电粒子12的突起14的高度H，优选65～500nm，更加优选100～300nm。并且，邻接的突起14间的距离S，优选1000nm以下，更加优选500nm。
并且，关于邻接的突起14间的距离S，为了使粘接剂组合物不进入导电粒子12和电路电极32、42之间，并且使导电粒子12和电路电极32、42充分接触，优选至少在50nm以上。这里，导电粒子12的突起14的高度H以及邻接的突起14间的距离S能够通过电子显微镜测定。
另外，导电粒子12如图2的(b)所示，核体21可以仅由中核部21a构成。换言之，在如图2的(a)所示的导电粒子12中，也可以不设有突起部21b。如图2的(b)所示的导电粒子12能够通过在核体21a的表面镀覆金属，在核体21a的表面上形成金属层22而得到。
在这里，对为了形成突起14的镀覆方法进行说明。例如，通过在镀覆反应的途中追加比最初使用的镀液高浓度的镀液使镀液浓度不均一而形成突起14。并且，可以通过调节镀液的pH值，例如使镍镀液的pH为6而能够得到瘤突状金属层，即具有突起14的金属层22(望月等，表面技术，Vol.48，No.4,429～432页，1997)。并且，作为对镀浴的稳定性有贡献的络合剂，与使用甘氨酸的情况下能够得到平滑的金属层(皮膜)相对，使用酒石酸或者DL-苹果酸的情况下能够得到瘤突状的皮膜、即具有突起14的金属层22(荻原等，非晶质镀覆(非晶質メッキ)，Vol.36，第35～37页，1994；荻原等，电路安装学会志(回路実装学会誌)，Vol.10，No.3，148～152页，1995)。
金属层22可以由单一的金属的层构成，也可以由多个金属的层构成。
粘接剂组合物
作为粘接剂组合物，优选(1)含有环氧树脂和环氧树脂的潜在性固化剂的组合物、(2)含有自由基聚合性物质和通过加热产生游离自由基的固化剂的组合物、或者(1)和(2)的混合组合物。
首先，对(1)含有环氧树脂和环氧树脂的潜在性固化剂的组合物进行说明。作为上述环氧树脂可以举出双酚A型环氧树脂、双酚F型环氧树脂、双酚S型环氧树脂、苯酚酚醛清漆型环氧树脂、甲酚酚醛清漆型环氧树脂、双酚A酚醛清漆型环氧树脂、双酚F酚醛清漆型环氧树脂、脂环式环氧树脂、缩水甘油酯型环氧树脂、缩水甘油胺型环氧树脂、海因型环氧树脂、异氰尿酸酯型环氧树脂、链状脂肪族环氧树脂。这些环氧树脂可以被卤化、也可以被加氢。这些环氧树脂也可以将2种以上并用。
作为潜在性固化剂只要是能使环氧树脂固化的就可以。作为这样的潜在性固化剂可以举出阴离子聚合性的催化剂型固化剂、阳离子聚合性的催化剂型固化剂、加聚型的固化剂。这些可以单独或者作为2种以上的混合物而使用。这其中，从快速固化性优异、不需要考虑化学当量的角度考虑，优选阴离子或者阳离子聚合性的催化剂型固化剂。
作为阴离子或者阳离子聚合性的催化剂型固化剂，可以举出咪唑系、酰肼系、三氟化硼-胺配位化合物、鋶盐、胺酰亚胺、二氨基顺丁烯二腈、三聚氰胺及其衍生物、聚胺的盐、双氰胺，还可以使用这些的改性物。作为加聚型的固化剂可以举出聚胺类、聚硫醇、多酚、酸酐。
作为阴离子聚合型的催化剂型固化剂在配合了叔胺类或咪唑类的情况下，环氧树脂通过在160℃～200℃程度的中温中加热数10秒～数小时程度来固化。因此，可用时间(适用期)变得比较长，所以优选。
作为阳离子聚合型的催化剂型固化剂，优选例如通过能量射线照射使环氧树脂固化的感光性鎓盐(以芳香族重氮盐、芳香族鋶盐等为主来使用)。
并且，作为除了能量射线照射以外通过加热活性化且使环氧树脂固化的物质，有脂肪族鋶盐。这种固化剂因为具有称为快速固化性的特征而优选。
将这些潜在性固化剂用聚氨酯系、聚酯系等高分子物质，镍、铜等金属薄膜以及硅酸钙等无机物被覆而微型胶囊化的固化剂，因为可以延长可用时间而优选。
接着，对(2)含有自由基聚合性物质和通过加热产生游离自由基的固化剂的组合物进行说明。
自由基聚合性物质是具有通过自由基来进行聚合的官能团的物质。作为这样的自由基聚合性物质，可以举出丙烯酸酯(也包括对应的甲基丙烯酸酯。以下相同)化合物、丙烯酰氧(包括对应的甲基丙烯酰氧。以下相同)化合物、马来酰亚胺化合物、柠康酰亚胺树脂、纳迪克酰亚胺树脂。自由基聚合性物质能够以单体或者低聚物的状态使用，也可以并用单体和低聚物。
作为上述丙烯酸类化合物的具体例子可以举出丙烯酸甲酯、丙烯酸乙酯、丙烯酸异丙脂、丙烯酸异丁酯、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、四羟甲基甲烷四丙烯酸酯、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-(丙烯酰氧基聚乙氧基)苯基]丙烷、丙烯酸双环戊烯酯、丙烯酸三环癸酯、三(丙烯酰氧乙基)异氰尿酸酯、氨酯丙烯酸酯等。这些可以单独或者将2种以上混合使用。
并且，根据需要可以适当使用对苯二酚、对苯二酚甲基醚类等阻聚剂。进一步，从提高耐热性的角度考虑，优选丙烯酸酯化合物具有选自由双环戊烯基、三环癸基以及三嗪环组成的群的至少1种的取代基。
上述马来酰亚胺化合物是在分子中至少含有2个以上马来酰亚胺基的化合物。作为此类马来酰亚胺化合物，例如可以举出1-甲基-2,4-双马来酰亚胺基苯、N,N’-间苯撑双马来酰亚胺、N,N’-对苯撑双马来酰亚胺、N,N’-间甲苯撑双马来酰亚胺、N,N’-4,4-联苯撑双马来酰亚胺、N,N’-4,4-(3,3’-二甲基联苯撑)双马来酰亚胺、N,N’-4,4-(3,3’-二甲基二苯基甲烷)双马来酰亚胺、N,N’-4,4-(3,3’-二乙基二苯基甲烷)双马来酰亚胺、N,N’-4,4-二苯基甲烷双马来酰亚胺、N,N’-4,4-二苯基丙烷双马来酰亚胺、N,N’-3,3’-二苯砜双马来酰亚胺、N,N’-4,4-二苯基醚双马来酰亚胺、2,2-双(4-(4-马来酰亚胺基苯氧基)苯基)丙烷、2,2-双(3-仲丁基-4,8-(4-马来酰亚胺基苯氧基)苯基)丙烷、1,1-双(4-(4-马来酰亚胺基苯氧基)苯基)癸烷、4,4’-亚环己基-双(1-(4-马来酰亚胺基苯氧基)苯氧基)-2-环己基苯、2,2-双(4-(4-马来酰亚胺基苯氧基)苯基)六氟丙烷。这些可以单独或者将2种以上混合使用。
上述柠康酰亚胺树脂是将在分子中至少有1个柠康酰亚胺基的柠康酰亚胺化合物进行聚合而成的物质。作为柠康酰亚胺化合物，例如可以举出苯基柠康酰亚胺、1-甲基-2,4-双柠康酰亚胺基苯、N,N’-间苯基双柠康酰亚胺、N,N’-对苯基双柠康酰亚胺、N,N’-4,4-联苯撑双柠康酰亚胺、N,N’-4,4-(3,3-二甲基联苯撑)双柠康酰亚胺、N,N’-4,4-(3,3-二甲基二苯基甲烷)双柠康酰亚胺、N,N’-4,4-(3,3-二乙基二苯基甲烷)双柠康酰亚胺、N,N’-4,4-二苯基甲烷双柠康酰亚胺、N,N’-4,4-二苯基丙烷双柠康酰亚胺、N,N’-4,4-二苯基醚双柠康酰亚胺、N,N’-4,4-二苯砜双柠康酰亚胺、2,2-双(4-(4-柠康酰亚胺基苯氧基)苯基)丙烷、2,2-双(3-仲丁基-3,4-(4-柠康酰亚胺基苯氧基)苯基)丙烷、1,1-双(4-(4-柠康酰亚胺基苯氧基)苯基)癸烷、4,4’-亚环己基-双(1-(4-柠康酰亚胺基苯氧基)苯氧基)-2-环己基苯、2,2-双(4-(4-柠康酰亚胺基苯氧基)苯基)六氟丙烷。这些可以单独或者2种以上混合使用。
上述纳迪克酰亚胺树脂是将在分子中至少有1个纳迪克酰亚胺基的纳迪克酰亚胺化合物进行聚合而成的物质。作为纳迪克酰亚胺化合物，例如可以举出苯基纳迪克酰亚胺、1-甲基-2,4-双纳迪克酰亚胺基苯、N,N’-间苯基双纳迪克酰亚胺、N,N’-对苯基双纳迪克酰亚胺、N,N’-4,4-联苯撑双纳迪克酰亚胺、N,N’-4,4-(3,3-二甲基联苯撑)双纳迪克酰亚胺、N,N’-4,4-(3,3-二甲基二苯基甲烷)双纳迪克酰亚胺、N,N’-4,4-(3,3-二乙基二苯基甲烷)双纳迪克酰亚胺、N,N’-4,4-二苯基甲烷双纳迪克酰亚胺、N,N’-4,4-二苯基丙烷双纳迪克酰亚胺、N,N’-4,4-二苯基醚双纳迪克酰亚胺、N,N’-4,4-二苯砜双纳迪克酰亚胺、2,2-双(4-(4-纳迪克酰亚胺基苯氧基)苯基)丙烷、2,2-双(3-仲丁基-3,4-(4-纳迪克酰亚胺基苯氧基)苯基)丙烷、1,1-双(4-(4-纳迪克酰亚胺基苯氧基)苯基)癸烷、4,4’-亚环己基-双(1-(4-纳迪克酰亚胺基苯氧基)苯氧基)-2-环己基苯、2,2-双(4-(4-纳迪克酰亚胺基苯氧基)苯基)六氟丙烷。这些可以单独或者将2种以上混合使用。
并且，优选并用上述自由基聚合性物和由下述化学式(Ⅰ)表示的具有磷酸酯结构的自由基聚合性物质。在这种情况下，由于提高对金属等无机物表面的粘接强度，适合于电路电极彼此的粘接。
[化1]
式中，n表示1～3的整数。
上述具有磷酸酯结构的自由基聚合性物质可以通过使磷酸酐和(甲基)丙烯酸2-羟基乙酯进行反应而得到。作为具有磷酸酯结构的自由基聚合性物质，具体的有一(2-甲基丙烯酰氧基乙基)酸式磷酸酯、二(2-甲基丙烯酰氧基乙基)酸式磷酸酯。这些可以单独或者将2种以上混合使用。
上述具有由化学式(Ⅰ)表示的磷酸酯结构的自由基聚合性物质的配合量，相对于自由基聚合性物质和根据需要配合的膜形成材料的合计100质量份，优选0.01～50质量份，更加优选0.5～5质量份。
上述自由基聚合性物质可以和烯丙基丙烯酸酯并用。在这种情况下，烯丙基丙烯酸酯的配合量，相对于自由基聚合性物质和根据需要配合的膜形成材料的合计100质量份，优选0.1～10质量份，更加优选0.5～5质量份。
通过加热而产生游离自由基的固化剂是通过加热分解而产生游离自由基的固化剂。作为这样的固化剂可以举出过氧化化合物、偶氮系化合物。这样的固化剂可以根据目标连接温度、连接时间、适用期等适当选择。从高反应性和提高适用期的观点出发，优选半衰期10小时的温度在40℃以上并且半衰期1分钟的温度在180℃以下的有机过氧化物，优选半衰期10小时的温度在60℃以上并且半衰期1分钟的温度在170℃以下的有机过氧化物。
上述固化剂的配合量，在连接时间为25秒以下的情况下，为了获得足够的反应率，相对于自由基聚合性物质和根据需要配合的膜形成材料的合计100质量份，优选2～10质量份程度，更加优选4～8质量份。另外，在不限定连接时间的情况下的固化剂的配合量，相对于自由基聚合性物质和根据需要配合的膜形成材料的合计100质量份，优选0.05～20质量份，更优选0.1～10质量份。
作为通过加热产生游离自由基的固化剂，更具体地可以举出二酰基过氧化物、过氧化二碳酸酯、过氧化酯过氧化缩酮、二烷基过氧化物、氢过氧化物、甲硅烷基过氧化物。
并且，从能抑制电路电极32、42的腐蚀的观点出发，固化剂优选固化剂中含有的氯离子或有机酸的浓度在5000ppm以下，进一步，更加优选加热分解后产生的有机酸少的固化剂。
作为这样的固化剂，具体地可以举出过氧化酯、二烷基过氧化物、氢过氧化物、甲硅烷基过氧化物，更加优选从可以得到高反应性的过氧化酯中选定。另外，上述固化剂可以适当混合使用。
作为过氧化酯，可以举出过氧化新癸酸异丙苯酯、1,1,3,3-四甲基丁基过氧化新癸酸酯、1-环己基-1-甲基乙基过氧化新癸酸酯、叔己基过氧化新癸酸酯、过氧化三甲基乙酸叔丁酯、1,1,3,3-四甲基丁基过氧化-2-乙基己酸酯、2,5-二甲基-2,5-二(2-乙基己酰基过氧化)己烷、1-环己基-1-甲基乙基过氧化-2-乙基己酸酯、过氧化-2-乙基己酸叔己酯、过氧化-2-乙基己酸叔丁酯、过氧化异丁酸叔丁酯、1,1-双(叔丁基过氧化)环己烷、过氧化异丙基一碳酸叔己酯、过氧化-3,5,5-三甲基己酸叔丁酯、过氧化月桂酸叔丁酯、2,5-二甲基-2,5-二(间甲苯酰基过氧化)己烷、过氧化异丙基一碳酸叔丁酯、过氧化-2-乙基己基一碳酸叔丁酯、过氧化苯甲酸叔己酯、过氧化乙酸叔丁酯。
作为二烷基过氧化物，可以举出α,α’-双(叔丁基过氧化)二异丙基苯、二异丙苯基过氧化物、2,5-二甲基-2,5-二(叔丁基过氧化)己烷、叔丁基异丙苯基过氧化物。
作为氢过氧化物，可以举出二异丙基苯过氧化氢、异丙苯过氧化氢。
作为二酰基过氧化物，可以举出异丁基过氧化物、2,4-二氯苯甲酰过氧化物、3,5,5-三甲基己酰过氧化物、辛酰过氧化物、月桂酰过氧化物、硬酯酰过氧化物、琥珀酰过氧化物、苯甲酰过氧化甲苯、苯甲酰过氧化物。
作为过氧化二碳酸酯，可以举出过氧化二碳酸二正丙酯、过氧化二碳酸二异丙酯、双(4-叔丁基环己基)过氧化二碳酸酯、二-2-乙氧基甲氧基过氧化二碳酸酯、二(2-乙基己基过氧化)二碳酸酯、过氧化二碳酸二甲氧基丁酯、二(3-甲基-3-甲氧基丁基过氧化)二碳酸酯。
作为过氧化缩酮，可以使用1,1-双(叔己基过氧化)-3,3,5-三甲基环己烷、1,1-双(叔己基过氧化)环己烷、1,1-双(叔丁基过氧化)-3,3,5-三甲基环己烷、1,1-(叔丁基过氧化)环十二烷、2,2-双(叔丁基过氧化)癸烷。
作为甲硅烷基过氧化物，可以举出叔丁基三甲基甲硅烷基过氧化物、双(叔丁基)二甲基甲硅烷基过氧化物、叔丁基三乙烯基甲硅烷基过氧化物、双(叔丁基)二乙烯基甲硅烷基过氧化物、三(叔丁基)乙烯基甲硅烷基过氧化物、叔丁基三烯丙基甲硅烷基过氧化物、双(叔丁基)二烯丙基甲硅烷基过氧化物、三(叔丁基)烯丙基甲硅烷基过氧化物。
这些固化剂可以单独或者将2种以上混合使用，还可以将分解促进剂、抑制剂等混合使用。并且，也可以将这些固化剂用聚氨酯系、聚酯系的高分子物质等被覆而微胶囊化。微胶囊化了的固化剂因为可用时间被延长而优选。
粘接剂组合物可以根据需要添加膜形成材料来使用。膜形成材料具有如下作用：将液态物质固体化并将构成组合物制成膜形状时，可以使此膜的操作变得容易，赋予此膜不易裂开、破碎、发粘的机械特性等，在通常的状态(常温常压)下能够作为膜来操作。
作为膜形成材料可以举出苯氧树脂、聚乙烯醇缩甲醛树脂、聚苯乙烯树脂、聚乙烯醇缩丁醛树脂、聚酯树脂、聚酰胺树脂、二甲苯树脂、聚氨酯树脂等。这其中，从粘接性、相溶性、耐热性、机械强度优异的角度考虑优选苯氧树脂。
苯氧树脂是通过将2官能酚类和环氧卤丙烷反应至高分子化，或者将2官能环氧树脂和2官能酚类进行加聚而得到的树脂。苯氧树脂例如可以通过使2官能酚类1摩尔和环氧卤丙烷0.985～1.015摩尔，在碱金属氢氧化物等催化剂的存在下，在非反应性溶剂中，在40～120℃的温度下进行反应而获得。
并且，作为苯氧树脂，从树脂的机械特性或者热特性的观点出发，尤其优选将2官能环氧树脂和2官能酚类的配合当量比设为环氧基/酚羟基＝1/0.9～1/1.1，在碱金属化合物、有机磷系化合物、环状胺系化合物等催化剂的存在下，在沸点120℃以上的酰胺系、醚系、酮系、内酯系、醇系等有机溶剂中，以反应固体成分在50质量％以下的条件加热到50～200℃进行加聚反应而获得。
作为上述2官能环氧树脂，可以举出双酚A型环氧树脂、双酚F型环氧树脂、双酚AD型环氧树脂、双酚S型环氧树脂、联苯二缩水甘油醚、甲基取代联苯二缩水甘油醚。
2官能酚类是具有2个酚性羟基的物质。作为2官能酚类例如可以举出对苯二酚、双酚A、双酚F、双酚AD、双酚S、双酚芴、甲基取代双酚芴、二羟基联苯、甲基取代二羟基联苯等双酚类。
苯氧树脂可以被自由基聚合性的官能团或者其他的反应性化合物改性(例如环氧改性)。苯氧树脂可以将1种单独或者将2种以上混合使用。
粘接剂组合物可以进一步含有将丙烯酸、丙烯酸酯、甲基丙烯酸酯以及丙烯腈中的至少一种作为单体成分的聚合物或者共聚物。在这里，从应力缓和优异的角度考虑，优选并用含有含缩水甘油醚基的丙烯酸缩水甘油酯或者甲基丙烯酸缩水甘油酯的共聚物系丙烯酸类橡胶。这些丙烯酸类橡胶的重均分子量，从提高粘接剂的凝聚力的角度考虑优选20万以上。
导电粒子12的配合量优选相对于粘接剂组合物100体积份为0.1～30体积份，其配合量可以根据用途具体使用。从防止由于过量的导电粒子12引起的电路电极的短路等的观点出发，导电粒子12的配合量更优选0.1～10体积份。
电路连接材料中也可以进一步含有橡胶微粒、填充剂、软化剂、促进剂、抗老化剂、着色剂、阻燃剂、触变剂、偶联剂、酚树脂、三聚氰胺树脂、异氰酸酯类。
橡胶微粒只要是具有所配合的导电粒子12的平均粒径的2倍以下的平均粒径，并且具有导电粒子12和粘接剂组合物在室温下的储存弹性模量的1/2以下的储存弹性模量的即可。尤其是橡胶微粒的材质为有机硅、丙烯酸类乳剂、SBR、NBR、聚丁二烯橡胶的微粒适合单独或者将2种以上混合使用。3维交联的这些橡胶微粒，耐溶剂性优异，容易分散在粘接剂组合物中。
电路连接材料中含有填充剂的情况下，由于连接可靠性等会提高所以优选。填充剂只要其最大直径为导电粒子12的粒径的1/2以下就能使用。只要其最大直径为导电粒子的粒径的1/2以下就能使用。并且，在并用不具有导电性的粒子的情况下，填充剂只要在不具有导电性的粒子的直径以下就能使用。
填充剂的配合量相对于粘接剂组合物100体积份，优选5～60体积份。配合量如果超过60体积份就会存在连接可靠性提高效果饱和的倾向，如果不足5体积份就会存在填充剂添加的效果不充分的倾向。
作为上述偶联剂，含有乙烯基、丙烯酰基、环氧基或者异氰酸酯基的化合物，因为粘接性提高所以优选。
电路部件的连接方法
接下来，对上述电路部件的连接结构的制造方法进行说明。
首先，准备具有上述的第1电路电极32的第1电路部件30、具有第2电路电极42的第2电路部件40、电路连接材料。作为电路连接材料准备例如成形为膜状的电路连接材料(以下，称为膜状电路连接材料)50。
图3是表示本发明涉及的膜状电路连接材料的一实施方式的截面图。膜状电路连接材料50是将上述电路连接材料成形为膜状的电路连接材料，电路连接材料通常含有在表面侧具有突起14的导电粒子12和粘接剂组合物51。一般，电路连接材料中含有的粘接剂组合物具有粘接性，通过对第1和第2电路电极30、40的固化处理来固化。膜状电路连接材料50的厚度优选10～50μm。
接着，在第1电路部件30的上面，放置膜状电路连接材料50。然后，将第2电路部件40放置在膜状电路连接材料50上，使第1电路电极32和第2电路电极42相对置。由此，能够使膜状电路路连接材料50介于第1电路部件30和第2电路部件40之间。此时，膜状电路连接材料50为膜状，容易操作。因此，根据此膜状电路连接材料50，在连接第1电路部件30和第2电路部件40时，可以容易地介于它们之间，可以使第1电路部件30和第2电路部件40的连接作业容易进行。
接着，通过第1电路部件30和第2电路部件40加热膜状电路连接材料50的同时加压实施固化处理，在第1和第2的电路部件30、40之间形成电路连接部件10。固化处理可以通过一般的方法进行，此方法可以通过粘接剂组合物适当选择。
此时，电路连接部件10中的导电粒子12的突起部14，贯穿绝缘性物质11而与第1电路电极32、第2电路电极42接触。并且，导电粒子12的突起部14的内侧的金属层22陷入核体21侧。此时，由于核体21的塑料(有机高分子)的斥力使突起部14被压向电路电极32、42侧，突起部14处于进一步还陷入电路电极的状态。并且，电路连接材料中的导电粒子12的金属层或者最外层为Ni或者Ni合金的情况下，因为比Au硬，所以与以往的最外层为Au的导电粒子相比，突起部14对于第1或者第2电路电极32、42陷入更深，导电粒子12和电路电极32、42的接触面积增加，连接电阻稳定。并且，通过使导电粒子12的金属层或者其最外层的维氏硬度在400～1000的范围，突起部14对于电路电极32、42的陷入就会变大。然后，通过电路连接材料被固化处理粘接剂组合物51被固化，实现对第1电路部件30和第2电路部件40的高粘接强度，长期保持导电粒子12和第1及第2电路电极32、42牢固接触的状态。这样的连接结构的状态可以通过用电子显微镜观察电路部件的连接结构的截面来确认。并且，作为电路基板使用透明的玻璃基板的情况下，可以通过玻璃基板观察电路连接部的表面来确认。
从而，不拘束于在第1和/或第2电路电极32、42的表面上有无凹凸，可以充分降低对置的第1和第2电路电极32、42间的连接电阻，并且可以在达成第1电路电极32和第2电路电极42的良好的电连接的同时充分提高第1和第2电路电极32、42间的电特性的长期可靠性。
另外，在上述实施方式中，使用膜状电路连接材料50来制造电路部件的连接结构，但是也可以代替膜状电路连接材料50，使用后述的电路连接材料。这种情况下，将电路连接材料溶解于溶剂中，再将此溶液涂布在第1电路部件30或者第2电路部件40的任一方并干燥，就能够介于第1和第2电路部件30、40之间。
另外，膜状电路连接材料50可以通过在支持体(聚对苯二甲酸乙二醇酯膜等)上用涂工装置(图中没有表示)涂布上述电路连接材料，并通过给定时间的热风干燥而制作。
以上，对本发明的适当的实施方式进行了说明，但是本发明不被此所限制。
实施例
以下，基于实施例具体说明本发明，但是本发明不被此所限定。
导电粒子的制作
核体的制作
改变四羟甲基甲烷四丙烯酸酯、二乙烯基苯和苯乙稀单体的混合比，作为聚合引发剂使用苯甲酰过氧化物进行悬浊聚合。接着，通过将所得聚合体分级得到了具有约3μm的平均粒径的核体。
导电粒子No.1的制作
对上述核体的表面实施无电解镀Ni处理，制作了具有均一厚度100nm的Ni层(金属层)的导电粒子No.1。
导电粒子No.2的制作
通过在导电粒子No.1上将Au以25nm的厚度进行置换镀，形成具有均一厚度的Au层，而制作了导电粒子No.2。
导电粒子No.3的制作
基于日本特许第3696429号等，通过调整镀Ni处理时的镀液的投入量、处理温度和时间并变更镀层的厚度，在上述核体的表面形成镀Ni的突起。由此，制作了还含有突起且Ni层的目标厚度为180～210nm的导电粒子No.3。
导电粒子No.4的制作
通过在导电粒子No.3上将Au以25nm的厚度进行置换镀，形成具有多个突起的Au层，而制作了导电粒子No.4。
对于如上所述制作的导电粒子No.1～4，使用电子显微镜(日立制作所制造，商品名“S-800”)观察，计算测定了突起的高度和邻接的突起间的距离。各导电粒子的金属层材质、维氏硬度、突起的高度和突起间的距离如表1所示。
表1
电路连接材料的制作
苯氧树脂溶液的调制
将苯氧树脂(重均分子量45000，美国联合碳化物公司制造，商品名“PKHC”)50g溶解于甲苯/乙酸乙酯＝50/50(质量比)的混合溶剂中，调制了固体成分40质量％的苯氧树脂溶液。
氨酯丙烯酸酯的合成
搅拌聚己内酯二醇(重均分子量：800)400质量份、2-羟基丙基丙烯酸酯131质量份、作为催化剂的二丁基锡二月桂酸酯0.5质量份和作为阻聚剂的对苯二酚一甲醚1.0质量份的同时加热到50℃进行混合。接着，向此混合液，滴加异佛尔酮二异氰酸酯222质量份，进一步搅拌的同时升温到80℃进行氨酯化反应。确认异氰酸酯基的反应率达到99％以上后，降低反应温度得到了氨酯丙烯酸酯。
电路连接材料A的制作
混合上述苯氧树脂溶液(固体成分含量：50g)125g、上述氨酯丙烯酸酯49g、磷酸酯型丙烯酸酯1g和作为通过加热产生游离自由基的固化剂的过氧化-2-乙基己酸叔己酯5g而得到了粘接剂组合物。相对于所得粘接剂组合物100质量份，将导电粒子No.3分散2.3质量份调制了电路连接材料。
然后，使用涂工装置将此电路连接材料涂布在将单面进行表面处理的厚度为50μm的PET膜上，通过70℃3分钟的热风干燥，在PET膜上形成了厚度为18μm的膜状电路连接材料A。
电路连接材料B的制作
代替导电粒子No.3使用2.3质量份的导电粒子No.1以外与电路连接材料A同样进行，制作了厚度为18μm的膜状电路连接材料B。
电路连接材料C的制作
代替导电粒子No.3使用2.1质量份的导电粒子No.2以外与电路连接材料A同样进行，制作了厚度为18μm的膜状电路连接材料C。
电路连接材料D的制作
代替导电粒子No.3使用2.1质量份的导电粒子No.4以外与电路连接材料A同样进行，制作了厚度为18μm的膜状电路连接材料D。
实施例1
作为第1电路部件准备具有由聚酰亚胺膜(厚度38μm)和镀锡铜箔(厚度8μm)组成的2层结构的挠性电路板(以下称为FPC)。对于此FPC的电路，设定为线宽18μm以及间距50μm。
接着，作为第2电路部件准备表面上具备ITO电路基板(厚度50nm，表面电阻<20Ω)的玻璃基板(厚度1.1mm)。对于此第2电路部件的电路，设定为线宽25μm以及间距50μm。
然后，在第2电路部件上贴上剪裁成规定尺寸(1.5×30mm)的电路连接材料A，在70℃、1.0MPa的条件下加热3秒，并进行加压临时连接。接着，剥离PET膜后，配置FPC使FPC和第2电路材料夹着电路连接材料A，使FPC的电路和第2电路部件的电路的位置对齐。然后，以170℃、3MPa、10秒的条件从FPC上方进行加热、加压将FPC和第2电路部件正式连接。这样制作了电路部件的连接结构。
实施例2
作为第1电路部件，准备与实施例1同样的FPC。接着，作为第2电路部件准备表面上具备IZO(最外层，厚度为50nm)/Cr(厚度20nm)/Al(厚度100nm)的3层结构的电路电极(表面电阻<20Ω)的玻璃基板(厚度1.1mm)。对于此第2电路部件的电路，设定为线宽25μm以及间距50μm。然后，与实施例1同样使用电路连接材料A，制作了电路部件的连接结构。
实施例3
作为第1电路部件，准备与实施例1同样的FPC。接着，作为第2电路部件准备表面上具备ITO(最外层，厚度为50nm)/Cr(厚度200nm)的2层结构的电路电极(表面电阻<20Ω)的玻璃基板(厚度1.1mm)。对于此第2电路部件的电路，设定为线宽25μm以及间距50μm。然后，与实施例1同样使用电路连接材料A，制作了电路部件的连接结构。
实施例4
作为第1电路部件，准备与实施例1同样的FPC。接着，作为第2电路部件准备表面上具备ITO(最外层，厚度为50nm)/Ti(厚度100nm)/Al(厚度200nm)/Ti(厚度100nm)的4层结构的电路电极(表面电阻<20Ω)的玻璃基板(厚度1.1mm)。对于此第2电路部件的电路，设定为线宽25μm以及间距50μm。然后，与实施例1同样使用电路连接材料A，制作了电路部件的连接结构。
实施例5
作为第1电路部件，准备与实施例1同样的FPC。接着，作为第2电路部件准备表面上具备Al电路电极(厚度200nm，表面电阻<5Ω)的玻璃基板(厚度1.1mm)。对于此第2电路部件的电路，设定为线宽25μm以及间距50μm。然后，与实施例1同样使用电路连接材料A，制作了电路部件的连接结构。
比较例1
代替电路连接材料A使用电路连接材料B以外其他按照实施例1进行，制作了电路部件的连接结构。
比较例2
代替电路连接材料A使用电路连接材料B以外其他按照实施例2进行，制作了电路部件的连接结构。
比较例3
代替电路连接材料A使用电路连接材料B以外其他按照实施例3进行，制作了电路部件的连接结构。
比较例4
代替电路连接材料A使用电路连接材料B以外其他按照实施例4进行，制作了电路部件的连接结构。
比较例5
代替电路连接材料A使用电路连接材料B以外其他按照实施例5进行，制作了电路部件的连接结构。
比较例6
代替电路连接材料A使用电路连接材料C以外其他按照实施例1进行，制作了电路部件的连接结构。
比较例7
代替电路连接材料A使用电路连接材料C以外其他按照实施例2进行，制作了电路部件的连接结构。
比较例8
代替电路连接材料A使用电路连接材料C以外其他按照实施例3进行，制作了电路部件的连接结构。
比较例9
代替电路连接材料A使用电路连接材料C以外其他按照实施例4进行，制作了电路部件的连接结构。
比较例10
代替电路连接材料A使用电路连接材料C以外其他按照实施例5进行，制作了电路部件的连接结构。
比较例11
代替电路连接材料A使用电路连接材料D以外其他按照实施例1进行，制作了电路部件的连接结构。
比较例12
代替电路连接材料A使用电路连接材料D以外其他按照实施例2进行，制作了电路部件的连接结构。
比较例13
代替电路连接材料A使用电路连接材料D以外其他按照实施例3进行，制作了电路部件的连接结构。
比较例14
代替电路连接材料A使用电路连接材料D以外其他按照实施例4进行，制作了电路部件的连接结构。
比较例15
代替电路连接材料A使用电路连接材料D以外其他按照实施例5进行，制作了电路部件的连接结构。
连接电阻的测定
对上述电路部件的连接结构，使用万用表(ADC株式会社制造，商品名“数字万用表7461A”)测定第1电路部件(FPC)的电路电极和第2电路部件的电路电极间的连接电阻值。连接电阻值是在初期(连接后立即)和80℃、95％RH的恒温恒湿槽中保持500小时(高温高湿处理)后测定。结果如表2所示。
在表2中，连接电阻值以邻接电路间的电阻37点的平均值和3倍的标准偏差值之和(x+3σ)表示。并且，电阻增加率是将从初期电阻值到高温高湿处理后电阻值的增加量以百分率表示，具体根据下述式算出：
电阻增加率(％)＝[(处理后电阻值-初期电阻值)/初期电阻值]×100
作为连接可靠性的改善效果的判断，将电阻增加率不足10％记为有改善效果，将10％以上且不足20％记为以往产品水平，将20％以上记为没有改善效果(NG)。
电路电极上存在的导电粒子数
使用微分干涉显微镜，将在上述电路部件的连接结构中各电路电极上存在的导电粒子数靠眼睛进行计数(n＝38)。其结果，在实施例1～15和比较例1～25的电路电极上的平均导电粒子数在32～45个的范围内，没有发现由电路连接材料或者电路部件的差异引起的导电粒子数的极端增减。
表2
如表2所示，在使用电路电极的整体或者表面由ITO或者IZO构成的第2电路部件的情况下，在实施例1～4的电路部件的连接结构中获得了电阻增加率不足7.5％这样非常小的结果。与此相对，比较例1～4的连接结构的电阻增加率约为27～39％，比较例6～9的连接结构的电阻增加率约为20～25％，比较例11～14的连接结构的电阻增加率约为14～18％。
由此可知，对于电路电极的整体或者表面由ITO或者IZO构成的电路电极，通过将含有具有突起且金属层或者金属层的最外层为Ni的导电粒子的电路连接材料用于连接，可以看到连接可靠性的改善。
并且，在使用具备Al电路电极的第2电路部件的情况下，用含有具有突起的导电粒子的电路连接材料进行连接的实施例5、比较例15中，结果为电阻增加率约为3.5％，较少。此结果，被认为可能是由于连接时导电粒子表面的突起把Al电路电极表面的氧化膜扎破而使其与电路电极接触的原因。对此，用含有没有突起的导电粒子的电路连接材料进行连接的比较例5、10中，比较例10的电阻增加率约为34％，比较例15的电阻增加率约为15％。
另外，使用具有突起且金属层为Ni的导电粒子的实施例5，和使用具有突起且最外层为Au的导电粒子的比较例15的电阻增加率为相同程度，因此，对于电路电极由Al构成的电路部件，存在由导电粒子最外层的不同金属种类引起的改善连接可靠性的效果并不显著的倾向。
并且，用扫描电子显微镜(SEM)观察在实施例1～5中制作的电路部件的连接结构的截面的结果，确认了构成导电粒子的金属层的突起部的内侧部分的金属层陷入核体。作为它的一个例子，将在实施例2中制作的电路部件的连接结构中连接部的截面SEM照片示于图4。
根据以上，确认了根据本发明的电路部件的连接结构，能够在达成对置的电路电极间的良好的电连接的同时，在高温高湿环境下或者热冲击试验等中也能够充分提高稳定的连接可靠性。
产业上的利用可能性
根据本发明的电路连接材料，能够在达成对置的电路电极间的良好的电连接的同时，能够充分提高电路电极间的电特性的长期可靠性。并且，根据本发明，能够提供电路电极间的电特性的长期可靠性十分优异的电路部件的连接结构及其连接方法。

Claims (8)

1.一种电路部件的连接结构，其具备：
形成有电路电极且所述电路电极被相对配置的2个电路部件；和
介于所述电路部件之间，通过加热加压而将所述电路电极电连接的电路连接部件，
所述2个电路部件的电路电极的至少一方的表面由铟锡氧化物形成，
所述电路连接部件为电路连接材料的固化物，所述电路连接材料含有粘接剂组合物和导电粒子，
所述粘接剂组合物为含有自由基聚合性物质和通过加热产生游离自由基的固化剂的组合物，
所述导电粒子具备由有机高分子化合物形成的核体以及被覆该核体的金属层，所述金属层具有向着导电粒子的外侧突起的突起部，所述金属层由镍或者镍合金构成，所述核体的平均粒径为2.5～3.5μm，所述金属层的厚度为75～100nm，
在所述电路连接材料所含有的导电粒子的突起部的内侧部分，金属层陷入核体。
2.根据权利要求1所述的电路部件的连接结构，其中，所述电路连接材料所含有的所述导电粒子的所述金属层的维氏硬度为400～1000。
3.一种电路部件的连接结构，其具备：
形成有电路电极且所述电路电极被相对配置的2个电路部件；和
介于所述电路部件之间，通过加热加压而将所述电路电极电连接的电路连接部件，
所述2个电路部件的电路电极的至少一方的表面由铟锡氧化物形成，
所述电路连接部件为电路连接材料的固化物，所述电路连接材料含有粘接剂组合物和导电粒子，
所述粘接剂组合物为含有自由基聚合性物质和通过加热产生游离自由基的固化剂的组合物，
所述导电粒子具备由有机高分子化合物形成的核体以及被覆该核体的多个金属层，所述金属层具有向着导电粒子的外侧突起的突起部，所述金属层的最外层由镍或者镍合金构成，所述核体的平均粒径为2.5～3.5μm，所述金属层的厚度为75～100nm，
在所述电路连接材料所含有的导电粒子的突起部的内侧部分，金属层陷入核体。
4.根据权利要求3所述的电路部件的连接结构，其中，所述电路连接材料所含有的所述导电粒子的所述金属层的最外层的维氏硬度为400～1000。
5.一种电路部件的连接方法，其中，在形成有电路电极且所述电路电极被相对配置的2个电路部件之间设置电路连接材料，
所述2个电路部件的电路电极的至少一方的表面由铟锡氧化物形成，
所述电路连接材料含有粘接剂组合物和导电粒子，所述粘接剂组合物为含有自由基聚合性物质和通过加热产生游离自由基的固化剂的组合物，所述导电粒子具备由有机高分子化合物形成的核体以及被覆该核体的金属层，所述金属层具有向着导电粒子的外侧突起的突起部，所述金属层由镍或者镍合金构成，所述核体的平均粒径为2.5～3.5μm，所述金属层的厚度为75～100nm，
通过加热加压使得所述电路连接材料所含有的导电粒子的突起部的内侧部分的金属层陷入核体，使所述电路电极电连接。
6.根据权利要求5所述的电路部件的连接方法，其中，所述电路连接材料所含有的所述导电粒子的所述金属层的维氏硬度为400～1000。
7.一种电路部件的连接方法，其中，在形成有电路电极且所述电路电极被相对配置的2个电路部件之间设置电路连接材料，
所述2个电路部件的电路电极的至少一方的表面由铟锡氧化物形成，
所述电路连接材料含有粘接剂组合物和导电粒子，所述粘接剂组合物为含有自由基聚合性物质和通过加热产生游离自由基的固化剂的组合物，所述导电粒子具备由有机高分子化合物形成的核体以及被覆该核体的多个金属层，所述金属层具有向着导电粒子的外侧突起的突起部，所述金属层的最外层由镍或者镍合金构成，所述核体的平均粒径为2.5～3.5μm，所述金属层的厚度为75～100nm，
通过加热加压使得所述电路连接材料所含有的导电粒子的突起部的内侧部分的金属层陷入核体，使所述电路电极电连接。
8.根据权利要求7所述的电路部件的连接方法，其中，所述电路连接材料所含有的所述导电粒子的所述金属层的最外层的维氏硬度为400～1000。
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