CN103351829A - 粘接剂以及使用该粘接剂的连接结构体 - Google Patents

粘接剂以及使用该粘接剂的连接结构体 Download PDF

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Publication number
CN103351829A
CN103351829A CN2013101829578A CN201310182957A CN103351829A CN 103351829 A CN103351829 A CN 103351829A CN 2013101829578 A CN2013101829578 A CN 2013101829578A CN 201310182957 A CN201310182957 A CN 201310182957A CN 103351829 A CN103351829 A CN 103351829A
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China
Prior art keywords
methyl
caking agent
circuit
compound
acrylate
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CN2013101829578A
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Inventor
宫泽笑
加藤木茂树
伊泽弘行
白坂敏明
富泽惠子
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Showa Denko Materials Co ltd
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Hitachi Chemical Co Ltd
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Publication of CN103351829A publication Critical patent/CN103351829A/zh
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    • H—ELECTRICITY
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    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/30—Assembling printed circuits with electric components, e.g. with resistor
    • H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
    • H05K3/321—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by conductive adhesives
    • 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
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Abstract

本发明涉及粘接剂以及使用该粘接剂的连接结构体，该粘接剂含有（a）热塑性树脂、（b）在30℃以下为固体的自由基聚合性化合物以及（c）自由基聚合引发剂。

Description

粘接剂以及使用该粘接剂的连接结构体
本发明是申请号为200880105355X（国际申请号为PCT/JP2008/065570），申请日为2008年8月29日、发明名称为“粘接剂以及使用该粘接剂的连接结构体”的发明申请的分案申请。
技术领域
本发明涉及一种粘接剂，以及使用该粘接剂的电路部件的连接结构体。背景技术
在半导体元件和液晶显示元件中，为了使元件中的各种部件粘结，一直以来使用各种粘接剂。对于该用途中所用的粘接剂，首先要求粘接强度，并且还要求耐热性、高温高湿环境下（例如，85℃/85％RH）的连接可靠性等多方面的特性。此外，作为粘接时所用的被粘接物，主要为印刷线路板和聚酰亚胺等有机基材，并且还可以使用铜、铝等金属和ITO、Si3N4、SiO2等具有多种表面状态的基材。因此，适合各种被粘接物的粘接剂的分子设计是必要的。
一直以来，作为上述半导体元件和液晶显示元件用的粘接剂，使用了含有显示出高粘接强度以及高连接可靠性的环氧树脂的热固性树脂被采用（例如，参见专利文献1）。作为热固性树脂，通常使用含有环氧树脂、具有和环氧树脂的反应性的酚醛树脂等固化剂、以及促进环氧树脂和固化剂反应的热潜在性催化剂作为构成成分的材料。
热潜在性催化剂是决定固化温度和固化速度的重要因素，并且从室温下的贮存稳定性和加热时的固化速度的观点考虑，其可以使用各种化合物。在实际的工序中，通过在170～250℃，1～3小时的固化条件下进行固化，而获得希望的粘接强度。
然而，随着近来半导体元件的高集成化、液晶元件的高精细化，元件之间和线路之间的间距不断变窄，因此固化时的加热导致对周边部件产生了不利影响。此外，为了低成本化，而需要提高生产量，并要求在更低的温度下且在短时间内固化，也就是说，要求低温快速固化的粘接。为了实现该低温快速固化，必须使用活化能量低的热潜在性催化剂，然而已知的是，很难兼具活化能量低以及在室温附近的贮存稳定性这两种性能。
对此，最近，将丙烯酸酯衍生物或甲基丙烯酸酯衍生物等自由基聚合性化合物和作为自由基聚合引发剂的过氧化物结合使用的自由基固化型粘接剂正受到关注。自由基固化型粘接剂，由于其中作为反应活性种子的自由基的反应性强，因此可以在短时间内固化（例如，参见专利文献2）。此外，还提出了使用氨酯丙烯酸酯化合物作为自由基聚合性化合物的自由基固化型粘接剂，其中所述的氨酯丙烯酸酯化合物通过酯键而被赋予了柔软性和挠性（参见专利文献3、4）。
专利文献1：日本特开平1－113480号公报
专利文献2：日本特开2002－203427号公报
专利文献3：日本特开2001－262079号公报
专利文献4：日本特开2002－285128号公报
发明内容
发明要解决的问题
然而，专利文献2等中所记载的以往的自由基固化型粘接剂，由于固化时的固化收缩大，因此和使用环氧树脂时相比，存在有粘接强度差的问题。
此外，专利文献3、4等中所记载的使用氨酯丙烯酸酯的自由基固化型粘接剂，由于在分子内具有酯键，因此存在有固化后的弹性率和玻璃化转变温度等粘接剂物性下降，以及吸水率上升，耐水解性下降的问题。因此，当其用于半导体元件和液晶显示元件的粘接剂时，存在有在高温高湿环境下（例如，85℃/85％RH）无法获得足够的连接可靠性的问题。
进一步，上述的氨酯丙烯酸酯在室温下为低粘度的液状，因此当其用作膜状粘接剂的配合成分时，可知表示表面胶粘程度的表面胶粘力增加，并且在操作性方面存在有问题。
本发明鉴于上述以往技术所存在的问题而进行，其目的是提供一种在低温下短时间内（例如，160℃下10秒种）固化、在连接电路部件时可以获得具有优异粘接强度的电路部件的连接结构体、并且能够充分抑制所得的连接结构体在高温高湿环境下的连接可靠性降低、此外操作性也优异的粘接剂，以及使用该粘接剂的电路部件的连接结构体。
另外，本说明书中，所谓“能够充分抑制连接结构体在高温高湿环境下的连接可靠性降低”，是指即使在高温高湿环境下经过长时间的情况下，也可以充分抑制电路部件间的粘接强度的降低，以及相对的连接端子间的连接电阻的上升。
解决问题的方法
为了实现上述目的，本发明提供一种粘接剂，其含有（a）热塑性树脂、（b）自由基聚合性化合物，以及（c）自由基聚合引发剂，其中（b）自由基聚合性化合物在30℃以下为固体。
根据本发明的粘接剂，可以在低温且短时间内固化，在连接了电路部件时可以获得具有优异粘接强度的电路部件的连接结构体，并且能够充分抑制所得的连接结构体在高温高湿环境下的连接可靠性降低，此外操作性也优异。虽然使用本发明的粘接剂可以获得这些效果的原因尚未明确，但是可以认为，（b）自由基聚合性化合物在操作温度（例如，30℃以下）下以固体存在，从而相对减少了液状成分是理由之一。
本发明的粘接剂，优选进一步含有（d）在分子内具有至少一个以上磷酸基的乙烯系化合物。由此，在低温并且短时间的固化条件下，可以获得更优异的粘接强度。
（a）热塑性树脂优选含有选自苯氧基树脂、聚酯树脂、聚氨酯树脂、聚酯型聚氨酯树脂、丁醛树脂、丙烯酸树脂、聚酰亚胺树脂的至少一种树脂。由此，可以更充分地抑制在高温高湿环境下经长时间后的粘接强度的降低。
本发明的粘接剂，优选进一步含有（e）导电性粒子。从而，由于可以对粘接剂赋予导电性或各向异性导电性，因此可以根据具有连接端子的电路部件彼此之间的连接用途等适当使用粘接剂。此外，可以充分降低通过上述粘接剂电连接的连接端子间的连接电阻。
此外，本发明提供一种电路部件的连接结构体，其为，将具有第一连接端子的第一电路部件和具有第二连接端子的第二电路部件配置成使所述第一连接端子和所述第二连接端子相对，使上述本发明的粘接剂存在于对向配置的所述第一连接端子和所述第二连接端子之间，进行加热加压，使所述第一连接端子和所述第二连接端子电连接而成。
这种连接结构体由于使用上述本发明的粘接剂，因此可以充分提高电路部件的粘接强度，并且可以充分抑制高温高湿环境下的连接可靠性的降低。
发明效果
根据本发明，可以提供一种在低温且短时间内固化、在连接电路部件时可以获得具有优异粘接强度的电路部件的连接结构体、并且能够充分抑制所得的连接结构体在高温高湿环境下的连接可靠性降低、此外操作性也优异的粘接剂，以及使用该粘接剂的电路部件的连接结构体。
附图的简单说明
[图1]表示本发明的电路部件的连接结构体的一种实施方式的概略截面图。
符号说明
7…导电性粒子，10…电路连接部件，11…树脂，20、30…电路部件，21、31…电路基板，22、32…电路电极。
具体实施方式
以下，对于本发明的优选实施方式进行详细说明。另外，在本说明书中，“熔点”是指由差示扫描热量测定所得的差示扫描热量测定曲线的发热峰温度。此外，上述差示扫描热量测定，例如可以使用差示扫描量热计（珀金埃尔默公司制造，Pyris DSC7），以10mL/min的流量通入空气，并在25℃保持后，在以10℃/min升温至120℃的条件下进行。
作为本发明中所用的（a）热塑性树脂，没有特别限制，可以使用公知材料。作为这种聚合物，可以使用聚酰亚胺、聚酰胺、苯氧基树脂类、聚（甲基）丙烯酸酯类、聚酰亚胺类、聚氨酯类、聚酯类、聚酯型聚氨酯类、聚乙烯缩丁醛类、乙烯－乙酸乙烯酯共聚物等。这些聚合物，可以根据需要单独使用，或将2种以上混合使用。进一步，这些聚合物中可以含有硅氧烷键或氟取代基。这些聚合物，只要是混合的树脂相互之间完全相容，或者是产生微相分离形成浑浊的状态，就可以很好地使用。上述聚合物的分子量越大，则越容易得到成膜性，并且可以将对用作粘接剂的流动性产生影响的熔融粘度设定为较宽范围。分子量并没有特别限制，但重均分子量通常优选为5,000～500,000，并更优选为10,000～100,000。当该值不到5,000时，成膜性有变差的倾向，而当其超过500,000时，和其它成分的相容性存在有变差的倾向。
作为本发明中所用的（b）自由基聚合性化合物，可以是苯乙烯衍生物、马来酰亚胺衍生物或分子内具有一个以上丙烯酰基或甲基丙烯酰基（以后，称为（甲基）丙烯酰基）的化合物，并且只要是在30℃以下为固体的物质，就没有特别限制，可以使用公知材料。
此处，“在30℃以下为固体”，是指将上述化合物在30℃以下单独静置时，显示为蜡状、蜡状、晶体状、玻璃状、粉状等没有流动性的固体状态，或者是对上述化合物进行上述差示扫描热量测定，其熔点超过30℃。
作为（b）自由基聚合性化合物的具体例子，可以列举N,N’－亚甲基二丙烯酰胺、二丙酮丙烯酸酰胺、N－羟甲基丙烯酰胺、N－苯基甲基丙烯酰胺、2－丙烯酰胺－2－甲基丙烷磺酸、三（2－丙烯酰氧基乙基）异氰脲酸酯、N－苯基马来酰亚胺、N－邻甲苯基马来酰亚胺、N－间甲苯基马来酰亚胺、N－对甲苯基马来酰亚胺、N－（邻甲氧基苯基）马来酰亚胺、N－（间甲氧基苯基）马来酰亚胺、N－（对甲氧基苯基）马来酰亚胺、N－甲基马来酰亚胺、N－乙基马来酰亚胺、N－辛基马来酰亚胺、4,4’－二苯基甲烷二马来酰亚胺、间亚苯基二马来酰亚胺、3,3’－二甲基－5,5’－二乙基－4,4’－二苯基甲烷二马来酰亚胺、4－甲基－1,3－亚苯基二马来酰亚胺、N－甲基丙烯酰氧基马来酰亚胺、N－丙烯酰氧基马来酰亚胺、1,6－二马来酰亚胺－（2,2,4－三甲基）己烷、N－甲基丙烯酰氧基琥珀酸酰亚胺、N－丙烯酰氧基琥珀酸酰亚胺、2－萘基甲基丙烯酸酯、2－萘基丙烯酸酯、季戊四醇四丙烯酸酯、二乙烯基亚乙基尿素、二乙烯基亚丙基尿素、乙烯基己内酰胺、乙烯基咔唑、2－聚苯乙烯基甲基丙烯酸乙酯、N－苯基－N’－（3－甲基丙烯酰氧基－2－羟丙基）－对亚苯基二胺、N－苯基－N’－（3－丙烯酰氧基－2－羟丙基）－对亚苯基二胺、二（4－乙烯基苯基）砜、2－叔丁氧基－6－乙烯基萘、四甲基哌啶甲基丙烯酸酯、四甲基哌啶丙烯酸酯、五甲基哌啶甲基丙烯酸酯、五甲基哌啶丙烯酸酯、十八烷基丙烯酸酯、N－叔丁基丙烯酰胺、二丙酮丙烯酰胺、N－羟甲基丙烯酸酰胺、下述通式（A）～（J）所表示的化合物。这些化合物中，从快速固化性的观点考虑，优选具有（甲基）丙烯酰基的化合物，从低温固化性和操作性的观点考虑，优选熔点为50～100℃的化合物。这些化合物，可以根据需要单独使用，或混合使用。
[化1]
Figure BDA00003205245100061
（此处，l表示1～10的整数。）
[化2]
Figure BDA00003205245100062
[化3]
Figure BDA00003205245100063
（此处，R1表示氢或甲基，R2表示氢或甲基，m表示15～30的整数。）
[化4]
Figure BDA00003205245100064
（此处，R3表示氢或甲基，R4表示氢或甲基，n表示15～30的整数。）
[化5]
Figure BDA00003205245100065
（此处，R5表示氢或甲基。）
[化6]
（此处，R6表示氢或甲基，o表示1～10的整数。）
[化7]
Figure BDA00003205245100072
（此处，R7表示氢或下述通式（a）、（b）所示的有机基团，p表示1～10的整数。）
[化8]
Figure BDA00003205245100073
[化9]
Figure BDA00003205245100074
[化10]
Figure BDA00003205245100075
（此处，R8表示氢或下述通式（c）、（d）所示的有机基团，q表示1～10的整数。）
[化11]
Figure BDA00003205245100076
[化12]
Figure BDA00003205245100081
[化13]
Figure BDA00003205245100082
（此处，R9表示氢或甲基。）
[化14]
Figure BDA00003205245100083
（此处，R10表示氢或甲基。）
（b）自由基聚合性化合物的添加量，相对于100质量份（a）热塑性树脂，优选为1～200质量份，更优选为5～100质量份。当添加量不到1质量份时，固化后的耐热性下降，同时随着膜表面的胶粘性增加，操作性下降。此外，当其超过200质量份时，在用作膜时，成膜性下降，同时固化后的膜质变脆，粘接力降低。本发明中，作为操作性的指标，可以使用在25～30℃时的表面胶粘力，并且，从粘接剂的操作性和被粘接物的临时固定性观点考虑，希望表面胶粘力为50gf以下。
作为本发明中所用的（c）自由基聚合引发剂，可以使用以往公知的过氧化物或偶氮化合物等公知化合物，从稳定性、反应性、相容性的观点考虑，优选1分钟半衰期温度为90～175℃，并且分子量为180～1,000的过氧化物。作为这种（c）自由基聚合引发剂的具体例子，可以列举1,1,3,3－四甲基丁基过氧化新癸酸酯、二（4－叔丁基环己基）过氧化二碳酸酯、二（2－乙基己基）过氧化二碳酸酯、枯基过氧化新癸酸酯、1,1,3,3－四甲基丁基过氧化新癸酸酯、二月桂酰基过氧化物、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、叔丁基过氧化新癸酸酯、叔丁基过氧化戊酸酯、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、叔己基过氧化－2－乙基己酸酯、叔丁基过氧化－2－乙基己酸酯、叔丁基过氧化新庚酸酯、叔戊基过氧化－2－乙基己酸酯、二叔丁基过氧化六氢对苯二甲酸酯、叔戊基过氧化－3,5,5－三甲基己酸酯、3－羟基－1,1－二甲基丁基过氧化新癸酸酯、1,1,3,3－四甲基丁基过氧化－2－乙基己酸酯、叔戊基过氧化新癸酸酯、叔戊基过氧化－2－乙基己酸酯、二（3－甲基苯甲酰基）过氧化物、二苯甲酰基过氧化物、二（4－甲基苯甲酰基）过氧化物、2,2’－偶氮二－2,4－二甲基戊腈、1,1’－偶氮二（1－乙酰氧基－1－苯基乙烷）、2,2’－偶氮二异丁腈、2,2’－偶氮二（2－甲基丁腈）、二甲基－2,2’－偶氮二异丁腈、4,4’－偶氮二（4－氰基戊酸）、1,1’－偶氮二（1－环己烷腈）、叔己基过氧化异丙基单碳酸酯、叔丁基过氧化马来酸、叔丁基过氧化－3,5,5－三甲基己酸酯、叔丁基过氧化月桂酸酯、2,5－二甲基－2,5－二（3－甲基苯甲酰基过氧化）己烷、叔丁基过氧化－2－乙基己基单碳酸酯、叔己基过氧化苯甲酸酯、2,5－二甲基－2,5－二（苯甲酰基过氧化）己烷、叔丁基过氧化苯甲酸酯、二丁基过氧化三甲基己二酸酯、叔戊基过氧化正辛酸酯、叔戊基过氧化异壬酸酯、叔戊基过氧化苯甲酸酯等。这些化合物，可以单独使用，或者将2种以上的化合物混合使用。
此外，作为本发明中所用的（c）自由基聚合引发剂，还可以使用在150～750nm的光照射下产生自由基的化合物。作为这种化合物，没有特别限制，可以使用公知化合物，例如，Photoinitiation，Photopolymerization，andPhotocuring，J.－P.Fouassier，Hanser Publishers（1995年），p17～p35中所记载的α－乙酰氨基酚衍生物和氧化膦衍生物对于光照射的感度高，因此更优选。这些化合物可以单独使用，或者与上述过氧化物或偶氮化合物混合使用。
本发明的（c）自由基聚合引发剂的添加量，相对于100质量份（a）热塑性树脂，优选为0.1～30质量份，并进一步优选为2～20质量份。当自由基聚合引发剂不到0.1质量份时，固化不足，而当其超过30质量份时，放置稳定性下降。
作为本发明中所用的（d）在分子内具有至少一个以上磷酸基的乙烯系化合物，没有特别限制，可以使用公知物质，更优选在分子内具有至少一个以上的自由基聚合性优异的（甲基）丙烯酰基作为乙烯基的磷酸（甲基）丙烯酸酯化合物。作为这种化合物，可以列举下述通式（K）～（M）所示的化合物。
[化15]
Figure BDA00003205245100101
（此处，R11表示丙烯酰氧基或甲基丙烯酰氧基，R12表示氢或甲基，r、s独立地表示1～8的整数。）
[化16]
Figure BDA00003205245100102
（此处，R13表示丙烯酰氧基或甲基丙烯酰氧基，t、u、v独立地表示1～8的整数。）
[化17]
Figure BDA00003205245100103
（此处，R14表示丙烯酰氧基或甲基丙烯酰氧基，R15表示氢或甲基，w、x独立地表示1～8的整数。）
作为（d）在分子内具有至少一个以上磷酸基的乙烯系化合物的具体例子，可以列举酸式磷酰氧基乙基甲基丙烯酸酯、酸式磷酰氧基乙基丙烯酸酯、酸式磷酰氧基丙基甲基丙烯酸酯、酸式磷酰氧基聚氧乙二醇单甲基丙烯酸酯、酸式磷酰氧基聚氧丙二醇单甲基丙烯酸酯、2－（甲基）丙烯酰氧基乙基磷酸酯、2,2’－二（甲基）丙烯酰氧基二乙基磷酸酯、EO改性磷酸二甲基丙烯酸酯、磷酸改性环氧基丙烯酸酯、磷酸乙烯醇酯等。
在添加（d）在分子内具有至少一个以上磷酸基的乙烯系化合物时，其添加量相对于100质量份（a）热塑性树脂，优选为0.05～30质量份，更优选为0.1～20质量份。当添加量不到0.05质量份时，难以获得高粘接强度，而当其超过30质量份时，固化后的粘接剂物性显著降低，可靠性可能下降。
作为本发明中所用的（e）导电性粒子，可以列举Au、Ag、Ni、Cu、焊锡等金属粒子或碳等。此外，还可以是以非导电性的玻璃、陶瓷、塑料等为核，并在该核上被覆有上述金属、金属粒子或碳而成的材料。当导电性粒子是以塑料为核，并在该核上被覆有上述金属、金属粒子或碳而成的材料或热熔融金属粒子时，由于在加热加压下具有变形性，因此连接时和电极的接触面积增加，可靠性提高，因此优选。此外，进一步用高分子树脂等被覆这些导电性粒子的表面所得的微粒，在增加导电性粒子配合量时，可以抑制因粒子相互之间的接触而产生的短路，提高电极电路间的绝缘性，因此可以适当地单独使用，或与导电性粒子混合使用。
该（e）导电性粒子的平均粒径，从分散性、导电性的观点考虑，优选为1～18μm。
（e）导电性粒子的添加量，没有特别限制，以粘接剂组合物的总体积为基准，优选为0.1～30体积％，更优选为0.1～10体积％。当该值不到0.1体积％时，存在有导电性变差的倾向，当其超过30体积％时，存在有产生电路短路的倾向。另外，体积％是基于23℃时的固化前的各成分的体积来确定的，各成分的体积，可以利用比重由重量换算为体积。此外，还可以将不溶解或膨润该成分，但能很好地润湿该成分的适当溶剂（水、醇等）放入量筒中，再加入该成分，求出增加的体积，并将其作为所述体积。
为了提高交联率和确保固化物的韧性，本发明的粘接剂，在30℃以下为固体的上述自由基聚合性化合物的同时，还可以适当添加多官能（甲基）丙烯酸酯化合物。
作为多官能（甲基）丙烯酸酯化合物的具体例子，可以列举环氧基（甲基）丙烯酸酯低聚物、尿烷（甲基）丙烯酸酯低聚物、聚醚（甲基）丙烯酸酯低聚物、聚酯（甲基）丙烯酸酯低聚物等低聚物、三羟甲基丙烷三（甲基）丙烯酸酯、聚乙二醇二（甲基）丙烯酸酯、聚亚烷基二醇二（甲基）丙烯酸酯、二环戊烯基（甲基）丙烯酸酯、二环戊烯氧基乙基（甲基）丙烯酸酯、新戊二醇二（甲基）丙烯酸酯、二季戊四醇六（甲基）丙烯酸酯、异氰脲酸改性2官能（甲基）丙烯酸酯、异氰脲酸改性3官能（甲基）丙烯酸酯、二苯氧基乙醇芴丙烯酸酯、在双酚芴二缩水甘油醚的缩水甘油基上加成了（甲基）丙烯酸的环氧基（甲基）丙烯酸酯、在双酚芴二缩水甘油醚的缩水甘油基上加成了乙二醇或丙二醇而得到的化合物中导入（甲基）丙烯酰氧基而成的化合物、下述通式（N）、（O）所示的化合物等多官能（甲基）丙烯酸酯化合物。这些化合物可以根据需要单独使用，或者混合使用。
[化18]
Figure BDA00003205245100121
（此处，R16表示氢或甲基，R17表示氢或甲基，y表示1～8的整数，z表示1～8的整数。）
[化19]
Figure BDA00003205245100122
（此处，R18表示氢或甲基，R19表示氢或甲基，a表示1～8的整数，b表示0～8的整数。）
为了进一步控制固化速度以及提高贮存稳定性，在本发明的粘接剂中可以适当添加稳定剂。作为这种稳定剂，没有特别限制，可以使用公知的化合物，优选苯醌、氢醌等醌衍生物、4－甲氧基苯酚、4－叔丁基邻苯二酚等苯酚衍生物、2,2,6,6－四甲基哌啶－1－氧基、4－羟基－2,2,6,6－四甲基哌啶－1－氧基等氨氧基（aminoxyl）衍生物、四甲基哌啶基甲基丙烯酸酯等位阻胺衍生物。
在添加稳定剂时，其添加量相对于100质量份（a）热塑性树脂，优选为0.01～30质量份，更优选为0.05～10质量份。当添加量不到0.01质量份时，添加效果可能会显著下降，而当其超过30质量份时，和其它成分的相容性可能会下降。
在本发明的粘接剂中，还可以适当添加以烷氧基硅烷衍生物或硅氮烷衍生物为代表的偶联剂以及粘接促进剂、流平剂、尿素树脂、三聚氰胺树脂等粘接助剂。作为粘接助剂，优选为下述通式（P）所示的化合物，并且它们可以单独使用，或将2种以上的化合物混合使用。
[化20]
Figure BDA00003205245100131
（此处，R20、R21、R22独立地表示氢、碳数为1～5的烷基、碳数为1～5的烷氧基、碳数为1～5的烷氧基羰基、芳基，R23表示（甲基）丙烯酰氧基、乙烯基、异氰酸酯基、咪唑基、巯基、氨基、甲基氨基、二甲基氨基、苄基氨基、苯基氨基、环己基氨基、吗啉基、哌嗪基、酰脲基、缩水甘油基，c表示1～10的整数。）
为了缓和应力和提高粘接性，在本发明的粘接剂中，可以添加橡胶成分。作为橡胶成分的具体例子，可以列举聚异戊二烯、聚丁二烯、羧基末端聚丁二烯、羟基末端聚丁二烯、1,2－聚丁二烯、羧基末端1,2－聚丁二烯、羟基末端1,2－聚丁二烯、丙烯酸橡胶、苯乙烯－丁二烯橡胶、羟基末端苯乙烯－丁二烯橡胶、丙烯腈－丁二烯橡胶、在聚合物末端含有羧基、羟基、（甲基）丙烯酰基或吗啉基的丙烯腈－丁二烯橡胶、羧基化腈橡胶、羟基末端聚（氧丙烯）、烷氧基甲硅烷基末端聚（氧丙烯）、聚（氧四亚甲基）二醇、聚烯烃二醇、聚ε－己内酯、丙烯酸橡胶。
作为上述橡胶成分，从粘接性提高的观点考虑，优选为在侧链或末端上含有作为高极性基团的氰基、羧基的橡胶成分，进一步，从流动性提高的观点考虑，更优选为液状橡胶。
作为液状橡胶的具体例子，可以列举液状丙烯腈－丁二烯橡胶，在聚合物末端含有羧基、羟基、（甲基）丙烯酰基或吗啉基的液状丙烯腈－丁二烯橡胶，液状羧基化腈橡胶，优选作为极性基团的丙烯腈含量为10～60％的橡胶。这些化合物可以单独使用，或将2种以上的化合物混合使用。
本发明的粘接剂，在室温下为液状时，可以以糊状使用。在室温下为固体时，除了加热使用外，还可以使用溶剂将其糊化后使用。作为可用的溶剂，只要是与粘接剂组合物和添加剂没有反应性，并且显示出充分的溶解性的物质，就没有特别限制，优选在常压下的沸点为50～150℃的溶剂。当沸点不到50℃时，在室温下放置时可能会挥发，因而在开放体系中使用受到限制。此外，当沸点超过150℃时，溶剂难以挥发，可能对粘接后的可靠性产生不良影响。
本发明的粘接剂还可以形成膜状来使用。粘接剂组合物，可以通过将根据需要加入了溶剂等的溶液涂布在氟树脂膜、聚对苯二甲酸乙二醇酯膜、脱模纸等剥离性基材上，或者使上述溶液浸渍无纺布等基材，并放置在剥离性基材上，除去溶剂等，从而形成膜来使用。在以膜的形状进行使用时，从操作性等观点考虑，更加便利。
上述粘接剂，通过将加热和加压并用，可以使被粘接物粘接。加热温度没有特别限制，例如，可以为100～250℃，为了充分抑制因固化时加热而对周围部件所产生的不良影响，优选为100～180℃。压力，只要是不会对被粘接物产生损伤的范围，就没有特别限制，通常优选为0.1～10MPa。这些加热和加压的时间，可以为0.5秒钟～120秒钟，从低成本化的观点考虑，优选为0.5秒钟～10秒钟。例如，可以通过140～200℃、3MPa、10秒钟的加热进行粘接。
本发明的粘接剂，可以用作热膨胀系数不同的不同种被粘接物的粘接剂。具体来说，可以用作各向异性导电粘接剂，以银糊、银膜等为代表的电路连接材料，CSP用弹性体、CSP用底填材料、芯片焊接（die bonding）膜、芯片焊接糊等为代表的半导体元件粘接材料。
本发明的电路部件的连接结构体，是将具有第一连接端子的第一电路部件和具有第二连接端子的第二电路部件配置成使第一连接端子和第二连接端子相对向，使上述粘接剂存在于对向配置的第一连接端子和第二连接端子之间，进行加热加压，使第一连接端子和第二连接端子电连接的连接结构体。
图1是表示本发明的电路部件的连接结构体的一个实施方式的概略截面图。如图1所示，本实施方式的连接结构体，具有彼此相对向的第一电路部件20和第二电路部件30，并且在第一电路部件20和第二电路部件30之间，设置有将它们连接的电路连接部件10。
第一电路部件20，具有电路基板（第一电路基板）21和在电路基板21的主面21a上所形成的电路电极（第一电路电极）22。另外，在第一电路基板21的主面21a上，可以根据情况形成绝缘层（未图示）。
另一方面，第二电路部件30，具有电路基板（第二电路基板）31和在电路基板31的主面31a上所形成的电路电极（第二电路电极）32。此外，在电路基板31的主面31a上，也可以根据情况形成绝缘层（未图示）。
作为第一和第二电路部件20、30，只要形成有需要电连接的电极，就没有特别限制。具体来说，可以列举用于液晶显示器的由ITO等形成电极的玻璃或塑料基板、印刷线路板、陶瓷线路板、挠性线路板、半导体硅芯片等。它们可以根据需要组合使用。在本实施方式中，主要使用印刷线路板以及由聚酰亚胺等有机物所形成的材质，并且还可以使用铜、铝等金属或ITO（indium tinoxide）、氮化硅（SiNx）、二氧化硅（SiO2）等无机材质等具有多种表面状态的电路部件。
电路连接部件10，由上述粘接剂的固化物形成。该电路连接部件10，含有树脂11和导电性粒子7。导电性粒子7不仅配置在相对向的电路电极22和电路电极32之间，而且还配置在主面21a、31a之间。在电路部件的连接结构中，电路电极22、32，通过导电性粒子7而被电连接。即，导电性粒子7与电路电极22、32这两者直接接触。
此处，导电性粒子7是前面所述的（e）导电性粒子，树脂11是上述粘接剂的固化物。
在该电路部件的连接结构中，如上所述，相对向的电路电极22和电路电极32通过导电性粒子7而被电连接。因此，电路电极22、32之间的连接电阻被充分降低。从而，电路电极22、32之间的电流可以顺畅通过，并且可以充分发挥电路所具有的功能。另外，当电路连接部件10不含有导电性粒子7时，通过使电路电极22和电路电极32直接接触，而进行电连接。
本实施方式的连接结构体的制造方法，即电路部件20、30的连接方法，例如如下所述。首先，使上述粘接剂存在于电路部件20、30之间。这时，将电路部件20、30配置成使电路电极22和32相对向。接着，一边隔着电路部件20、30加热粘接剂，一边在它们的叠层方向上加压，实施粘接剂的固化处理，形成电路连接部件10。固化处理，可以在例如上述的加热温度、加压压力下进行，并且其方法可以根据粘接剂适当选择。
由于电路连接部件10由上述粘接剂的固化物构成，因此电路连接部件10相对于电路部件20或30的粘接强度充分提高，并且可以充分抑制在高温高湿环境下的连接可靠性的降低。
另外，虽然在上述实施方式中对于含有导电性粒子的情况作了说明，但本发明的电路部件的连接结构体也可以不含有导电性粒子。在不含有导电性粒子时，通过使相对的电极互相直接接触而进行电连接。
实施例
以下，基于实施例具体说明本发明，但本发明并不限定于此。
[尿烷树脂的合成]
将450质量份重均分子量为2000的聚亚丁基己二酸酯二醇、450质量份平均分子量为2000的聚四亚甲基二醇和100质量份1,4－丁二醇，溶解在4000质量份甲乙酮中，并加入390质量份二苯基甲烷二异氰酸酯，使其在70℃反应60分钟，得到尿烷树脂。通过凝胶渗透色谱法（GPC）测定所得的尿烷树脂的重均分子量，结果为10万。
（实施例1～9、比较例1～3）
作为热塑性树脂，将上述尿烷树脂溶解在甲乙酮和甲苯的混合溶剂中而成的固体成分为30重量％的溶液，和以固体成分为40重量％溶解在甲乙酮中的苯氧基树脂（ZX－1356－2，东都化成株式会社制商品名）或以固体成分为40重量％溶解在甲乙酮和甲苯的混合溶剂中的聚酯型聚氨酯树脂（UR－1350，东洋纺织株式会社制商品名）并用。
作为自由基聚合性化合物，单独使用在30℃下为固体的环氧基丙烯酸酯（VR－60以及VR－90，昭和高分子株式会社制商品名），或者将作为液状自由基聚合性化合物的异氰脲酸EO改性三丙烯酸酯（M－215，东亚合成株式会社制商品名）和氨酯丙烯酸酯（UA6100，新中村化学株式会社制商品名）并用。
作为酸性化合物，使用2－（甲基）丙烯酰氧基乙基磷酸酯（轻酯（ライトエステル）P－2M，共荣社株式会社制商品名）。
作为自由基聚合引发剂，使用叔己基过氧化－2－乙基己酸酯（PERHEXYL O，日本油脂株式会社制商品名）。
此外，制作在以聚苯乙烯为核的粒子表面上设置有厚度为0.2μm的镍层，并在该镍层的外侧设置有厚度为0.02μm的金层，并且平均粒径为4μm、比重为2.5的导电性粒子。
以下述表1所示的固体重量比配合上述成分，再将上述导电性粒子以1.5体积％的量配合分散。使用涂布装置将其涂布在厚度为80μm的氟树脂膜上，并在70℃热风干燥10分钟，得到粘接剂层的厚度为18μm的实施例1～9、比较例1～3的膜状粘接剂。
[表1]
Figure BDA00003205245100171
使用粘性测试机（株式会社レスカ制，LT25A－500）（基础温度为30℃），并根据JISZ－0237测定实施例1～9、比较例1～3的膜状粘接剂的表面胶粘力。
[连接电阻、粘接强度的测定]
将实施例1～9、比较例1～3的膜状粘接剂，设置在具有500根线宽为25μm、间距为50μm、厚度为12μm的铜电路的挠性线路板（FPC）和形成有0.2μm氧化铟（ITO）薄层的玻璃（厚度为1.1mm，表面电阻为20Ω/□）之间。使用热压装置（加热方式：恒热型，东丽工程株式会社制造），在160℃、3MPa下加热加压10秒钟，将所述材料在宽度为2mm上进行连接，制作连接体。
在粘接后即刻以及在85℃、85％RH的高温高湿中保持168小时后（试验后），使用万用表测定该连接体的相邻电路间的电阻值。电阻值以相邻电路间的37处电阻的平均值进行表示。
此外，根据JIS－Z0237，使用90度剥离法测定该连接体的粘接强度，并进行评价。此处，粘接强度的测定装置，使用东洋ボールドウィン株式会社制天希隆（テンシロン）UTM－4（剥离速度50mm/min，25℃）。如上所进行的膜状粘接剂的表面胶粘力、连接电阻以及粘接强度的测定结果示于下述表2。
[表2]
Figure BDA00003205245100191
由此可知，实施例1～9所得的粘接剂组合物，在加热温度160℃时，在粘接后即刻以及在85℃、85％RH的高温高湿槽中保持168小时后（试验后），显示出约3Ω以下的良好连接电阻以及400N/m以上的良好粘接强度。进一步，由此可知，表示表面胶粘程度的表面胶粘力低，操作性优异。
相反可知，不使用本发明中在30℃下为固体的自由基聚合性化合物的比较例1，其表面胶粘力高，操作性差，除此之外，粘接强度也低。并且还可知，在比较例2、3中，虽然显示出了良好的连接电阻和粘接强度，但是表面胶粘力大，并且在操作性方面存在有问题。

Claims (1)

1.一种粘接剂，其含有（a）热塑性树脂、（b）在30℃以下为固体的自由基聚合性化合物以及（c）自由基聚合引发剂。
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