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CN102934243B - 光反射性各向异性导电浆料和发光装置 - Google Patents

光反射性各向异性导电浆料和发光装置 Download PDF

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Publication number
CN102934243B
CN102934243B CN201180028298.1A CN201180028298A CN102934243B CN 102934243 B CN102934243 B CN 102934243B CN 201180028298 A CN201180028298 A CN 201180028298A CN 102934243 B CN102934243 B CN 102934243B
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Prior art keywords
light
light reflective
anisotropic conductive
particle
conductive paste
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CN102934243A (zh
Inventor
马越英明
波木秀次
石神明
青木正治
蟹泽士行
新家由久
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Dexerials Corp
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Dexerials Corp
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
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    • H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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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
    • 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
    • C08G59/40—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 curing agents used
    • C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
    • 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
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    • 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
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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Abstract

一种光反射性各向异性导电浆料，其作为在配线板上倒装芯片安装发光二极管元件(LED)等发光元件来制造发光装置时使用的各向异性导电浆料，在没有在LED上设置导致制造成本增加的光反射层、为了改善发光效率而混合光反射性绝缘颗粒的情况下，可以抑制高温环境下的发光元件与配线板的粘合强度的降低，而且在TCT后还可以抑制导通可靠性的降低，该光反射性各向异性导电浆料是将导电颗粒和光反射性绝缘颗粒分散在热固化性树脂组合物中形成的。热固化性树脂组合物含有环氧化合物和热催化型固化剂。

Description

光反射性各向异性导电浆料和发光装置
技术领域
本发明涉及用于在配线板上各向异性导电连接发光二极管元件(LED)等发光元件的光反射性各向异性导电浆料、使用该各向异性导电浆料在配线板上安装发光元件而形成的发光装置。
背景技术
使用发光二极管元件(LED)的发光装置被广泛使用，老式发光装置的结构如图8所示，使用芯片接合(Die Bond)粘合剂32将LED33接合在基板31上，再通过金属线37将其上面的p电极34和n电极35引线接合(Wire Bonding)在基板31的连接端子36上，LED33整体用透明模压树脂38密封。然而，当为图7的发光装置时，LED33发出的光中，射到上面侧的400～500nm的波长的光被金属线吸收，射到下面侧的一部分光被芯片接合粘合剂32吸收，存在着LED33的发光效率降低的问题。
因此，如图7所示，有人提出倒装芯片(Flip chip)安装LED33 (专利文献1)。在该倒装芯片安装技术中，在p电极34和n电极35上分别形成有凸块39 (bump 39)，并且在LED33的凸块形成面上设有光反射层40，以使p电极34和n电极35绝缘。而且，使用各向异性导电浆料41并使其固化，以连接固定LED33和基板31。因此，在图7的发光装置中，射向LED33上方的光没有被金属线吸收，而射向下方的光几乎都被光反射层40反射而射到上方，因此发光效率(光输出效率)不会降低。需要说明的是，作为这样的各向异性导电浆料41，在包含作为固化成分的环氧化合物和通过加成反应能够使环氧化合物固化的咪唑系潜在性固化剂的热固化性树脂组合物中分散有导电颗粒的各向异性导电浆料被广泛使用。
现有技术文献
专利文献
专利文献1：日本特开平11-168235号公报。
发明内容
发明所要解决的课题
但是，在专利文献1的技术中，必须通过金属蒸镀法等在LED33上设置光反射层40，以使p电极34和n电极35绝缘，存在着无法避免制造成本上升的问题。另一方面，在没有设置光反射层40的情况下，已固化的各向异性导电浆料或各向异性导电膜中的被金、镍或铜包覆的导电颗粒的表面呈茶色至暗茶色，另外，使导电颗粒分散的环氧树脂粘合剂本身也因通常用于使其固化的咪唑系潜在性固化剂而呈茶色，还存在着难以使发光元件发出的光的发光效率(光输出效率)提高的问题。
因此，本发明人等为了使各向异性导电浆料本身具有光反射功能以使发光效率不会降低，在各向异性导电浆料中混合光反射性绝缘颗粒，而且使用酸酐系固化剂来代替导致固化物着色的咪唑系潜在性固化剂，从而赋予光反射性，使用该各向异性导电浆料在配线板上各向异性导电连接发光元件来制造发光装置时，出乎预料地发现不会使发光元件的发光效率降低。
然而，将如此制造的发光装置在高温环境下保持时，存在着在配线板上连接发光元件的各向异性导电浆料的粘合强度不仅在高温环境下、即使在将高温环境下的发光装置放置冷却达到的室温环境下也大幅降低的问题。另外，还存在着导通可靠性在热循环试验(TCT)后也大幅降低的问题。
本发明的目的在于解决以上现有的技术问题，提供光反射性各向异性导电浆料，其作为在配线板上倒装芯片安装发光二极管元件(LED)等发光元件来制造发光装置时使用的各向异性导电浆料，在LED上不设置导致制造成本增加的光反射层的情况下，为了改善发光效率而混合光反射性绝缘颗粒时，可以抑制高温环境下的发光元件与配线板的粘合强度的降低，而且在TCT后也可以抑制导通可靠性的降低。本发明还提供发光装置，该发光装置是使用该各向异性导电浆料在配线板上倒装芯片安装发光元件而形成的。
解决课题的方法
本发明人在对混合在构成光反射性各向异性导电浆料的热固化性树脂组合物中的环氧化合物用的固化剂进行研究时获得了以下经验：由于酸酐系固化剂与环氧化合物通过加成反应进行聚合，因此必需在聚合系统中大量混合酸酐系固化剂，同时由于酸酐系固化剂容易挥发，因此在进行各向异性导电连接时热固化性树脂组合物的成分组成比变大。在由于该成分组成比的变化各向异性导电浆料的粘合强度或导通可靠性大幅下降的假设下，发现：使用通过环氧基的开环聚合而少量存在且通过加热能够引发热固化性树脂组合物发生固化的热催化型固化剂来代替与环氧化合物进行加聚反应以促进热固化性树脂组合物发生固化的酸酐系固化剂，由此可以达到上述目的，从而完成了本发明。
即，本发明提供光反射性各向异性导电浆料，是用于在配线板上各向异性导电连接发光元件的光反射性各向异性导电浆料，其特征在于：是将导电颗粒和光反射性绝缘颗粒分散在热固化性树脂组合物中而形成的，该热固化性树脂组合物含有环氧化合物和热催化型固化剂。
本发明还提供发光装置，其中经由上述的光反射性各向异性导电浆料将发光元件以倒装芯片方式安装在配线板。
发明效果
用于在配线板上各向异性导电连接发光元件的本发明的光反射性各向异性导电浆料，其使用能够引发热阳离子聚合或热阴离子聚合的热催化型固化剂作为适合混合在含有环氧化合物作为主固化成分的热固化树脂组合物中的固化剂。因此，不是通过加聚反应、而是通过热催化型固化剂来引发热阳离子聚合或热阴离子聚合，连锁地进行聚合反应，因此在用于各向异性导电连接的加热加压时，不会出现热催化型固化剂挥发而导致热固化性树脂组合物的组成大幅变化的情况。因此，可以抑制高温环境下的粘合强度的降低或连接可靠性的降低。
附图说明
图1A是各向异性导电浆料用的光反射性导电颗粒的截面图；
图1B是各向异性导电浆料用的光反射性导电颗粒的截面图；
图2是本发明的发光装置的截面图；
图3是式(1a)的硼酸锍络合物的1H-NMR图谱；
图4是式(1b)的硼酸锍络合物的1H-NMR图谱；
图5是式(1A)的硼酸锍络合物的IR图谱；
图6A是式(1A)的硼酸锍络合物的1H-NMR图谱；
图6B是THF的1H-NMR图谱；
图7是现有的发光装置的截面图；
图8是现有的发光装置的截面图。
具体实施方式
本发明涉及用于在配线板上各向异性导电连接发光元件的光反射性各向异性导电浆料，其特征在于：是将导电颗粒和光反射性绝缘颗粒分散在热固化性树脂组合物中而形成的，热固化性树脂组合物含有环氧化合物和热催化型固化剂。
本发明中使用的热固化性树脂组合物含有环氧化合物作为主固化成分，还含有热催化型固化剂，该热催化型固化剂起到使上述环氧化合物进行热阴离子聚合或热阳离子聚合的聚合引发剂的作用。作为这样的热催化型固化剂，优选使用热阴离子聚合催化型固化剂或热阳离子聚合催化型固化剂，从得到高粘合力的角度考虑，更优选使用热阳离子聚合催化型固化剂。
作为热阴离子聚合催化型固化剂，可以使用作为热阴离子聚合催化剂而已知的路易斯碱，特别是从可以从较宽范围的条件中选择固化条件(温度、时间)的角度考虑，可以优选列举胺系路易斯碱。具体而言，可以列举：苄基二甲基胺(BDMA)、2,4,6-三(二甲基氨基甲基)苯酚(DMP-30)等叔胺化合物。
作为热阳离子聚合催化型固化剂，可以使用作为热阳离子聚合催化剂而已知的路易斯酸。例如可以列举：三氟化硼、芳族盐等。特别是从比较容易控制热分解的角度考虑，可以优选使用芳族盐。
作为这样的芳族盐，可以列举：芳族碘盐、芳族锍盐等，可以优选列举：式(1)所表示的硼酸锍络合物。
式(1)中，R1为芳烷基，R2为低级烷基，R3为氢原子或低级烷氧基羰基。X为卤原子，n为1～3的整数。
式(1)中，作为R1的芳烷基，可以列举：苄基、邻甲基苄基、(1-萘基)甲基、吡啶基甲基、蒽基甲基等。其中，在良好的速固化性和获取容易性方面，优选邻甲基苄基。
作为R2的低级烷基，可以列举：甲基、乙基、丙基、丁基等。其中，在良好的速固化性和获取容易性方面，优选甲基。
表示与锍残基结合的苯基的羟基或低级烷氧基羰氧基的个数的n为1～3的整数。作为这样的苯基，当n为1时，可以列举：4-羟基苯基或4-低级烷氧基羰氧基苯基、2-羟基苯基或2-低级烷氧基羰氧基苯基、3-羟基苯基或3-低级烷氧基羰氧基苯基等；当n为2时，可以列举：2,4-二羟基苯基或2,4-二低级烷氧基羰氧基苯基、2,6-二羟基苯基或2,6-二低级烷氧基羰氧基苯基、3,5-二羟基苯基或3,5-二低级烷氧基羰氧基苯基、2,3-二羟基苯基或2,3-二低级烷氧基羰氧基苯基。当n为3时，可以列举：2,4,6-三羟基苯基或2,4,6-三低级烷氧基羰氧基苯基、2,4,5-三羟基苯基或2,4,5-三低级烷氧基羰氧基苯基、2,3,4-三羟基苯基或2,3,4-三低级烷氧基羰氧基苯基等。其中，在良好的速固化性和获取容易性方面，优选n为1的4-羟基苯基或4-低级烷氧基羰氧基苯基、特别是4-甲氧基羰氧基苯基。
作为X的卤原子，有氟原子、氯原子、溴原子或碘原子。其中，从提高反应性的角度考虑，优选具有高的电子吸引性的氟原子。
因此，作为芳族锍盐的优选的具体例子，有以下的式(1a)、(1b)、(1c)和(1A)所表示的硼酸锍络合物，特别优选式(1A)所表示的硼酸锍络合物。
式(1)的硼酸锍络合物可以按照以下的反应式进行制备。需要说明的是，式(1)、(2)或(3)中的各取代基如上所述，即，R1为芳烷基、R2为低级烷基、R3为氢原子或低级烷氧基羰基。X为卤原子，n为1～3的整数。
即，R3为羟基的式(1)的硼酸锍络合物可以如下得到：将R3为羟基的式(2)的锑酸锍络合物(合成方法参照日本特开平10-245378号公报)溶解于乙酸乙酯等有机溶剂中，向该溶液中混合等摩尔量的式(3)的硼酸钠盐(合成方法参照日本特开平10-310587号公报)的水溶液，将所得的两层系混合物在20～80℃的温度下搅拌1～3小时，使式(3)的硼酸钠盐与式(2)的锑酸锍络合物反应，从而可以得到式(1)的硼酸锍络合物。关于式(1)的硼酸锍络合物的分离，通过将有机溶剂层分液、干燥，之后减压蒸发除去有机溶剂，以蒸发残余物的形式得到目的物，从而可以进行式(1)的硼酸锍络合物的分离。
另外，R3为低级烷氧基羰基的式(1)的硼酸锍络合物可以如下得到：将式(2)的锑酸锍络合物(合成方法参照日本特开2006-96742号公报。具体而言，在三乙胺的存在下、在乙腈中使氯甲酸低级烷基酯化合物(例如氯甲酸甲酯)与相当于从式(2)的络合物中除去甲酸酯残基而得到的化合物的羟基苯基锑酸锍络合物反应即可。)溶解于乙酸乙酯等有机溶剂中，向该溶液中混合等摩尔量的式(3)的硼酸钠盐(合成方法参照日本特开平10-310587号公报)的水溶液，将所得的两层系混合物在20～80℃的温度下搅拌1～3小时，使式(3)的硼酸钠盐与式(2)的锑酸锍络合物反应，从而可以得到式(1)的硼酸锍络合物。关于式(1)的硼酸锍络合物的分离，通过将有机溶剂层分液、干燥，之后减压蒸发除去有机溶剂，从而以蒸发残余物的形式得到目的物，从而可以进行式(1)的硼酸锍络合物的分离。
作为本发明中使用的构成热固化性树脂组合物的环氧化合物，可以适当使用一直以来用于电子材料的接合的热固化性环氧化合物。作为这样的热固化性环氧化合物，可以是溶液状也可以是固体状，优选环氧当量通常为100～4000左右、且分子中具有两个以上的环氧基的环氧化合物。例如可以优选使用双酚A型环氧化合物、酚醛型环氧化合物、甲酚醛型环氧化合物、酯型环氧化合物、脂环式环氧化合物等。另外，这些化合物中包括单体或低聚物。
除上述的环氧化合物以外，根据需要，还可以使用杂环系环氧化合物或加氢环氧化合物等。
作为杂环系环氧化合物，可以列举具有三嗪环的环氧化合物，可以特别优选列举：1,3,5-三(2,3-环氧丙基)-1,3,5-三嗪-2,4,6-(1H,3H,5H)-三酮。
作为加氢环氧化合物，可以使用上述的脂环式环氧化合物或杂环系环氧化合物的氢化物、或其他公知的加氢环氧树脂。
需要说明的是，脂环式环氧化合物或杂环系环氧化合物或加氢环氧化合物可以单独使用，也可以将两种以上结合使用。其中，从可以实现较高的可见光透过率的角度考虑，优选必须使用脂环式环氧化合物。作为这样的脂环式环氧化合物的具体例子，可以列举：缩水甘油基六氢双酚A、3,4-环氧环己烯基甲基-3’,4’-环氧环己烯羧酸酯等。其中，从可以确保固化物具有适于安装LED等的光透过性、并且速固化性也优异的角度考虑，可以优选使用缩水甘油基六氢双酚A、3,4-环氧环己烯基甲基-3’,4’-环氧环己烯羧酸酯。
另外，除以上说明的环氧化合物以外，只要不损及本发明的效果，还可以结合使用其他的环氧化合物。例如可以列举：使双酚A、双酚F、双酚S、四甲基双酚A、二芳基双酚A、氢醌、邻苯二酚、间苯二酚、甲酚、四溴双酚A、三羟基联苯、二苯甲酮、双间苯二酚、双酚六氟丙酮、四甲基双酚A、四甲基双酚F、三(羟基苯基)甲烷、联二甲苯酚(bixylenol)、苯酚酚醛、甲酚醛等多元酚与环氧氯丙烷反应得到的缩水甘油醚；使甘油、新戊二醇、乙二醇、丙二醇、丁二醇、己二醇、聚乙二醇、聚丙二醇等脂肪族多元醇与环氧氯丙烷反应得到的聚缩水甘油醚；使对羟基苯甲酸、β-羟基萘甲酸等羟基甲酸与环氧氯丙烷反应得到的缩水甘油醚酯；由邻苯二甲酸、邻苯二甲酸甲酯、间苯二甲酸、对苯二甲酸、四氢邻苯二甲酸、内次甲基四氢邻苯二甲酸、内次甲基六氢邻苯二甲酸、偏苯三酸、聚合脂肪酸等聚羧酸得到的聚缩水甘油酯；由氨基苯酚、氨基烷基苯酚得到的缩水甘油基氨基缩水甘油醚；由氨基苯甲酸得到的缩水甘油基氨基缩水甘油酯；由苯胺、甲苯胺、三溴苯胺、二甲苯二胺、二氨基环己烷、双氨基甲基环己烷、4,4’-二氨基二苯基甲烷、4,4’-二氨基二苯基砜等得到的缩水甘油胺；环氧化聚烯烃等公知的环氧树脂类。
本发明中使用的热固化性树脂组合物中的热催化型固化剂的混合量若太少，则固化不充分；若太多，则保存稳定性降低，因此相对于100质量份的环氧化合物，热催化型固化剂的混合量优选0.1～7质量份，更优选为0.5～3质量份。
在本发明中使用的热固化性树脂组合物中，除作为主固化成分的上述环氧化合物以外，在不损及发明效果的范围内，可以结合使用热固化性脲树脂、热固化性蜜胺树脂、热固化性酚醛树脂等热固化性树脂、或聚酯树脂或聚氨酯树脂等热塑性树脂。
在本发明中使用的热固化性树脂组合物中，根据需要，可以含有颜料、抗静电剂、防老化剂、硅烷偶联剂、溶剂等。
本发明中使用的热固化性树脂组合物可以通过将环氧化合物、热催化型固化剂等均匀混合来制备。另外，不必预先混合，只要将后述的导电颗粒和光反射性绝缘颗粒一同混合即可。
作为以上说明的热固化性树脂组合物，优选尽量使用无色透明的热固化性树脂组合物。这是为了使各向异性导电浆料中的光反射性绝缘颗粒的光反射效率不降低，而且在不改变入射光的光色的情况下反射该入射光。这里，无色透明是指各向异性导电浆料的固化物对于波长380～780nm的可见光光路长1cm的光透过率(JIS K7105)为80%以上、优选90%以上。
以上说明的分散在热固化性树脂组合物中的光反射性绝缘颗粒用于将入射到各向异性导电浆料中的光反射到外部。
需要说明的是，具有光反射性的颗粒包括：金属颗粒、将金属颗粒进行树脂包覆而得到的颗粒、在自然光下呈灰色～白色的金属氧化物、金属氮化物、金属硫化物等无机颗粒、用无机颗粒包覆树脂芯粒而得到的颗粒、与颗粒的材质无关而其表面具有凹凸的颗粒。但是，在上述颗粒中，由于要求显示出绝缘性的关系，本发明中可以使用的光反射性绝缘颗粒不包括金属颗粒。另外，在金属氧化物颗粒中，不可以使用象ITO那样具有导电性的金属氧化物颗粒。另外，即使是显示出光反射性和绝缘性的无机颗粒，但象SiO2那样其折射率较所用的热固化性树脂组合物的折射率低的无机颗粒也不可以使用。
作为这样的光反射性绝缘颗粒的优选的具体例子，可以列举选自氧化钛(TiO2)、氮化硼(BN)、氧化锌(ZnO)和氧化铝(Al2O3)的至少一种无机颗粒。其中，从高折射率的角度考虑，优选使用TiO2。其原因在于：这些无机颗粒本身基本上呈白色，因此对可见光的反射特性的波长依赖性小，因此可以提高发光效率，而且可以使发光元件的发光色以其原来的颜色进行反射。
作为光反射性绝缘颗粒的形状，可以是球状、鳞片状、无定形状、针状等，但若考虑到反射效率，则优选球状、鳞片状。另外，作为其大小，当为球状时，若太小则反射率降低，若太大则存在着阻碍经由各向异性导电颗粒进行的连接的倾向，因此优选0.02～20μm、更优选为0.2～1μm；当为鳞片状时，长径优选0.1～100μm、更优选1～50μm，短径优选0.01～10μm、更优选0.1～5μm，厚度优选0.01～10μm、更优选为0.1～5μm。
由无机颗粒构成的光反射性绝缘颗粒，优选其折射率(JIS K7142)较热固化性树脂组合物的固化物的折射率(JIS K7142)大，更优选至少大0.02左右。这是由于：若折射率差小，则它们的界面的反射效率降低。
作为光反射性绝缘颗粒，可以使用以上说明的无机颗粒，但也可以使用用透明的绝缘性树脂包覆鳞片状或球状金属颗粒的表面而得到的树脂包覆金属颗粒。作为金属颗粒，可以列举镍、银、铝等。作为颗粒的形状，可以列举无定形状、球状、鳞片状、针状等，其中，从光扩散效果的角度考虑，优选球状的形状；从全反射效果的角度考虑，优选鳞片状的形状。从光的反射率的角度考虑，特别优选的金属颗粒为鳞片状银颗粒。另外，在金属颗粒的表面，优选预先通过硅烷偶联剂导入γ-缩水甘油氧基或乙烯基等。由于这些树脂包覆金属颗粒本身基本为白色，因此对可见光的反射特性的波长依赖性小，因此可以提高发光效率，而且可以使发光元件的发光色以其原来的颜色进行反射。
作为光反射性绝缘颗粒的树脂包覆金属颗粒的大小还根据形状而不同，但通常而言，若太大，则有可能阻碍经由各向异性导电颗粒进行的连接；若太小，则不易反射光，因此优选当为球状时，粒径为0.1～30μm，更优选为0.2～10μm；当为鳞片状时，长径优选0.1～100μm、更优选1～50μm，厚度优选0.01～10μm、更优选为0.1～5μm。这里，关于光反射性绝缘颗粒的大小，当被绝缘包覆时，是指还包括其绝缘包覆在内的大小。
作为这样的树脂包覆金属颗粒中的该树脂，可以使用各种绝缘性树脂。从机械强度或透明性等方面考虑，可以优选使用丙烯酸系树脂的固化物。可以优选列举：在苯甲酰过氧化物等有机过氧化物等自由基引发剂的存在下，使甲基丙烯酸甲酯和甲基丙烯酸-2-羟乙酯进行自由基共聚而得到的树脂。此时，更优选通过2,4-甲苯二异氰酸酯等异氰酸酯系交联剂进行交联。
这样的树脂包覆金属颗粒例如可以如下制备：将金属颗粒和硅烷偶联剂投入甲苯等溶剂中，在室温下搅拌约1小时，之后投入自由基单体和自由基聚合引发剂、并根据需要投入交联剂，边加热至自由基聚合开始的温度边进行搅拌，从而可以制备树脂包覆金属颗粒。
以上说明的光反射性绝缘颗粒在光反射性各向异性导电浆料中的混合量若太少，则无法实现充分的光反射；若太多，则阻碍基于结合使用的导电颗粒的连接，因此相对于100质量份的热固化性树脂组合物，优选40～120质量份，更优选为50～100质量份。
作为构成本发明的光反射性各向异性导电浆料的导电颗粒，可以使用现有的各向异性导电连接用导电颗粒中使用的金属颗粒。例如可以列举：金、镍、铜、银、焊锡、钯、铝、它们的合金、它们的多层化物(例如镀镍/镀薄金物)等。其中，由于金、镍、铜使导电颗粒呈茶色，所以较其他金属材料更可以享受本发明的效果。
用作导电颗粒的金属颗粒的形状可以是球状、片状、针状、块状，也可以是表面形成有针状的镀金属(例如镍)的形状。
关于用作导电颗粒的金属颗粒的粒径，从发生短路或导通可靠性的角度考虑，当为球状时，优选0.2～10μm，更优选为1～7μm；当为片状时，厚度优选为0.2～0.4μm、长径优选为1～10μm。
作为导电颗粒，可以使用用金属材料包覆树脂颗粒而得到的金属包覆树脂颗粒。作为这样的树脂颗粒，可以列举：苯乙烯系树脂颗粒、苯并胍胺树脂颗粒、尼龙树脂颗粒等。用金属材料包覆树脂颗粒的方法也可以采用以往公知的方法，可以采用无电解电镀法、电解电镀法等。另外，包覆的金属材料的层厚为足以确保良好的连接可靠性的厚度，虽然也取决于树脂颗粒的粒径或金属的种类，但通常为0.1～3μm。
若树脂颗粒的粒径太小，则发生导通不良；若太大，则存在发生图案(pattern)间短路的倾向，因此优选为1～20μm，更优选为3～10μm，特别优选为3～5μm。此时，芯粒1的形状优选为球形，但也可以是片状、橄榄球状。
优选的金属包覆树脂颗粒为球状形状，若其粒径太大，则连接可靠性降低，因此优选1～20μm，更优选为3～10μm。
特别是在本发明中，优选赋予上述的导电颗粒光反射性，形成光反射性导电颗粒。图1A、图1B是这样的光反射性导电颗粒10、20的截面图。首先，从图1A的光反射性导电颗粒开始说明。
光反射性导电颗粒10由被金属材料包覆的芯粒1、和在该芯粒表面由选自氧化钛(TiO2)颗粒、氧化锌(ZnO)颗粒或氧化铝(Al2O3)颗粒的至少一种无机颗粒2形成的光反射层3构成。氧化钛颗粒、氧化锌颗粒或氧化铝颗粒是在太阳光下呈白色的无机颗粒。因此，由它们形成的光反射层3呈白色～灰色。呈白色～灰色是指对可见光的反射特性的波长依赖性小、并且容易反射可见光。因此，可以进一步提高发光效率，而且可以使发光元件的发光色以其原来的颜色反射。
需要说明的是，在氧化钛颗粒、氧化锌颗粒或氧化铝颗粒中，当担心已固化的各向异性导电浆料的热固化性树脂组合物的固化物的光劣化时，可以优选使用对光劣化不具催化性、且折射率也高的氧化锌。
由于芯粒1为供给各向异性导电连接的芯粒，所以其表面由金属材料构成。这里，作为表面被金属材料包覆的方案，如上所述，可以列举：芯粒1本身为金属材料的方案、或树脂颗粒的表面被金属材料包覆的方案。
关于由无机颗粒2形成的光反射层3的层厚，从其与芯粒1的粒径的相对大小的角度考虑，若相对于芯粒1的粒径太小，则反射率的下降显著；若相对于芯粒1的粒径太大，则发生导通不良，因此优选为0.5～50%，更优选为1～25%。
另外，在光反射性导电颗粒10中，若构成光反射层3的无机颗粒2的粒径太小，则难以产生光反射现象；若太大，则存在着难以形成光反射层的倾向，因此优选为0.02～4μm，更优选为0.1～1μm，特别优选为0.2～0.5μm。此时，从发生光反射的光的波长的角度考虑，无机颗粒2的粒径优选为应该反射的光(即发光元件发出的光)的波长的50%以上，以使该光不会透过。此时，作为无机颗粒2的形状，可以列举无定型、球状、鳞片状、针状等，其中，从光扩散效果的角度考虑，优选球状；从全反射效果的角度考虑，优选鳞片状的形状。
图1A的光反射性导电颗粒10，可以利用公知的成膜技术、即通过使大小粉末之间发生物理碰撞而在大粒径颗粒的表面形成由小粒径颗粒构成的膜的技术(所谓机械融合法)来制造。此时，无机颗粒2以侵入芯粒1的表面的金属材料中的方式被固定，另一方面，无机颗粒之间不易被熔合固定，所以无机颗粒的单层构成光反射层3。因此，在图1A的情况下，认为光反射层3的层厚与无机颗粒2的粒径同等或稍薄。
接下来，对图1B的光反射性导电颗粒20进行说明。在该光反射性导电颗粒20中，光反射层3含有发挥粘合剂作用的热塑性树脂4，通过该热塑性树脂4，无机颗粒2彼此之间也被固定，无机颗粒2形成多层(例如形成两层或三层)，在这方面与图1A的光反射性导电颗粒10不同。通过含有这样的热塑性树脂4，光反射层3的机械强度提高，无机颗粒不易发生剥落等。
作为热塑性树脂4，为了减轻环境负荷，可以优选使用不含卤素的热塑性树脂，例如可以优选使用聚乙烯、聚丙烯等聚烯烃或聚苯乙烯、丙烯酸树脂等。
这样的光反射性导电颗粒20，也可以利用机械融合法来制造。若机械融合法中使用的热塑性树脂4的粒径太小，则粘合功能降低；若太大，则难以附着在芯粒上，因此优选为0.02～4μm，更优选为0.1～1μm。另外，若上述热塑性树脂4的混合量太少，则粘合功能降低；若太多，则形成颗粒聚集体；因此相对于100质量份的无机颗粒2，上述热塑性树脂4的混合量优选为0.2～500质量份，更优选为4～25质量份。
在本发明的光反射性各向异性导电浆料中，相对于100质量份的热固化性树脂组合物，若光反射性导电颗粒等导电颗粒的混合量太少，则发生导通不良；若太多，则存在着发生图案间短路的倾向，因此优选为1～100质量份，更优选为10～50质量份。
关于本发明的光反射性各向异性导电浆料的反射特性，为了提高发光元件的发光效率，优选光反射性各向异性导电浆料的固化物对波长450nm的光的反射率(JIS K7105)至少为30%。为了达到这样的反射率，可以适当调整所使用的光反射性导电颗粒的反射特性或混合量、热固化性树脂组合物的混合组成等。通常，当增加反射特性良好的光反射性导电颗粒的混合量时，反射率也趋于增大。
另外，还可以从折射率的角度评价光反射性各向异性导电浆料的反射特性。即，这是由于，若光反射性各向异性导电浆料的固化物的折射率较除去导电颗粒和光反射性绝缘颗粒之后的热固化性树脂组合物的固化物的折射率大，则在光反射性绝缘颗粒与包围其的热固化性树脂组合物的固化物的界面光反射量增大。具体而言，优选从光反射性绝缘颗粒的折射率(JIS K7174)中减去热固化性树脂组合物的折射率(JIS K7174)而得到的差优选为0.02以上、更优选为0.2以上。需要说明的是，通常以环氧树脂为主体的热固化性树脂组合物的折射率为约1.5。
本发明的光反射性各向异性导电浆料可以通过将光反射性绝缘颗粒、导电颗粒和热固化性树脂组合物均匀混合来制造。
接下来，参照图2对本发明的发光装置进行说明。发光装置200是，在基板21上的连接端子22与分别形成于作为发光元件的LED23的n电极24和p电极25上的连接用凸块26之间涂布上述本发明的光反射性各向异性导电浆料、并倒装芯片安装有基板21和LED23的发光装置。这里，光反射性各向异性导电浆料的固化物100是光反射性导电颗粒10分散在热固化性树脂组合物的固化物11中形成的。需要说明的是，根据需要，可以用透明模压树脂密封整个LED23以覆盖该元件。另外，与以往一样，可以在LED23上设置光反射层。
在如此构成的发光装置200中，从LED23发出的光中，朝着基板21侧发出的光被光反射性各向异性导电浆料的固化物100中的光反射性导电颗粒10反射，从LED23的上面射出。因此，可以防止发光效率的降低。
本发明的发光装置200中的光反射性各向异性导电浆料以外的构成(LED23、凸块26、基板21、连接端子22等)可以和现有的发光装置的构成一样。另外，本发明的发光装置200，除了使用本发明的光反射性各向异性导电浆料以外，还可以利用现有的各向异性导电连接技术来制造。需要说明的是，作为发光元件，除LED以外，在不损及本发明效果的范围内，可以使用公知的发光元件，但为了在元件的单侧的同一平面上配置阳极和阴极这两个电极，从可以容易地进行安装的角度考虑，可以优选使用LED。
实施例
参考例1～4 (硼酸锍络合物的合成)
将式(2a)～(2d)的锑酸锍络合物(合成方法参照日本特开平10-245378号公报、日本特开2006-96742号公报)溶解于乙酸乙酯中，分别制备该络合物的10质量%乙酸乙酯溶液。除此之外，制备式(3)的硼酸钠盐(合成方法参照日本特开平10-310587号公报)的10质量%水溶液。
接下来，在室温下向该锑酸盐络合物的10质量%乙酸乙酯溶液中混合等摩尔量的式(3)的硼酸钠盐的10质量%水溶液，直接搅拌30分钟。之后，从反应混合液中分离乙酸乙酯层，干燥，减压除去乙酸乙酯。以蒸发残余物的形式得到式(1a)、(1b)、(1c)和式(1A)的硼酸锍络合物。
对式(1a)、(1b)和式(1A)的硼酸锍络合物进行质量分析(测定仪器：AQUITY UPLC系统、WATERS公司)、元素分析(测定仪器：PHOENIX、EDAX公司)、IR测定(测定仪器：7000eFT-IR、VARIAN公司)和1H-NMR分析(测定仪器：MERCURY PLUS、VARIAN公司)。关于这些硼酸锍络合物，由所得结果可以确认是目的化合物。
(i) 式(1a)的硼酸锍络合物[4-羟基苯基-甲基-1-萘基甲基锍四(五氟苯基)硼酸盐]的分析
结果
＜MS分析结果＞
M＋＝281(锍残基)
M＋＝679(硼酸盐残基)
＜元素分析结果＞
实测值 C；52．51 H；1.89
理论值 C；52．52 H；1.78
＜IR分析结果(cm-1)＞
＜1H-NMR分析结果(δ值)、参照图3 (使用THF)＞
(质子归属)
。
(ii) 式(1b)的硼酸锍络合物[4-羟基苯基-甲基-(2-甲基苄基)锍四(五氟苯基)硼酸盐]的分析结果
＜MS分析结果＞
M＋＝245(锍残基)
M＋＝679(硼酸盐残基)
＜元素分析结果＞
实测值 C；50.39 H；1.77
理论值 C；50.60 H；1.80
＜IR分析结果(cm-1)＞
＜1H-NMR分析结果(δ值)、参照图4 (使用THF)＞
(质子归属)
。
(iii) 实施例1的式(1A)的硼酸锍络合物[对甲氧基羰氧基苯基-苄基-甲基锍四(五氟苯基)硼酸盐]的分析结果
＜MS分析结果＞
M＋＝289(锍残基)；
M＋＝679(硼酸盐残基)。
＜元素分析结果＞
实测值与理论值一致。
＜IR分析结果(cm-1)＞
测定结果的IR图谱见图5。在图5的IR图谱中观察式(1A)的硼酸锍络合物的键的IR特性吸收。
＜1H-NMR分析结果(δ值)＞
测定结果的1H-NMR图谱见图6A，作为对照的溶剂的THF的1H-NMR图谱见图6B。在图6A的1H-NMR图谱中，可以确定以下的质子归属。
(质子归属)
。
实施例1～16和比较例1
通过使用搅拌机均匀混合表1所示的组成的成分，得到外观为白色的光反射性各向异性导电浆料。
需要说明的是，表1记载的成分的详细内容如下。
＜环氧化合物＞
脂环式环氧化合物(Celoxide 2021P、Daicel化学工业(株))
双酚A型环氧化合物(YX8000、三菱化学(株))；
＜防老化剂＞
脂环式环氧受阻酚系化合物(AO-60、ADEKA(株))；
＜粘度调节剂＞
氧化硅(球状平均粒径为10～20nm、R202、日本Aerosil(株))；
＜光反射性导电颗粒＞
金颗粒(球状平均粒径为5μm)；
＜光反射性绝缘颗粒＞
氧化锌(球状平均粒径为0.1～1μm、堺化学(株))；
＜酸酐系固化剂＞
甲基六氢邻苯二甲酸酐(MH-700、新日本理化(株))；
＜咪唑系固化促进剂＞
2-乙基-4-甲基咪唑(2E4MZ、四国化成(株))；
＜胺系热催化型固化剂＞
2,4,6-三(二甲基氨基甲基)苯酚(DMP-30、日进BM(株))；
＜芳族锍系热催化型固化剂＞
式(2b)、(2c)、(2d)、(1a)、(1b)、(1c)和(1A)的锑酸锍络合物或硼酸锍络合物。需要说明的是，式(2b)、(2c)、(2d)的锑酸锍络合物分别由三新化成(株)以商品名SI-60、SI-80、SI-100进行市售。
＜评价＞
对于得到的光反射性各向异性导电浆料，按照以下说明的方式，对“挥发量”、“粘合力”、“导通可靠性”、“光反射率”和“LED安装样品中的总光束量”进行试验评价。所得结果见表1。
(挥发量评价试验)
将5g实施例1～16或比较例1的光反射性各向异性导电浆料装入开口径为50mm的铝杯中，放在设定为各向异性导电连接温度即180℃的热板上加热30秒，然后在室温下放置冷却，之后测定重量，由该数值W(g)求出挥发量(%)[＝{(5-W)/5}×100]。除了将加热时间改为1分钟、5分钟以外，同样地求出挥发量。虽然挥发量为0是理想的，但在实用上优选挥发量不足0.5%。
(粘合力评价试验)
在镀Au的玻璃环氧电路基板上涂布光反射性各向异性导电浆料，使干燥厚度达到10μm，之后在其上暂时设置底面为边长6.3mm的正方形的LED芯片，使用倒装芯片粘合剂，在1N/芯片、180℃、30秒的条件下加压加热进行安装。关于该安装品的LED的剥离强度([N/芯片]晶片抗切强度测定(PTR-1100、RHESCA(公司)))，在刚刚安装后(初期)于室温下、安装后在150℃的环境中放置100小时后于室温下、或者刚刚安装后(初期)于150℃下、在模剪切速度为20μm/秒的条件下进行测定。优选粘合力为70N/芯片、至少为50N/芯片以上。
(导通可靠性评价试验)
在镀Au的玻璃环氧电路基板上涂布光反射性各向异性导电浆料，使干燥厚度达到10μm，之后在其上暂时设置底面为边长6.3mm的正方形的IC芯片，使用倒装芯片粘合剂，在1N/芯片、180℃、30秒的条件下加压加热进行安装。利用4端子法测定该安装品的初期导通电阻。接下来，对该安装品进行热冲击试验(TCT：-55℃、0.5小时←→125℃、0.5小时的500个循环)，试验后利用4端子法测定导通电阻。按照以下的标准进行评价。
评价标准
G(好)：导通电阻值不足1Ω的情形；
NG(不好)：导通电阻值为1Ω以上的情绪。
(光反射率评价试验)
将所得的光反射性各向异性导电浆料涂布在陶瓷制的白色板上，使干燥厚度达到100μm，在200℃下加热1分钟，使之固化。对于该固化物，使用分光光度计(U3300、日立制作所(株))，测定对波长450nm的光的反射率(JIS K7105)。其结果，在实施例1～16和比较例1的光反射性各向异性导电浆料中，由于使用的光反射性导电颗粒和使用的光反射性绝缘颗粒分别为相同种类、相同混合量，因此光反射率均为40～42%。实用上优选反射率为30%以上。
(LED安装样品中的总光束量评价试验)
在具有对间距为100μm的铜配线进行镀Ni/Au (5.0μm厚/0.3μm厚)处理而得到的配线的玻璃环氧基板上，使用凸块粘合剂(FB700、KAIJO(株))形成15μm高的金凸块。在该带有金凸块的环氧基板上，使用光反射性各向异性导电浆料，在200℃、60秒、1Kg/芯片的条件下倒装芯片安装蓝色LED(Vf＝3.2(If＝20mA))，得到试验用LED 模块(module)。
对于所得的试验用LED模块，使用总光束量测定系统(积分全球) (LE-2100、大塚电子株式会社)测定总光束量(测定条件 If＝20mA(恒电流控制))。其结果，在实施例1～16和比较例1的光反射性各向异性导电浆料中，由于使用的光反射性导电颗粒和使用的光反射性绝缘颗粒分别为相同种类、相同混合量，因此光反射率均为523～525mlm。实用上优选总光束量为300mlm以上。
[表1]
由表1可知：当为使用热催化型固化剂的实施例1～16的光反射性各向异性导电浆料时，各向异性导电连接时的挥发量为0，粘合力和导通可靠性也显示出优选的结果。而且，由于结合使用光反射性导电颗粒和光反射性绝缘颗粒，因此光反射率均为30%以上，450nm的光的蓝色以其原来的颜色反射。而且，总光束量也为300mlm以上。其中，当使用式(1A)的硼酸锍络合物时，粘合力的结果是特别优选的结果。
需要说明的是，由使用较低温活性的式(2b)的锑酸锍络合物和较高温活性的式(2d)的锑酸锍络合物的结果可知：使用低温活性的热催化型固化剂时，粘合力趋于变高。
相对于此，在使用酸酐系固化剂的比较例1的情况下，由于结合使用光反射性导电颗粒和光反射性绝缘颗粒，所以光反射率均为30%以上、总光束量也为300mlm以上，但在各向异性导电连接时酸酐系固化剂的挥发显著，其结果，特别是高温下的粘合力大幅下降，具体而言，150℃时的粘合力为初期粘合力的一半以下(88N/芯片→35N/芯片)。另外，TCT后的导通可靠性也为NG。
产业实用性
本发明的光反射性各向异性导电浆料，使用能够引发热阳离子聚合或热阴离子聚合的热催化型固化剂作为适合混合在含有环氧化合物作为主固化成分的热固化树脂组合物中的固化剂。因此，不是通过加聚反应、而是通过热催化型固化剂引发热阳离子聚合或热阴离子聚合，连锁地进行聚合反应，因此在进行用于各向异性导电连接的加热加压时，不会出现热催化型固化剂挥发而使固化性树脂组合物的组成发生大的变化的情况。因此，可以抑制高温环境下的粘合强度的降低或连接可靠性的降低。而且，使用各向异性导电浆料在配线板上倒装芯片安装发光二极管元件(LED)等发光元件来制造发光装置时，即使没有在发光元件上设置导致制造成本增加的光反射层，也不会使发光效率降低。因此，本发明的光反射性各向异性导电浆料在倒装芯片安装LED时有用。
符号说明
1：芯粒；
2：无机颗粒；
3：光反射层；
4：热塑性树脂；
10、20：光反射性导电颗粒；
11：热固化性树脂组合物的固化物；
21：基板；
22：连接端子；
23：LED；
24：n电极；
25：p电极；
26：凸块；
100：光反射性各向异性导电浆料的固化物；
200：发光装置。

Claims (11)

1.光反射性各向异性导电浆料，是用于在配线板上各向异性导电连接发光元件的光反射性各向异性导电浆料，其特征在于：是将光反射性导电颗粒和光反射性绝缘颗粒分散在热固化性树脂组合物中形成的，在100质量份的热固化性树脂组合物中光反射性绝缘颗粒的混合量为40～120质量份，相对于100质量份的热固化性树脂组合物，光反射性导电颗粒的混合量为1～100质量份，所述光反射性导电颗粒是由被金属材料包覆的芯粒、和在该芯粒表面由选自氧化钛颗粒、氧化锌颗粒或氧化铝颗粒的至少一种无机颗粒形成的光反射层构成的光反射性导电颗粒，所述光反射性绝缘颗粒为选自氮化硼、氧化锌和氧化铝的至少一种无机颗粒，该热固化性树脂组合物含有环氧化合物和热催化型固化剂。
2.权利要求1所述的光反射性各向异性导电浆料，其中，热催化型固化剂为胺系热阴离子聚合催化型固化剂或芳族锍系热阳离子聚合催化型固化剂。
3.权利要求2所述的光反射性各向异性导电浆料，其中，热阳离子聚合催化型固化剂为式(1)所表示的芳族锍系化合物：
式(1)中，R1为芳烷基，R2为低级烷基，R3为氢原子或低级烷氧基羰基；X为卤原子，n为1～3的整数。
4.权利要求3所述的光反射性各向异性导电浆料，其中芳族锍系化合物为下述式(1a)、(1b)、(1c)和(1A)中的任一式所述的硼酸锍络合物，
5.权利要求4所述的光反射性各向异性导电浆料，其中，芳族锍系化合物为式(1A)的硼酸锍络合物。
6.权利要求1～5中任一项所述的光反射性各向异性导电浆料，其中，环氧化合物为脂环式环氧化合物。
7.权利要求1～5中任一项所述的光反射性各向异性导电浆料，其中，相对于100质量份的环氧化合物，热固化性树脂组合物中的热催化型固化剂的混合量为0.5～3质量份。
8.权利要求1所述的光反射性各向异性导电浆料，其中，根据JIS K7142测定的光反射性绝缘颗粒的折射率较根据JIS K7142测定的热固化性树脂组合物的固化物的折射率大。
9.权利要求1～5中任一项所述的光反射性各向异性导电浆料，其中，光反射性绝缘颗粒为用绝缘性树脂包覆鳞片状或球状银颗粒的表面而得到的树脂包覆金属颗粒。
10.发光装置，该发光装置经由权利要求1～9中任一项所述的光反射性各向异性导电浆料以倒装芯片方式在配线板上安装有发光元件。
11.权利要求10所述的发光装置，其中，发光元件为发光二极管元件。
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