TW201543506A - 異向性導電膜及其製造方法 - Google Patents

異向性導電膜及其製造方法 Download PDF

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Publication number
TW201543506A
TW201543506A TW104103698A TW104103698A TW201543506A TW 201543506 A TW201543506 A TW 201543506A TW 104103698 A TW104103698 A TW 104103698A TW 104103698 A TW104103698 A TW 104103698A TW 201543506 A TW201543506 A TW 201543506A
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Taiwan
Prior art keywords
layer
conductive particles
resin layer
connecting layer
connection
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TW104103698A
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English (en)
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TWI664644B (zh
Inventor
Yasushi Akutsu
Reiji Tsukao
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Dexerials Corp
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Publication date
Priority claimed from JP2014019864A external-priority patent/JP6217422B2/ja
Priority claimed from JP2014019865A external-priority patent/JP6260312B2/ja
Application filed by Dexerials Corp filed Critical Dexerials Corp
Publication of TW201543506A publication Critical patent/TW201543506A/zh
Application granted granted Critical
Publication of TWI664644B publication Critical patent/TWI664644B/zh

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    • H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
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    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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    • C—CHEMISTRY; METALLURGY
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    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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Abstract

本發明之異向性導電膜具有第1連接層及形成於第1連接層單面之第2連接層。第1連接層為光聚合樹脂層，第2連接層為熱或光陽離子、陰離子或者自由基聚合性樹脂層。於第1連接層之第2連接層側表面，異向性導電連接用之導電粒子係以單層排列。關於第1連接層之硬化率，具有硬化率較該單面之硬化率低的區域，其斜向地存在於第1連接層之厚度方向。或者，與第1連接層之該單面之硬化率相比，第1連接層之導電粒子附近區域中相對接近第1連接層之另一面之區域之硬化率較低。

Description

異向性導電膜及其製造方法
本發明係關於一種異向性導電膜及其製造方法。
異向性導電膜被廣泛用於IC(integrated circuit，積體電路)晶片等電子零件之構裝，近年來，就應用在高密度構裝之觀點而言，且為了導通可靠性或絕緣性之提高、構裝導電粒子捕捉率之提高、製造成本之降低等目的，提出有使異向性導電連接用之導電粒子以單層排列於絕緣性接著層而成的2層構造之異向性導電膜(專利文獻1)。
該2層構造之異向性導電膜係藉由如下方式製造：使導電粒子以單層且緊密填充之方式排列於轉印層後，對轉印層進行雙軸延伸處理，藉此形成導電粒子以特定間隔均等地排列之轉印層，此後，將該轉印層上之導電粒子轉印至含有熱硬化性樹脂及聚合起始劑之絕緣性樹脂層，進而於轉印後之導電粒子上層壓含有熱硬化性樹脂但不含聚合起始劑之另外絕緣性樹脂層(專利文獻1)。
專利文獻1：日本專利第4789738號說明書
然而，專利文獻1之2層構造之異向性導電膜由於使用有不含聚合起始劑之絕緣性樹脂層，故而儘管使導電粒子以單層且以特定間隔均等地排列，亦因異向性導電連接時之加熱而於不含聚合起始劑之絕緣性樹脂層易產生相對較大之樹脂流，導電粒子亦容易順著該樹脂流而流動，因此，產生構裝導電粒子捕捉率之降低、短路之發生、絕緣性之降低等問題。
本發明之目的在於解決以上習知之技術問題，於具有以單層排列之導電粒子的多層構造之異向性導電膜中，實現良好之導通可靠性、良好之絕緣性、及良好之構裝導電粒子捕捉率。
本發明人等發現，於使導電粒子以單層排列於光聚合性樹脂層後，藉由傾斜地照射紫外線或藉由自至少2個方向傾斜地照射紫外線，而使導電粒子固定化或者暫時固定化，進而，藉由在經固定或者暫時固定之導電粒子上積層熱或光陽離子、陰離子或者自由基聚合性樹脂層而獲得異向性導電膜，該異向性導電膜為可達成上述本發明之目的之構成，以至完成本發明。
即，本發明之第1態樣提供一種異向性導電膜，其具有第1連接層及形成於第1連接層單面之第2連接層，其特徵在於：第1連接層為光聚合樹脂層，第2連接層為熱或光陽離子、陰離子或者自由基聚合性樹脂層，於第1連接層之該單面，將異向性導電連接用之導電粒子以單層排列，關於第1連接層之硬化率，具有硬化率較該單面之硬化率低的區域，其斜向地存在於第1連接層之厚度方向。
又，本發明之第2態樣提供一種異向性導電膜，其具有第1連接層及形成於第1連接層單面之第2連接層，其特徵在於：第1連接層為光聚合樹脂層，第2連接層為熱或光陽離子、陰離子或者自由基聚合性樹脂層，於第1連接層之該單面，將異向性導電連接用之導電粒子以單層排列，與第1連接層之該單面之硬化率相比，第1連接層之導電粒子附近區域中相對接近第1連接層之另一面之區域之硬化率較低。
再者，於本發明中，第2連接層較佳為使用有藉由加熱而使聚合反應開始之熱聚合起始劑的熱聚合性樹脂層，但亦可為使用有藉由光而使聚合反應開始之光聚合起始劑的光聚合性樹脂層。亦可為併用有熱聚合起始劑與光聚合起始劑之熱-光聚合性樹脂層。此處，第2連接層於製造上有時被限定於使用熱聚合起始劑之熱聚合性樹脂層。
本發明之異向性導電膜亦可為了防止應力緩和等之接合體之翹曲，而於第1連接層之另一面具有與第2連接層大致相同構成之第3連接層。即，亦可於第1連接層之另一面具有由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層。
再者，第3連接層較佳為使用有藉由加熱而使聚合反應開始之熱聚合起始劑的熱聚合性樹脂層，但亦可為使用有藉由光而使聚合反應開始之光聚合起始劑的光聚合性樹脂層。亦可為併用有熱聚合起始劑及光聚合起始劑之熱-光聚合性樹脂層。此處，第3連接層於製造上有時被限定於使用熱聚合起始劑之熱聚合性樹脂層。
又，本發明提供一種製造方法，其係上述本發明之第1態樣 之異向性導電膜之製造方法，具有以一階段之光聚合反應形成第1連接層之以下之步驟(A)~(C)，或具有以二階段之光聚合反應形成第1連接層之後述之步驟(AA)~(DD)。
(以一階段之光聚合反應形成第1連接層之情形)
步驟(A)
使導電粒子以單層排列於光聚合性樹脂層之步驟；
步驟(B)
藉由對排列有導電粒子之光聚合性樹脂層傾斜地照射紫外線而使之進行光自由基聚合反應，而形成表面固定有導電粒子之第1連接層的步驟；及
步驟(C)
於第1連接層之導電粒子側表面形成由熱或光陽離子或者陰離子聚合性樹脂層、或熱或光自由基聚合性樹脂層所構成之第2連接層的步驟。
(以二階段之光聚合反應形成第1連接層之情形)
步驟(AA)
使導電粒子以單層排列於光聚合性樹脂層之步驟；
步驟(BB)
藉由對排列有導電粒子之光聚合性樹脂層傾斜地照射紫外線而使之進行光自由基聚合反應，而形成表面暫時固定有導電粒子之暫時第1連接層的步驟；
步驟(CC)
於暫時第1連接層之導電粒子側表面形成由熱陽離子、陰離子或者自 由基聚合性樹脂層所構成之第2連接層的步驟；及
步驟(DD)
藉由自與第2連接層相反之側對暫時第1連接層照射紫外線而使之進行光聚合反應，而使暫時第1連接層正式硬化而形成第1連接層的步驟。
又，本發明提供一種製造方法，其係上述本發明之第2態樣之異向性導電膜之製造方法，具有以一階段之光聚合反應形成第1連接層之以下之步驟(A')~(C')，或具有以二階段之光聚合反應形成第1連接層之後述之步驟(AA')~(DD')。
(以一階段之光聚合反應形成第1連接層之情形)
步驟(A')
使導電粒子以單層排列於光聚合性樹脂層之步驟；
工穆(B')
藉由對排列有導電粒子之光聚合性樹脂層自至少2個方向傾斜地照射紫外線而使之進行光聚合反應，而形成表面固定有導電粒子之第1連接層的步驟；及
步驟(C')
於第1連接層之導電粒子側表面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第2連接層的步驟。
(以二階段之光聚合反應形成第1連接層之情形)
步驟(AA')
使導電粒子以單層排列於光聚合性樹脂層之步驟；
步驟(BB')
藉由對排列有導電粒子之光聚合性樹脂層自至少2個方向傾斜地照射紫外線而使之進行光聚合反應，而形成表面暫時固定有導電粒子之暫時第1連接層的步驟；及
步驟(CC')
於暫時第1連接層之導電粒子側表面形成由熱陽離子、陰離子或者自由基聚合性樹脂層所構成之第2連接層的步驟；及
步驟(DD')
藉由自與第2連接層相反之側對暫時第1連接層照射紫外線而使之進行光聚合反應，而使暫時第1連接層正式硬化而形成第1連接層的步驟。
將步驟(CC)及(CC')中第2連接層形成時所使用之起始劑限定於熱聚合起始劑，其原因在於：為了不對作為異向性導電膜之產品壽命、連接及連接構造體之穩定性產生不良影響。即，於對第1連接層分二階段照射紫外線之情形時，有時由於其步驟上之制約而第2連接層不得不限定於熱聚合硬化性者。再者，於連續進行二階段照射之情形時，可以與一階段大致相同之步驟形成，因此，可期待同等之作用效果。
又，本發明提供一種製造方法，其係於第1連接層之另一面具有與第2連接層相同構成之第3連接層的異向性導電膜之製造方法，除了以上之步驟(A)~(C)之外於步驟(C)之後(或者除了步驟(A')~(C')之外於步驟(C')之後)具有以下之步驟(Z)；或者，除了以上之步驟(AA)~(DD)之外於步驟(DD)之後(或者除了步驟(AA')~(DD')之外於步驟(DD')之後)具有以下之步驟(Z)。
步驟(Z)
於第1連接層之導電粒子側之相反面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟。
進而，本發明提供一種製造方法，其係於第1連接層之另一面具有與第2連接層大致相同構成之第3連接層的異向性導電膜之製造方法，除了以上之步驟(A)~(C)以外於步驟(A)之前(或者除了步驟(A‘)~(C')以外於步驟(A')之前)具有以下之步驟(a)；或者，除了以上之步驟(AA)~(DD)以外於步驟(AA)之前(或者除了步驟(AA')~(DD')以外於步驟(AA')之前)具有以下之步驟(a)。
步驟(a)
於光聚合性樹脂層之單面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟。
再者，於具有該步驟(a)之製造方法之步驟(A)或步驟(A')或者步驟(AA)或步驟(AA')中，於光聚合性樹脂層之另一面使導電粒子以單層排列即可。
於利用上述步驟設置第3連接層之情形時，出於上述理由而聚合起始劑較佳為限定於利用熱反應者。然而，若藉由設置第1連接層後不對產品壽命或連接產生不良影響之方法，來設置含有光聚合起始劑之第2及第3連接層，則製造「含有光聚合起始劑且依據本發明之主旨」的異向性導電膜並無特別限制。
再者，第2連接層或第3連接層之任一者作為黏著層而發揮功能的態樣亦包含於本發明。
另外，本發明提供一種利用上述異向性導電膜將第1電子零 件異向性導電連接於第2電子零件而成之連接構造體。
本發明之第1態樣及第2態樣之異向性導電膜具有由光聚合樹脂層所構成之第1連接層、及形成於第1連接層單面且由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第2連接層，進而，於第1連接層之第2連接層側表面以單層排列有異向性導電連接用之導電粒子。因此，可將導電粒子牢牢地固定於第1連接層。而且，於本發明之第1態樣之異向性導電膜之情形時，關於第1連接層之硬化率，由於斜向地進行光照射，故而具有硬化率較第2連接層側表面之硬化率低的區域會斜向地存在於第1連接層之厚度方向。結果，於異向性導電連接時，可使較低硬化率之區域及導電粒子之流動方向於斜向方向上一致，因此，可無損初期導通特性或導通可靠性而大為抑制短路之發生。又，於本發明之第2態樣之異向性導電膜之情形時，自至少2個方向傾斜地進行紫外線之照射，因此，第1連接層中之導電粒子之下方(背側)之區域因導電粒子之存在而未充分照射紫外線，因此，硬化率相對降低。換言之，第1連接層之導電粒子附近區域中相對接近第1連接層之另一面之區域之硬化率低於第1連接層之單面(第2連接層側表面)之硬化率。結果，第1連接層中導電粒子之下方(背側)之區域顯示良好之壓入性，結果，可實現良好之導通可靠性、絕緣性、構裝導電粒子捕捉率。再者，所謂第1連接層之導電粒子附近區域，係指圍繞導電粒子之導電粒子直徑0.2~5倍寬度之區域。該第1連接層樹脂層之硬化率相對較低之區域較理想為僅存在於第1連接層內。此係為了防止於連接時之壓入初期時導電粒子向連接方向以外偏離。
再者，於異向性導電連接利用熱時，成為與通常之異向性導 電膜之連接方法相同之方法。於為利用光時，使利用連接工具之壓入進行直至反應結束即可。即便於該情形時，連接工具等為了促進樹脂流動或粒子之壓入而受到加熱之情形亦較多。又，於併用熱與光之情形時，亦與上述同樣地進行即可。
1、100‧‧‧異向性導電膜
2‧‧‧第1連接層
2a‧‧‧第1連接層之第2連接層側之表面
2b‧‧‧第1連接層之最外表面
2X、2Y‧‧‧(暫時)第1連接層之區域
3‧‧‧第2連接層
4‧‧‧導電粒子
5‧‧‧第3連接層
30、40‧‧‧剝離膜
20‧‧‧暫時第1連接層
31‧‧‧光聚合性樹脂層
50‧‧‧暫時異向性導電膜
圖1係本發明之第1態樣之異向性導電膜之剖面圖。
圖2係本發明之第1態樣之異向性導電膜之製造步驟(A)之說明圖。
圖3A係本發明之第1態樣之異向性導電膜之製造步驟(B)之說明圖。
圖3B係本發明之第1態樣之異向性導電膜之製造步驟(B)之說明圖。
圖4A係本發明之第1態樣之異向性導電膜之製造步驟(C)之說明圖。
圖4B係本發明之第1態樣之異向性導電膜之製造步驟(C)之說明圖。
圖5係本發明之第1態樣所包括之異向性導電膜之剖面圖。
圖6係本發明之異向性導電膜之製造步驟(AA)之說明圖。
圖7A係本發明之第1態樣之異向性導電膜之製造步驟(BB)之說明圖。
圖7B係本發明之第1態樣之異向性導電膜之製造步驟(BB)之說明圖。
圖8A係本發明之第1態樣之異向性導電膜之製造步驟(CC)之說明圖。
圖8B係本發明之第1態樣之異向性導電膜之製造步驟(CC)之說明圖。
圖9A係本發明之第1態樣之異向性導電膜之製造步驟(DD)之說明圖。
圖9B係本發明之第1態樣之異向性導電膜之製造步驟(DD)之說明圖。
圖10係本發明之第2態樣之異向性導電膜之剖面圖。
圖11係本發明之第2態樣之異向性導電膜之製造步驟(A')之說明圖。
圖12A係本發明之第2態樣之異向性導電膜之製造步驟(B')之說明圖。
圖12B係本發明之第2態樣之異向性導電膜之製造步驟(B')之說明圖。
圖13A係本發明之第2態樣之異向性導電膜之製造步驟(C')之說明圖。
圖13B係本發明之第2態樣之異向性導電膜之製造步驟(C')之說明圖。
圖14係本發明之第2態樣之異向性導電膜之剖面圖。
圖15係本發明之第2態樣之異向性導電膜之製造步驟(AA')之說明圖。
圖16A係本發明之第2態樣之異向性導電膜之製造步驟(BB')之說明圖。
圖16B係本發明之第2態樣之異向性導電膜之製造步驟(BB')之說明圖。
圖17A係本發明之第2態樣之異向性導電膜之製造步驟(CC')之說明圖。
圖17B係本發明之第2態樣之異向性導電膜之製造步驟(CC')之說明圖。
圖18A係本發明之第2態樣之異向性導電膜之製造步驟(DD')之說明圖。
圖18B係本發明之第2態樣之異向性導電膜之製造步驟(DD')之說明圖。
《本發明之異向性導電膜》
以下，對本發明之第1態樣及第2態樣之異向性導電膜(以下，有時僅稱為本發明之異向性導電膜)之較佳一例進行詳細說明。
圖1所示之本發明之第1態樣之異向性導電膜1以及圖10所示之本發明之第2態樣之異向性導電膜1具有如下構造：於由使光聚合性樹脂層進行光聚合而成的光聚合樹脂層所構成之第1連接層2之單面，具有由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第2連接層3。而且，於第1連接層2之第2連接層3側之表面2a，為了進行異向性導電連接而使導電粒子4以單層排列、較佳為均等地排列。此處，所謂均等，係指導電粒子沿平面方向排列之狀態。關於其規則性，可以一定間隔設置。
<第1連接層2>
構成本發明之異向性導電膜1之第1連接層2由於係使光陽離子、陰離子或自由基聚合性樹脂層等光聚合性樹脂層進行光聚合而成之光聚合樹脂層，故而可使導電粒子固定。又，由於進行聚合，故而即便於異向性導電連接時被加熱，樹脂亦難以流動，故而可大為抑制短路之發生，因此可提高導通可靠性及絕緣性，且亦可提高構裝粒子捕捉效率。尤佳之第1連接層2係使含有丙烯酸酯化合物及光自由基聚合起始劑之光自由基聚合性樹脂層進行光自由基聚合而成之光自由基聚合樹脂層。以下，對第1連接層2為光自由基聚合樹脂層之情形進行說明。
(丙烯酸酯化合物)
作為形成丙烯酸酯單位之丙烯酸酯化合物，可使用以往公知之光自由基聚合性丙烯酸酯。例如，可使用：單官能(甲基)丙烯酸酯(此處，(甲基)丙烯酸酯包括丙烯酸酯與甲基丙烯酸酯)、二官能以上之多官能(甲基)丙烯酸酯。於本發明中，為了使接著劑成為熱硬化性，較佳為丙烯酸系單體之至少一部分使用多官能(甲基)丙烯酸酯。
關於第1連接層2中丙烯酸酯化合物之含量，若過少，則有難以賦予與第2連接層3之黏度差之傾向，若過多，則有硬化收縮較大而作業性降低之傾向，因此，較佳為2~70質量%，更佳為10~50質量%。
(光自由基聚合起始劑)
作為光自由基聚合起始劑，可自公知之光自由基聚合起始劑中適當選擇而使用。例如，可列舉苯乙酮系光聚合起始劑、苯偶醯縮酮系光聚合起始劑、磷系光聚合起始劑等。
關於光自由基聚合起始劑之使用量，相對於丙烯酸酯化合物100質量份，若過少則光自由基聚合不充分進行，若過多則成為剛性降低之原因，因此較佳為0.1~25質量份，更佳為0.5~15質量份。
(導電粒子)
作為導電粒子，可自以往公知之異向性導電膜中所使用者中適當選擇而使用。例如，可列舉：鎳、鈷、銀、銅、金、鈀等金屬粒子、金屬被覆樹脂粒子等。亦可併用2種以上。
作為導電粒子之平均粒徑，若過小則無法吸收配線之高度不均而有電阻變高之傾向，若過大亦有成為短路之原因之傾向，因此，較佳為1~10μm，更佳為2~6μm。
關於上述導電粒子於第1連接層2中之粒子量，若過少，則構裝導電粒子捕捉數降低而異向性導電連接變難，若過多，則有短路之虞，因此，較佳為每1平方毫米為50~50000個，更佳為200~30000個。
第1連接層2中，視需要可併用苯氧基樹脂、環氧樹脂、不飽和聚酯樹脂、飽和聚酯樹脂、胺酯樹脂(urethane resin)、丁二烯樹脂、聚醯亞胺樹脂、聚醯胺樹脂、聚烯烴樹脂等膜形成樹脂。第2連接層及第3連接層中可同樣地併用。
關於第1連接層2之層厚，若過薄，則有構裝導電粒子捕捉率降低之傾向，若過厚，則有導通電阻變高之傾向，因此，較佳為1.0~6.0μm，更佳為2.0~5.0μm。
亦可使第1連接層2中進而含有環氧化合物，及熱或光陽離子或者陰離子聚合起始劑。於該情形時，如後述般，較佳為第2連接層3亦設為含有環氧化合物與熱或光陽離子或者陰離子聚合起始劑之熱或光陽離子或者陰離子聚合性樹脂層。藉此，可提高層間剝離強度。關於環氧化合物及熱或光陽離子或者陰離子聚合起始劑，於第2連接層3處進行說明。
於第1連接層2中，如圖1(或者圖10)所示般，較佳為導電粒子4沒入第2連接層3(換言之，導電粒子4露出於第1連接層2之表面)。其原因在於：若導電粒子完全埋沒於第1連接層2中，則有電阻導通變高之虞。關於沒入之程度，若過小則有構裝導電粒子捕捉率降低之傾向，若過大則有導通電阻變高之傾向，因此，較佳為導電粒子之平均粒徑之10~90%、更佳為20~80%。
又，於圖1所示之本發明之第1態樣之異向性導電膜之第1 連接層2中，由於斜向地進行光照射，故而具有硬化率較第2連接層側之第1連接層之表面之硬化率低的區域，其斜向地存在於第1連接層之厚度方向。藉此，於異向性導電連接之熱壓接時，第1連接層之區域2X易被排除，而導通可靠性提高。此處，硬化率被定義為乙烯基之減少比率之數值，第1連接層之區域2X之硬化率較佳為40~80%，第1連接層之區域2Y之硬化率較佳為70~100%。
又，於圖10所示之本發明之第2態樣之異向性導電膜之第1連接層2中，較佳為第1連接層2之導電粒子附近區域中相對接近第1連接層2之另一面(最外表面2b)的區域(第1連接層之區域2X)之硬化率低於第1連接層2之單面(第2連接層側表面)(第1連接層之區域2Y)之硬化率。藉此，於異向性導電連接之熱壓接時，第1連接層之區域2X易被排除，而導通可靠性提高。此處，硬化率被定義為乙烯基之減少比率之數值，第1連接層之區域2X之硬化率較佳為40~80%，第1連接層之區域2Y之硬化率較佳為70~100%。
再者，第1連接層2形成時之光自由基聚合可以一階段(即，一次光照射)進行，亦可以二階段(即，二次光照射)進行。於該情形時，第二階段之光照射較佳為於在第1連接層2之單面形成有第2連接層3後於含氧環境(大氣中)下自第1連接層2之另一面側進行。藉此，可期待自由基聚合反應受氧阻礙而未硬化成分之表面濃度提高而可提高黏著性之效果。又，因以二階段進行硬化，故而聚合反應亦複雜化，因此，亦可期待可精確控制樹脂或粒子之流動性。
上述二階段之光自由基聚合中，第1連接層之區域2X於第 一階段中之硬化率較佳為10~50%，於第二階段中之硬化率較佳為40~80%，第1連接層之區域2Y於第一階段中之硬化率較佳為30~90%，於第二階段中之硬化率較佳為70~100%。
又，當第1連接層2形成時之光自由基聚合反應以二階段進行時，作為自由基聚合起始劑可僅使用1種，但使用使自由基反應開始之波長頻帶不同之2種光自由基聚合起始劑時黏著性提高，因此較佳。例如，較佳為將利用來自LED光源之波長365nm之光使自由基反應開始之光自由基聚合起始劑(例如，IRGACURE 369、BASF JAPAN(股))與利用來自高壓水銀燈光源之光使自由基反應開始之光自由基聚合起始劑(例如，IRGACURE 2959、BASF JAPAN(股))併用。藉由如上述般使用2種不同之光自由基聚合起始劑而樹脂之結合複雜化，因此，可更精密地控制連接時之樹脂之熱流動之舉動。其原因在於：於異向性導電連接之壓入時，粒子易受到施加於厚度方向之力，而在面方向之流動受到抑制，因此更易表現本發明之效果。
又，第1連接層2利用流變計測定時之最低熔融黏度高於第2連接層3之最低熔融黏度，具體而言，[第1連接層2之最低熔融黏度(mPa‧s)]/[第2連接層3之最低熔融黏度(mPa‧s)]之數值較佳為1~1000，更佳為4~400。再者，關於各者之較佳最低熔融黏度，前者為100~100000mPa‧S，更佳為500~50000mPa‧s。後者較佳為0.1~10000mPa‧s，更佳為0.5~1000mPa‧s。
第1連接層2之形成可藉由如下方式形成：藉由膜轉印法、模具轉印法、噴墨法、靜電附著法等方法使導電粒子附著於含有光自由基 聚合性丙烯酸酯及光自由基聚合起始劑之光自由基聚合性樹脂層，並自導電粒子側、其相反側、或者兩側照射紫外線。尤其是，僅自導電粒子側照射紫外線時，就可將第1連接層之區域2X之硬化率抑制得相對較低方面而言，較佳。
<第2連接層3>
第2連接層3係由熱或光陽離子、陰離子或者自由基聚合性樹脂層構成，較佳為由含有環氧化合物及熱或光陽離子或者陰離子聚合起始劑之熱或光陽離子或者陰離子聚合性樹脂層、或含有丙烯酸酯化合物及熱或光自由基聚合起始劑之熱或光自由基聚合性樹脂層構成。此處，由熱聚合性樹脂層形成第2連接層3時，並不因形成第1連接層2時之紫外線照射而發生第2連接層3之聚合反應，因此，就生產之簡便性及品質穩定性方面而言，較理想。
於第2連接層3為熱或光陽離子或者陰離子聚合性樹脂層之情形時，進而可含有丙烯酸酯化合物及熱或光自由基聚合起始劑。藉此，可提高與第1連接層2之層間剝離強度。
(環氧化合物)
於第2連接層3為含有環氧化合物及熱或光陽離子或者陰離子聚合起始劑之熱或光陽離子或者陰離子聚合性樹脂層時，作為環氧化合物，較佳可列舉分子內具有2個以上環氧基之化合物或者樹脂。該等可為液狀，亦可為固體狀。
(熱陽離子聚合起始劑)
作為熱陽離子聚合起始劑，可採用公知者作為環氧化合物之熱陽離子 聚合起始劑，例如，藉由熱而產生可使陽離子聚合性化合物發生陽離子聚合之酸者，可使用公知之錪鹽、鋶鹽、鏻鹽、二茂鐵類等，可較佳地使用對溫度顯示良好潛伏性之芳香族鋶鹽。
關於熱陽離子聚合起始劑之調配量，過少則有硬化不良之傾向，過多則有產品壽命降低之傾向，因此，相對於環氧化合物100質量份較佳為2~60質量份、更佳為5~40質量份。
(熱陰離子聚合起始劑)
作為熱陰離子聚合起始劑，可採用公知者作為環氧化合物之熱陰離子聚合起始劑，例如，藉由熱而產生可使陰離子聚合性化合物發生陰離子聚合之鹼者，可使用公知之脂肪族胺系化合物、芳香族胺系化合物、二級或三級胺系化含物、咪唑系化合物、聚硫醇系化合物、三氟化硼-胺錯合物、雙氰胺、有機醯肼等，可較佳地使用對溫度顯示良好潛伏性之膠囊化咪唑系化合物。
關於熱陰離子聚合起始劑之調配量，過少則有硬化不良之傾向，過多則有產品壽命降低之傾向，因此，相對於環氧化合物100質量份較佳為2~60質量份、更佳為5~40質量份。
(光陽離子聚合起始劑及光陰離子聚合起始劑)
作為環氧化合物用之光陽離子聚合起始劑或光陰離子聚合起始劑，可適當使用公知者。
(丙烯酸酯化合物)
於第2連接層3為含有丙烯酸酯化合物及熱或光自由基聚合起始劑之熱或光自由基聚合性樹脂層之情形時，作為丙烯酸酯化合物，可自關於第1 連接層2所說明者中適當選擇而使用。
(熱自由基聚合起始劑)
又，作為熱自由基聚合起始劑，例如，可列舉有機過氧化物或偶氮系化合物等，但可較佳地使用不產生成為氣泡之原因之氮的有機過氧化物。
關於熱自由基聚合起始劑之使用量，若過少則硬化不良，若過多則產品壽命降低，因此，相對於丙烯酸酯化合物100質量份較佳為2~60質量份、更佳為5~40質量份。
(光自由基聚合起始劑)
作為丙烯酸酯化合物用之光自由基聚合起始劑，可使用公知之光自由基聚合起始劑。
關於光自由基聚合起始劑之使用量，若過少則硬化不良，若過多則產品壽命降低，因此，相對於丙烯酸酯化合物100質量份較佳為2~60質量份、更佳為5~40質量份。
(第3連接層5)
以上，已說明圖1及圖10之2層構造之異向性導電膜，但亦可如圖5及圖14所示般於第1連接層2之另一面形成有第3連接層5。藉此，獲得可更精確地控制層整體之流動性之效果。此處，作為第3連接層5，可設為與前述之第2連接層3相同之構成。即，第3連接層5與第2連接層3同樣地為由熱或光陽離子、陰離子或者自由基聚合性樹脂層構成者。關於上述第3連接層5，可於在第1連接層之單面形成第2連接層後形成於第1連接層之另一面，亦可於第2連接層形成前，於第1連接層或者其前驅物即光聚合性樹脂層之另一面(未形成第2連接層之面)預先形成第3連接層。
《本發明之第1態樣之異向性導電膜之製造方法》
本發明之第1態樣之異向性導電膜之製造方法中，可列舉進行一階段光聚合反應之製造方法、及進行二階段光聚合反應之製造方法。
<進行一階段光聚合反應之製造方法>
對以一階段進行光聚合而製造圖1(圖4B)之異向性導電膜之一例進行說明。該製造例具有以下之步驟(A)~(C)。
(步驟(A))
如圖2所示般，使導電粒子4以單層排列於視需要形成於剝離膜30上之光聚合性樹脂層31。作為導電粒子4之排列方法，並無特別限制，可採用日本專利第4789738號之實施例1中對未延伸聚丙烯膜利用雙軸延伸操作之方法，或日本特開2010-33793號公報之使用模具之方法等。再者，作為排列之程度，考慮到連接對象之尺寸、導通可靠性、絕緣性、構裝導電粒子捕捉率等，較佳為二維地相互隔開1~100μm左右地排列。
(步驟(B))
繼而，如圖3A所示般，使用LED光源等自導電粒子側對排列有導電粒子4之光聚合性樹脂層31傾斜地照射紫外線(UV)，藉此使之進行光聚合反應，而形成表面固定有導電粒子4之第1連接層2。藉此，如圖3B所示般，可使位於導電粒子4與第1連接層2之最外表面之間的斜向之第1連接層之區域2X之硬化率低於位於相互鄰接之導電粒子4間之第1連接層之區域2Y之硬化率。照射時，視需要可將紫外線脈波狀地進行照射，亦可設置擋板而進行照射。藉由如上所述般，而粒子之背側之硬化性確實降低而使接合時之壓入變得容易，且可使導電粒子之流動方向於斜向方向一 致，可防止多個導電粒子過度連接，而可抑制短路之發生。
所謂傾斜地照射紫外線，係指相對於光聚合性樹脂層31帶有傾斜角θ而照射紫外線。該傾斜角θ為0°<θ<90°，較佳為30°≦θ≦60°。於該情形時，較佳為在與異向性導電膜之長邊方向正交之方向呈傾斜。若以上述方式進行，則可使導電粒子之流動方向與凸塊之長邊方向(即，異向性導電膜之寬度方向)一致。於該情形時，較佳為，遮住異向性導電膜之長邊方向之光聚合性樹脂層之左半部分，並對右半部分以朝異向性導電膜之右邊產生流動之方式傾斜地照射紫外線，繼而，遮住右半部分，並對左半部分以朝異向性導電膜之左邊產生流動之方式傾斜地照射紫外線。
(步驟(C))
繼而，如圖4A所示般，於第1連接層2之導電粒子4側表面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第2連接層3。作為具體之一例，將藉由常用方法而形成於剝離膜40之第2連接層3載置於第1連接層2之導電粒子4側表面，並以不發生過大之熱聚合之程度進行熱壓接。然後，可藉由去除剝離膜30及40而獲得圖4B之異向性導電膜。
再者，圖5之異向性導電膜100可藉由在步驟(C)之後實施以下之步驟(Z)而獲得。
(步驟(Z))
於第1連接層之導電粒子側之相反面，較佳為與第2連接層同樣地形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層。藉此，可獲得圖5之異向性導電膜。
又，圖5之異向性導電膜100亦可不進行步驟(Z)而藉由 在步驟(A)之前實施以下之步驟(a)而獲得。
(步驟(a))
該步驟係於光聚合性樹脂層之單面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟。藉由繼該步驟(a)後實施步驟(A)、(B)及(C)，可獲得圖5之異向性導電膜100。其中，於步驟(A)中，使導電粒子以單層排列於光自由基聚合性樹脂層之另一面。
(進行二階段光聚合反應之製造方法)
繼而，對以二階段進行光聚合而製造圖1(圖4B)之異向性導電膜之一例進行說明。該製造例具有以下之步驟(AA)~(DD)。
(步驟(AA))
如圖6所示般，使導電粒子4以單層排列於視需要形成於剝離膜30上之光聚合性樹脂層31。作為導電粒子4之排列方法，並無特別限制，可採用日本專利第4789738號之實施例1中對未延伸聚丙烯膜利用雙軸延伸操作之方法，或日本特開2010-33793號公報之使用模具之方法等。再者，作為排列之程度，考慮到連接對象之尺寸、導通可靠性、絕緣性、構裝導電粒子捕捉率等，較佳為二維地相互隔開1~100μm左右地排列。
(步驟(BB))
繼而，如圖7A所示般，藉由對排列有導電粒子4之光聚合性樹脂層31自導電粒子側傾斜地照射紫外線(UV)而使之進行光自由基聚合反應，而形成表面暫時固定有導電粒子4之暫時第1連接層20。藉此，如圖7B所示般，可使位於導電粒子4與暫時第1連接層20之最外表面之間的斜向之暫時第1連接層之區域2X之硬化率低於位於相互鄰接之導電粒子4間之暫時 第1連接層之區域2Y之硬化率。
(步驟(CC))
繼而，如圖8A所示般，於暫時第1連接層20之導電粒子4側表面形成由熱陽離子、陰離子或者自由基聚合性樹脂層所構成之第2連接層3。作為具體之一例，將藉由常用方法而形成於剝離膜40之第2連接層3載置於第1連接層2之導電粒子4側表面，並以不發生過大之熱聚合之程度進行熱壓接。然後，可藉由去除剝離膜30及40而獲得圖8B之暫時異向性導電膜50。
(步驟(DD))
繼而，如圖9A所示般，使用LED光源等自與第2連接層3相反側對暫時第1連接層20照射紫外線，藉此使之進行光自由基聚合反應，而使暫時第1連接層20正式硬化而形成第1連接層2。藉此，可獲得圖9B之異向性導電膜1。該步驟中之紫外線之照射較佳為自垂直於暫時第1連接層之方向進行。又，為了使第1連接層之區域2X與2Y之硬化率差不消失，較佳為介隔遮罩(mask)進行照射，或根據照射部位而對照射光量設置差。
再者，於以2階段進行光自由基聚合之情形時，圖5之異向性導電膜100可藉由在步驟(DD)之後實施以下之步驟(Z)而獲得。
(步驟(Z))
於第1連接層之導電粒子側之相反面，較佳為與第2連接層同樣地形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層。藉此，可獲得圖5之異向性導電膜。
又，圖5之異向性導電膜100亦可不進行步驟(Z)而藉由 在步驟(AA)之前實施以下之步驟(a)而獲得。
(步驟(a))
該步驟係於光聚合性樹脂層之單面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟。藉由繼該步驟(a)之後實施步驟(AA)~(DD)，可獲得圖5之異向性導電膜100。其中，於步驟(AA)中，使導電粒子以單層排列於光聚合性樹脂層之另一面。於該情形時，作為第2連接層形成時所使用之聚合起始劑，較佳為應用熱聚合起始劑。於為光聚合起始劑之情形時，有步驟上會對作為異向性導電膜之產品壽命、連接及連接構造體之穩定性造成不良影響之虞。
《本發明之第2態樣之異向性導電膜之製造方法》
本發明之第2態樣之異向性導電膜之製造方法中，與第1態樣之異向性導電膜之製造方法同樣地，可列舉：進行一階段光聚合反應之製造方法、及進行二階段光聚合反應之製造方法。
<進行一階段光聚合反應之製造方法>
對以一階段進行光聚合而製造圖10(圖13B)之異向性導電膜之一例進行說明。該製造例具有以下之步驟(A')~(C')。
(步驟(A'))
如圖11所示般，使導電粒子4以單層排列於視需要形成於剝離膜30上之光聚合性樹脂層31。作為導電粒子4之排列方法，並無特別限制，可採用日本專利第4789738號之實施例1中對未延伸聚丙烯膜利用雙軸延伸操作之方法，或日本特開2010-33793號公報之使用模具之方法等。再者，作 為排列之程度，考慮到連接對象之尺寸、導通可靠性、絕緣性、構裝導電粒子捕捉率等，較佳為二維地相互隔開1~100μm左右而排列。
(步驟(B'))
繼而，如圖12A所示般，使用LED光源等自導電粒子側對排列有導電粒子4之光聚合性樹脂層31自至少2個方向傾斜地照射紫外線(UV)，藉此使之進行光聚合反應，而形成表面固定有導電粒子4之第1連接層2。藉此，如圖12B所示般，可使位於導電粒子4與第1連接層2之最外表面之間的第1連接層之區域2X(換言之，第1連接層之導電粒子背側區域)之硬化率低於位於相互鄰接之導電粒子4間的第1連接層之區域2Y之硬化率。換言之，於第1連接層2中，可使第1連接層2之導電粒子附近區域中相對接近第1連接層2之另一面(最外表面2b)的區域(第1連接層之區域2X)之硬化率低於第2連接層側之第1連接層2之區域2Y之硬化率。藉由以上述方式進行，而第1連接層之導電粒子背側區域之硬化率確實地降低，使接合時之壓入變得容易，且亦可防止導電粒子之流動。
所謂「自至少2個方向傾斜地進行」中之方向，為相交之方向，且其等之方向亦可不處於同一面內。於為2個方向之情形時，較佳為相對於光聚合性樹脂層31在垂直之平面內線對稱地呈傾斜。關於傾斜角θ，相對於光聚合性樹脂層31較佳為0°<θ≦90°、更佳為30°≦θ≦60°。再者，於為多個方向時，較佳為具有相同之傾斜角，但亦可具有不同之傾斜角。例如，可列舉：一個傾斜角θ為30°而另一個傾斜角θ為60°之情形，又，一個傾斜角θ為90°而另一個傾斜角θ為30°之情形等。如此，藉由自2個以上方向傾斜地進行光照射，而可使硬化率相對較低之區域即第1連接 層之區域2X部分存在於導電粒子之背側區域。又，亦可藉由使2個方向之傾斜角度不對稱，而控制第1連接層之區域2X之位置。
(步驟(C'))
繼而，如圖13A所示般，於第1連接層2之導電粒子4側表面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第2連接層3。作為具體之一例，將藉由常用方法而形成於剝離膜40之第2連接層3載置於第1連接層2之導電粒子4側表面，並以不發生過大之熱聚合之程度進行熱壓接。然後，可藉由去除剝離膜30及40而獲得圖13B之異向性導電膜。
再者，圖14之異向性導電膜100可藉由在步驟(C')之後與本發明之第1態樣之異向性導電膜之製造方法同樣地實施以下之步驟(Z)而獲得。
(步驟(Z))
於第1連接層之導電粒子側之相反面，較佳為與第2連接層同樣地形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層。藉此，可獲得圖14之異向性導電膜。
又，圖14之異向性導電膜100與本發明之第1態樣之異向性導電膜之製造方法同樣地，亦可不進行步驟(Z)而藉由在步驟(A')之前實施以下之步驟(a)而獲得。
(步驟(a))
該步驟係於光聚合性樹脂層之單面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟。藉由繼該步驟(a)之後實施步驟(A')、(B')及(C')，可獲得圖14之異向性導電膜100。其中， 於步驟(A')中，使導電粒子以單層排列於光聚合性樹脂層之另一面。
(進行二階段光聚合反應之製造方法)
繼而，對以二階段進行光聚合而製造圖10(圖13B)之異向性導電膜之一例進行說明。該製造例具有以下之步驟(AA')~(DD')。
(步驟(AA'))
如圖15所示般，使導電粒子4以單層排列於視需要形成於剝離膜30上之光聚合性樹脂層31。作為導電粒子4之排列方法，並無特別限制，可採用日本專利第4789738號之實施例1中對未延伸聚丙烯膜利用雙軸延伸操作之方法，或日本特開2010-33793號公報之使用模具之方法等。再者，作為排列之程度，考慮到連接對象之尺寸、導通可靠性、絕緣性、構裝導電粒子捕捉率等，較佳為二維地相互隔開1~100μm左右而排列。
(步驟(BB'))
繼而，如圖16A所示般，自導電粒子側對排列有導電粒子4之光聚合性樹脂層31自至少2個方向傾斜地照射紫外線(UV)，藉此使之進行光聚合反應，而形成表面暫時固定有導電粒子4之暫時第1連接層20。藉此，如圖16B所示般，可使位於導電粒子4與暫時第1連接層20之最外表面之間的暫時第1連接層之區域2X之硬化率低於位於相互鄰接之導電粒子4間的暫時第1連接層之區域2Y之硬化率。換言之，於第1連接層20中，可使暫時第1連接層20之導電粒子附近區域中相對接近暫時第1連接層20之另一面(最外表面2b)的區域(暫時第1連接層之區域2X)之硬化率低於暫時第1連接層20之單面(第2連接層側表面)(暫時第1連接層之區域2Y)之硬化率。
(步驟(CC'))
繼而，如圖17A所示般，於暫時第1連接層20之導電粒子4側表面形成由熱陽離子、陰離子或者自由基聚合性樹脂層所構成之第2連接層3。作為具體之一例，將藉由常用方法而形成於剝離膜40之第2連接層3載置於第1連接層2之導電粒子4側表面，並以不發生過大之熱聚合之程度進行熱壓接。然後，可藉由去除剝離膜30及40而獲得圖17B之暫時異向性導電膜50。
(步驟(DD'))
繼而，如圖18A所示般，使用LED光源等自與第2連接層3相反側對暫時第1連接層20照射紫外線，藉此使之進行光聚合反應，而使暫時第1連接層20正式硬化而形成第1連接層2。藉此，可獲得圖18B之異向性導電膜1。該步驟中之紫外線之照射較佳為自垂直於暫時第1連接層20之方向進行。又，為了使第1連接層之區域2X與2Y之硬化率差不消失，較佳為介隔遮罩進行照射，或根據照射部位而於照射光量設置差。
再者，於以2階段進行光聚合之情形時，圖14之異向性導電膜100可與本發明之第1態樣之異向性導電膜之製造方法同樣地，藉由在步驟(DD')之後實施以下之步驟(Z)而獲得。
(步驟(Z))
於第1連接層之導電粒子側之相反面，較佳為與第2連接層同樣地形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層。藉此，可獲得圖5之異向性導電膜。
又，圖14之異向性導電膜100亦可與本發明之第1態樣之 異向性導電膜之製造方法同樣地，不進行步驟(Z)而藉由在步驟(AA')之前實施以下之步驟(a)而獲得。
(步驟(a))
該步驟係於光聚合性樹脂層之單面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟。藉由繼該步驟(a)之後實施步驟(AA')~(DD')，可獲得圖14之異向性導電膜100。其中，於步驟(AA')中，使導電粒子以單層排列於光聚合性樹脂層之另一面。於該情形時，作為第2連接層形成時所使用之聚合起始劑，較佳為應用熱聚合起始劑。於為光聚合起始劑之情形時，有步驟上會對作為異向性導電膜之產品壽命、連接及連接構造體之穩定性造成不良影響之虞。
《連接構造體》
以上述方式所獲得之本發明之異向性導電膜可較佳地應用於將IC晶片、IC模組等第1電子零件與撓性基板、玻璃基板等第2電子零件進行異向性導電連接之時。以上述方式獲得之連接構造體亦為本發明之一部分。再者，將異向性導電膜之第1連接層側配置於撓性基板等第2電子零件側，並將第2連接層側配置於IC晶片等第1電子零件側時，於提高導通可靠性方面較佳。
實施例
以下，利用實施例具體地說明本發明。
實施例1~3、比較例1
依據日本專利第4789738號之實施例1(導電粒子之均等配置)之操作進行導電粒子之排列，並且依照表1所示之組成(質量份)製成使第1連 接層與第2連接層積層而成之2層構造之異向性導電膜。
(第1連接層)
具體而言，首先，利用乙酸乙酯或甲苯將丙烯酸酯化合物及光自由基聚合起始劑等以固形物成分成為50質量%之方式製備混合液。將該混合液以乾燥厚度成為5μm之方式塗佈於厚度50μm之聚對苯二甲酸乙二酯膜，並於80℃之烘箱中乾燥5分鐘，藉此形成第1連接層之前驅層即光自由基聚合性樹脂層。
繼而，對所獲得之光自由基聚合性樹脂層，使平均粒徑4μm之導電粒子(鍍Ni/Au樹脂粒子、AUL704、積水化學工業(股))相互分隔4μm並以單層排列。進而，自該導電粒子側對光自由基聚合性樹脂層以表1中記載之角度向與異向性導電膜之長邊方向正交之方向照射來自LED光源波長365nm、累計光量4000mJ/cm2之紫外線，藉此形成表面固定有導電粒子之第1連接層。比較例1中，自導電粒子側對光自由基聚合樹脂層以90°之角度照射紫外線。
(第2連接層)
利用乙酸乙酯或甲苯將熱硬化性樹脂及潛伏性硬化劑等以固形物成分成為50質量%之方式製備混合液。將該混合液以乾燥厚度成為12μm之方式塗佈於厚度50μm之聚對苯二甲酸乙二酯膜，並於80℃之烘箱中乾燥5分鐘，藉此形成第2連接層。
(異向性導電膜)
將以上述方式所獲得之第1連接層與第2連接層以導電粒子處於內側之方式進行層壓，藉此獲得異向性導電膜。
(連接構造樣本體)
使用所獲得之異向性導電膜，以50℃、5MPa、1秒之條件將0.5×1.8×20.0mm大小之IC晶片(凸塊尺寸30×85μm、凸塊高度15μm、凸塊間距50μm)暫時貼於0.5×50×30mm大小之康寧公司製造之玻璃配線基板(1737F)，進而以180℃、80MPa、5秒之條件進行構裝而獲得連接構造樣本體。
(試驗評價)
關於所獲得之連接構造樣本體，如以下說明般，對「構裝導電粒子捕捉效率」、「異向性導電連接時之導電粒子之方向性」、「初期導通電阻」、「老化後之導通電阻」、「短路發生率」進行試驗、評價。將所獲得之結果示於表1。
「構裝導電粒子捕捉率」
求出構裝時加熱加壓後連接構造樣本體之凸塊實際捕捉到之粒子量相對於加熱加壓前存在於連接構造樣本體之凸塊上之理論粒子量的比率。粒子量係使用光學顯微鏡進行計數。實際使用上較理想為50%以上。
「異向性導電連接時之導電粒子之方向性」
利用光學顯微鏡觀測異向性導電連接後之凸塊所捕捉到之導電粒子，研究是否可藉由LED之傾斜而獲得流動方向之均一性。數出2個以上連接而成之導電粒子之群100單位(計200個)，將該等之中70%以上方向一致者記作「均一」，將未達者記作「無規」。
「初期導通電阻」
使用數位萬用錶(Agilent Technologies(股))測定連接構造樣本體之導通電阻值。
「老化後之導通電阻」
將連接構造樣本體於85℃、85%RH之高溫高濕環境下放置500小時後，使用數位萬用錶(Agilent Technologies(株))測定其導通電阻。實際使用上較理想為4Ω以下。
「短路發生率」
求出7.5μm間隔之梳齒TEG(Test Element Group，測試元件組)圖案之短路發生率。若實際使用上為100ppm以下，則絕緣性可判斷為良好。
根據表1可知，對於實施例1~3之異向性導電膜，於其製造時傾斜地進行UV照射，因此，與比較例1相比不僅構裝導電粒子捕捉率稍有提高，亦可將異向性導電連接時之導電粒子之流動方向性調整為均一。結果可知，與比較例相比而可大幅降低短路之發生率。
實施例4~9、比較例2~3
依據日本專利第4789738號之實施例1之操作而進行導電粒子之排列， 並且依據表1所示之組成(質量份)製成使第1連接層與第2連接層積層而成之2層構造之異向性導電膜。
(第1連接層)
具體而言，首先，利用乙酸乙酯或甲苯將丙烯酸酯化合物及光自由基聚合起始劑等以固形物成分成為50質量%之方式製備混合液。將該混合液以乾燥厚度成為5μm之方式塗佈於厚度50μm之聚對苯二甲酸乙二酯膜，並於80℃之烘箱中乾燥5分鐘，藉此形成第1連接層之前驅層即光自由基聚合性樹脂層。
繼而，對所獲得之光自由基聚合性樹脂層，使平均粒徑4μm之導電粒子(鍍Ni/Au樹脂粒子、AUL704、積水化學工業(股))相互分隔4μm並以單層排列。進而，自該導電粒子側對光自由基聚合性樹脂層以表2所示之方向及角度照射來自LED光源波長365nm、累計光量4000mJ/cm2之紫外線，藉此，形成表面固定有導電粒子之第1連接層。
再者，於實施例4~6中，自導電粒子側對光自由基聚合性樹脂層，從於垂直平面內分別呈60°之角度且夾角成為60°之2個方向照射紫外線。於實施例7中，自導電粒子側對光自由基聚合性樹脂層，從於垂直平面內呈60°及30°之角度且夾角成為90°之2個方向照射紫外線。於實施例8中，自導電粒子側對光自由基聚合性樹脂層，從於垂直平面內為90°及30°之角度且夾角成為60°之2個方向照射紫外線。於實施例9中，自導電粒子側對光自由基聚合性樹脂層，從於垂直平面內為90°之方向及60°之角度且夾角成為30°之2個方向照射紫外線。比較例2中，自光自由基聚合性樹脂層之背面(未排列導電粒子一側之表面)以90°之角度照射紫外線。比較例3 中，相反地，自導電粒子側對光自由基聚合性樹脂層呈90°以一方向照射紫外線。
(第2連接層)
利用乙酸乙酯或甲苯將熱硬化性樹脂及潛伏性硬化劑等以固形物成分成為50質量%之方式製備混合液。將該混合液以乾燥厚度成為12μm之方式塗佈於厚度50μm之聚對苯二甲酸乙二酯膜，並於80℃之烘箱中乾燥5分鐘，藉此形成第2連接層。
(異向性導電膜)
將以上述方式所獲得之第1連接層與第2連接層以導電粒子處於內側之方式進行層壓，藉此獲得異向性導電膜。
(連接構造樣本體)
使用所獲得之異向性導電膜，以50℃、5MPa、1秒之條件將0.5×1.8×20.0mm大小之IC晶片(凸塊尺寸30×85μm、凸塊高度15μm、凸塊間距50μm)暫時貼於0.5×50×30mm大小之康寧公司製造之玻璃配線基板(1737F)，進而以180℃、80MPa、5秒之條件進行構裝而獲得連接構造樣本體。
(試驗評價)
為了對所獲得之連接構造樣本體研究連接時於凸塊平面內之導電粒子之表現，而按以下說明之方式研究「第1連接層中成為90%以上之硬化率之厚度比率(%)」、「載置於凸塊邊緣之導電粒子之比率(%)」、及「凸塊平面內之平均導電粒子間距離(μm)」。將所獲得之結果示於表2。
「第1連接層中成為90%以上之硬化率之厚度比率(%)」
利用剖面研磨使第1連接層之剖面自連接構造樣本體露出，對所露出 之導電粒子之附近有無乙烯基進行IR測定，求出硬化率成為90%以上之區域之厚度相對於總厚度的比率。
「載置於凸塊邊緣之導電粒子之比率(%)」
製造連接構造樣本體時，使用光學顯微鏡對暫時貼附時載置於凸塊邊緣(凸塊之6μm寬之外緣部)之導電粒子數進行計數，又，對構裝後存在於相同外緣部之導電粒子數進行計數，求出構裝後之導電粒子數相對於暫時貼附時之導電粒子數的比率。
「凸塊平面內之平均導電粒子間距離(μm)」
對於連接構造體樣本體之凸塊平面內之100個導電粒子，使用光學顯微鏡測定導電粒子之相互間距離，求出測定結果之算數平均值並作為平均導電粒子間距離。
根據表2可知，關於實施例4~9之異向性導電膜，於第1連接層中導電粒子附近區域之下方(與第2連接層相反之側之第1連接層表面方向)之區域中，硬化率成為90%以上之厚度之比率為20~90%，因此，構裝時一面能以導電粒子不發生位置偏移之方式，換言之，抑制在平面方向之活動，一面良好地壓入，結果，凸塊上之導電粒子間距離難以變化，而導電粒子自凸塊邊緣流出至凸塊外之比率大幅減少。可知，因此，可實現良好之導通可靠性、良好之絕緣性、及良好之構裝導電粒子捕捉率。
相對於此，關於比較例2之異向性導電膜，可知，由於第1連接層之整體為90%以上之硬化率，故而無法一面抑制在平面方向之活動一面良好地壓入，結果，凸塊上之導電粒子間距離擴大，導電粒子自凸塊邊緣流出至凸塊外之比率大幅增加。關於比較例3之異向性導電膜，可知，並未自2個方向照射紫外線，而自導電粒子側從90°方向(垂直方向)此一個方向照射紫外線，因此，於導電粒子下方，成為90%以上之硬化率之比率過小為未達10%，因此，與實施例4~6相比，無法一面抑制在平面方向之活動一面良好地壓入，結果，凸塊上之導電粒子間距離擴大，而導電粒子自凸塊邊緣流出至凸塊外的比率大幅增加。
[產業上之可利用性]
本發明之第1態樣之異向性導電膜具有使將光自由基聚合性樹脂層進行光自由基聚合而獲得之第1連接層與第2連接層積層而成的2層構造，該第2連接層積層係由熱或光陽離子或者陰離子聚合性樹脂層、或較佳為含有丙烯酸酯化合物與熱或光自由基聚合起始劑之熱或光自由基聚合性樹脂層所構成，進而，於第1連接層之第2連接層側表面以單層排 列有異向性導電連接用之導電粒子。而且，關於第1連接層之硬化率，具有硬化率較單面(第2連接層側表面)之硬化率低的區域，其斜向地存在於第1連接層之厚度方向。因此，異向性導電連接時，可使導電粒子之流動方向均一化。因此，顯示良好之導通可靠性、絕緣性、構裝導電粒子捕捉率。
本發明之第2態樣之異向性導電膜具有由光聚合樹脂層所構成之第1連接層、與由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第2連接層積層而成的2層構造，進而，於第1連接層之第2連接層側表面以單層排列有異向性導電連接用之導電粒子。而且，第1連接層之導電粒子附近區域中相對接近第1連接層之另一面之區域之硬化率低於第1連接層之單面(第2連接層側表面)之硬化率。因此，顯示良好之導通可靠性、絕緣性、構裝導電粒子捕捉率。因此，可用於IC晶片等電子零件對配線基板之異向性導電連接。上述電子零件之配線正朝狹小化發展，本發明於對上述技術進步做貢獻之情形時，尤其表現該效果。

Claims (25)

  1. 一種異向性導電膜，其具有第1連接層及形成於第1連接層單面之第2連接層，其特徵在於：第1連接層為光聚合樹脂層，第2連接層為熱或光陽離子、陰離子或者自由基聚合性樹脂層，於第1連接層之該單面以單層排列有異向性導電連接用之導電粒子，關於第1連接層之硬化率，具有硬化率較該單面之硬化率低之區域，其斜向地存在於第1連接層之厚度方向。
  2. 一種異向性導電膜，其具有第1連接層及形成於第1連接層單面之第2連接層，其特徵在於：第1連接層為光聚合樹脂層，第2連接層為熱或光陽離子、陰離子或者自由基聚合性樹脂層，於第1連接層之該單面以單層排列有異向性導電連接用之導電粒子，與第1連接層之該單面之硬化率相比，第1連接層之導電粒子附近區域中相對接近第1連接層之另一面之區域之硬化率較低。
  3. 如申請專利範圍第1或2項之異向性導電膜，其中，第1連接層係使含有丙烯酸酯化合物及光自由基聚合起始劑之光自由基聚合性樹脂層進行光自由基聚合而成之光自由基聚合樹脂層。
  4. 如申請專利範圍第3項之異向性導電膜，其中，第1連接層進而含有環氧化合物，及熱或光陽離子或者陰離子聚合起始劑。
  5. 如申請專利範圍第1至4項中任一項之異向性導電膜，其中，第2連接層係熱或光陽離子或者陰離子聚合性樹脂層，或熱或光自由基聚合性樹脂層，又，上述熱或光陽離子或者陰離子聚合性樹脂層含有環氧化合物及熱或光陽離子或者陰離子聚合起始劑，上述熱或光自由基聚合性樹脂層含有丙烯酸酯化合物及熱或光自由基聚合起始劑。
  6. 如申請專利範圍第5項之異向性導電膜，其中，第2連接層係含有環氧化合物及熱或光陽離子或者陰離子聚合起始劑之熱或光陽離子或者陰離子聚合性樹脂層，進而含有丙烯酸酯化合物及熱或光自由基聚合起始劑。
  7. 如申請專利範圍第1至6項中任一項之異向性導電膜，其中，導電粒子沒入第2連接層。
  8. 如申請專利範圍第1至7項中任一項之異向性導電膜，其中，第1連接層之最低熔融黏度高於第2連接層之最低熔融黏度。
  9. 一種申請專利範圍第1項之異向性導電膜之製造方法，其具有以下之步驟(A)~(C)：步驟(A)使導電粒子以單層排列於光聚合性樹脂層之步驟；步驟(B)對排列有導電粒子之光聚合性樹脂層傾斜地照射紫外線，藉此使之進行光聚合反應，而形成表面固定有導電粒子之第1連接層的步驟；及步驟(C)於第1連接層之導電粒子側表面，形成由熱或光陽離子或者陰離子 聚合性樹脂層、或熱或光自由基聚合性樹脂層所構成之第2連接層的步驟。
  10. 如申請專利範圍第9項之製造方法，其中，自光聚合性樹脂層之排列有導電粒子之側進行步驟(B)之紫外線照射。
  11. 一種申請專利範圍第1項之異向性導電膜之製造方法，其具有以下之步驟(AA)~(DD)：步驟(AA)使導電粒子以單層排列於光聚合性樹脂層之步驟；步驟(BB)對排列有導電粒子之光聚合性樹脂層傾斜地照射紫外線，藉此使之進行光聚合反應，而形成表面暫時固定有導電粒子之暫時第1連接層的步驟；步驟(CC)於暫時第1連接層之導電粒子側表面形成由熱陽離子、陰離子或者自由基聚合性樹脂層所構成之第2連接層的步驟；及步驟(DD)自與第2連接層相反之側對暫時第1連接層照射紫外線，藉此使之進行光聚合反應，而使暫時第1連接層正式硬化而形成第1連接層的步驟。
  12. 如申請專利範圍第11項之製造方法，其中，自光聚合性樹脂層之排列有導電粒子之側進行步驟(BB)之紫外線照射。
  13. 如申請專利範圍第9項之製造方法，其中，於步驟(C)之後具有以下 之步驟(Z)：步驟(Z)於第1連接層之導電粒子側之相反面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟。
  14. 如申請專利範圍第9項之製造方法，其中，於步驟(A)之前具有以下之步驟(a)：步驟(a)於光聚合性樹脂層之單面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟，於步驟(A)中，於光聚合性樹脂層之另一面使導電粒子以單層排列。
  15. 如申請專利範圍第11項之製造方法，其中，於步驟(DD)之後具有以下之步驟(Z)：步驟(Z)於第1連接層之導電粒子側之相反面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟。
  16. 如申請專利範圍第11項之製造方法，其中，於步驟(AA)之前具有以下之步驟(a)：步驟(a)於光聚合性樹脂層之單面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟，於步驟(AA)中，於光聚合性樹脂層之另一面使導電粒子以單層 排列。
  17. 一種申請專利範圍第2項之異向性導電膜之製造方法，其具有以下之步驟(A')~(C')：步驟(A')使導電粒子以單層排列於光聚合性樹脂層之步驟；步驟(B')對排列有導電粒子之光聚合性樹脂層自至少2個方向傾斜地照射紫外線，藉此使之進行光聚合反應，而形成表面固定有導電粒子之第1連接層的步驟；及步驟(C')於第1連接層之導電粒子側表面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第2連接層的步驟。
  18. 如申請專利範圍第17項之製造方法，其中，自光聚合性樹脂層之排列有導電粒子之側進行步驟(B')之紫外線照射。
  19. 一種申請專利範圍第2項之異向性導電膜之製造方法，其具有以下之步驟(AA')~(DD')：步驟(AA')使導電粒子以單層排列於光聚合性樹脂層之步驟；步驟(BB')對排列有導電粒子之光聚合性樹脂層自至少2個方向傾斜地照射紫外線，藉此使之進行光聚合反應，而形成表面暫時固定有導電粒子之暫時第1連接層的步驟； 步驟(CC')於暫時第1連接層之導電粒子側表面形成由熱陽離子、陰離子或者自由基聚合性樹脂層所構成之第2連接層的步驟；及步驟(DD')自與第2連接層相反之側對暫時第1連接層照射紫外線，藉此使之進行光聚合反應，使暫時第1連接層正式硬化而形成第1連接層的步驟。
  20. 如申請專利範圍第19項之製造方法，其中，自光聚合性樹脂層之排列有導電粒子之側進行步驟(BB')之紫外線照射。
  21. 如申請專利範圍第17項之製造方法，其中，於步驟(C')之後具有以下之步驟(Z)：步驟(Z)於第1連接層之導電粒子側之相反面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟。
  22. 如申請專利範圍第17項之製造方法，其中，於步驟(A')之前具有以下之步驟(a)：步驟(a)於光聚合性樹脂層之單面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟，於步驟(A')中，於光聚合性樹脂層之另一面使導電粒子以單層排列。
  23. 如申請專利範圍第19項之製造方法，其中，於步驟(DD')之後具有以下之步驟(Z)： 步驟(Z)於第1連接層之導電粒子側之相反面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟。
  24. 如申請專利範圍第19項之製造方法，其中，於步驟(AA')之前具有以下之步驟(a)：步驟(a)於光聚合性樹脂層之單面形成由熱或光陽離子、陰離子或者自由基聚合性樹脂層所構成之第3連接層的步驟，於步驟(AA')中，於光聚合性樹脂層之另一面使導電粒子以單層排列。
  25. 一種連接構造體，其係利用申請專利範圍第1至8項中任一項之異向性導電膜將第1電子零件異向性導電連接於第2電子零件而成。
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