TW201606036A - 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
TW201606036A
TW201606036A TW104103699A TW104103699A TW201606036A TW 201606036 A TW201606036 A TW 201606036A TW 104103699 A TW104103699 A TW 104103699A TW 104103699 A TW104103699 A TW 104103699A TW 201606036 A TW201606036 A TW 201606036A
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Taiwan
Prior art keywords
layer
conductive particles
resin layer
connection
anisotropic conductive
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TW104103699A
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English (en)
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TWI664262B (zh
Inventor
Reiji Tsukao
Yasushi Akutsu
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Dexerials Corp
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Priority claimed from JP2014019866A external-priority patent/JP6233069B2/ja
Priority claimed from JP2014019855A external-priority patent/JP6409281B2/ja
Application filed by Dexerials Corp filed Critical Dexerials Corp
Publication of TW201606036A publication Critical patent/TW201606036A/zh
Application granted granted Critical
Publication of TWI664262B publication Critical patent/TWI664262B/zh

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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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
    • H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; 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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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於第1連接層之埋入率成為80%以上之方式或成為1%以上且20%以下之方式排列。

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，使導電粒子以按特定比率掩埋之方式以單層排列於光聚合性樹脂層，此後，藉由照射紫外線而將導電粒子固定化或者暫時固定化，進而於經固定化或者暫時固定化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，藉此獲得異向性導電膜，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，且導電粒子於第1連接層之埋入率為80%以上或為1%以上且20%以下。
此處，埋入率係指導電粒子掩埋於第1連接層之程度，可定義為導電 粒子掩埋至第1連接層中之深度Lb相對於導電粒子之粒徑La的比率(埋入率)，可按「埋入率(%)=(Lb/La)×100」之式求出。
再者，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，其係上述異向性導電膜之製造方法，其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) 使導電粒子以導電粒子於第1連接層之埋入率成為80%以上之方式或成為1%以上且20%以下之方式以單層排列於光聚合性樹脂層的步驟；步驟(B)藉由對排列有導電粒子之光聚合性樹脂層照射紫外線而使之進行光聚合反應，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)使導電粒子以導電粒子於第1連接層之埋入率成為80%以上之方式或成為1%以上且20%以下之方式以單層排列於光聚合性樹脂層的步驟；步驟(BB)藉由對排列有導電粒子之光聚合性樹脂層照射紫外線而使之進行光聚合反應，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，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)中第2連接層形成時所使用之起始劑限定於 熱聚合起始劑之原因在於：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，且除了以上之步驟(A)~(C)外於步驟(C)後具有以下之步驟(Z)，或者，除了以上之步驟(AA)~(DD)外於步驟(DD)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，且除了以上之步驟(A)~(C)外於步驟(A)之前亦具有以下之步驟(a)，或者除了以上之步驟(AA)~(DD)外於步驟(AA)之前亦具有以下之步驟(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)之製造方法的步驟(A)或步驟 (AA)中，使導電粒子於光聚合性樹脂層之另一面以導電粒子於第1連接層之埋入率成為80%以上之方式或成為1%以上且20%以下之方式單層地排列即可。
於利用上述步驟設置第3連接層之情形時，出於上述之理由，故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「含有光聚合起始劑之依據本發明之主旨」的異向性導電膜時並無特別限制。
再者，本發明之第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、及形成於其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，異向性導電連接用之導電粒子以導電粒子於第1連接層之埋入率成為80%以上之方式或成為1%以上且20%以下之方式以單層排列。因此，可將導電粒子牢牢固定於第1連接層，尤其，於以埋入率成為80%以上之方式以單層排列之情形時，可將導電粒子更為牢固地固定於第1連接層。想當然，異向性導電膜之貼附性穩定提高，異向性導電連接之生產性亦提高。而且，第1連接層中之導電粒子之下方(背側)之光自由基聚合性樹脂層因導電 粒子之存在而無法充分照射紫外線，因此，硬化率相對降低，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，於以埋入率成為1%以上且20%以下之方式以單層排列之情形時，第1連接層之樹脂量亦不大幅減少，因此，可進一步提高黏著性及接著強度。
再者，於異向性導電連接利用熱之情形時，為與通常之異向性導電膜之連接方法相同的方法。於為利用光者之情形時，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
2X、2Y‧‧‧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
La‧‧‧導電粒子之粒徑
Lb‧‧‧導電粒子埋入第1連接層中之深度
圖1係本發明之異向性導電膜之剖面圖。
圖2係本發明之異向性導電膜之製造步驟(A)之說明圖。
圖3A係本發明之異向性導電膜之製造步驟(B)之說明圖。
圖3B係本發明之異向性導電膜之製造步驟(B)之說明圖。
圖4A係本發明之異向性導電膜之製造步驟(C)之說明圖。
圖4B係本發明之異向性導電膜之製造步驟(C)之說明圖。
圖5係本發明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係本發明之異向性導電膜之製造步驟(BB)之說明圖。
圖7B係本發明之異向性導電膜之製造步驟(BB)之說明圖。
圖8A係本發明之異向性導電膜之製造步驟(CC)之說明圖。
圖8B係本發明之異向性導電膜之製造步驟(CC)之說明圖。
圖9A係本發明之異向性導電膜之製造步驟(DD)之說明圖。
圖9B係本發明之異向性導電膜之製造步驟(DD)之說明圖。
<<異向性導電膜>>
以下，對本發明之異向性導電膜之較佳一例進行詳細說明。
如圖1所示般，本發明之異向性導電膜1具有如下構造：於由使光聚合性樹脂層進行光聚合而成之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，如圖1所示般導電粒子4掩埋於第1連接層2。若將掩埋程度定義為導電粒子4於第1連接層2中之掩埋深度Lb相對於導電粒子4之粒徑La的比率(埋入率)，則埋入率可利用「埋入率(%)=(Lb/La)×100」之式求出。
於本發明中，為了解決「為了實現良好之構裝導電粒子捕捉性而使導電粒子可固定於意圖之位置」之課題，而將導電粒子4對於第1連接層2之埋入率以成為80%以上、較佳為85%以上、更佳為大於90%之方式進行調整。於該情形時，導電粒子4亦可完全埋沒於第1連接層2中，但較佳設為120%以下。
又，於本發明中，為了兼顧良好地解決「為了實現良好之構裝導電粒子捕捉性而使導電粒子可固定於意圖之位置」之課題、與「為了提高第1連接層2與被接著體之間之接著強度而確保存在於導電粒子下方之樹脂量並實現良好之黏著性」之課題，而將導電粒子4於第1連接層2之埋入率以其下限成為1%以上、較佳為大於1%、且上限成為20%以下、較佳為未達20%之方式進行調整。
再者，導電粒子4於第1連接層2之埋入率之調整，例如可藉由利用表面具有剝離材之橡膠輥反覆進行抵壓而進行。具體而言，於使埋入率變小之情形時，減少反覆次數即可，於使埋入率變大之情形時，增多反覆次數即可。
又，於對光聚合性樹脂層照射紫外線而形成第1連接層2之情形時，可自未配置導電粒子一側之面與配置有導電粒子一側之面中之任一者進行照射，但於自配置有導電粒子一側進行照射之情形時，於第1連接層2中，可使位於導電粒子4與第1連接層2之最外表面2b之間的第1連接層之區域2X的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的硬化率。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%。
此處，於自未配置導電粒子之面進行照射之情形時，第1連接層之區域2X與2Y間硬化率之差實質上消失。該情況就ACF之產品品質方面而言，較佳。其原因在於：於ACF製造步驟中，促進導電粒子之固定化，而可確保穩定之品質。且其原因在於：於製作產品而進行通常之長條化時，於捲繞開始及捲繞結束時，可使施加於排列之導電粒子之壓力大致相同，而可防止排列散亂。
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(股份))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，JRGACURE 2959、BASF JAPAN(股份))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，但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)
當第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之2層構造之異向性導電膜，但亦可如圖5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為由熱或光陽離子或者陰離子聚合性樹脂層(較佳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聚合性樹脂層)、或熱或光自由基聚合性樹脂層(較佳為含有丙烯酸酯化合物及熱或光自由基聚合起始劑之聚合性樹脂層)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，再形成於第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(不形成第2連接層之面)預先形成第3連接層。
<<異向性導電膜之製造方法>>
本發明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以埋入率成為80%以上之方式或成為1%以上且20%以下之方式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之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。
埋入率之調整可藉由反覆抵壓橡膠輥等彈性體而進行。
(步驟(B))
繼而，如圖3A所示般，對排列有導電粒子4之光聚合性樹脂層31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。於該情形時，可自導電粒子側照射紫外線(UV)，亦可自相反側照射紫外線，但於自導電粒子側照射紫外線(UV)之情形時，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間的第1連接層之區域2Y之硬化率。藉由如此，粒子背側之硬化性確實變低而使接合時之壓入變得容易，且亦可同時具備防止粒子流動之效果。
(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，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，使導電粒子以埋入率成為80%以上之方式或成為1%以上且20%以下之方式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以埋入率成為80%以上之方式或成為1%以上且20%以下之方式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之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，對排列有導電粒子4之光聚合性樹脂層31照射紫外線(UV)，藉此使之進行光聚合反應，而形成「於表面暫時固定有導電粒子4」之暫時第1連接層20。於該情形時，可自導電粒子側照射紫外線(UV)，亦可自相反側進行照射，但於自導電粒子側照射紫外線(UV)之情形時，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，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9B之異向性導電膜1。該步驟中之紫外線之照射較佳為自相對於暫時第1連接層垂直之方向進行。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異。
再者，於以2階段進行光聚合之情形時，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)而可獲得圖5之異向性導電膜100。其中，於步驟(AA)中，使導電粒子以埋入率成為80%以上之方式或成為1%以上且20%以下之方式以單層排列於光聚合性樹脂層之另一面。於該情形時，作為用於第2連接層形成時之聚合起始劑，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1~6、比較例1
依據日本專利第4789738號之實施例1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，並藉由調整利用橡膠輥之反覆抵壓次數，而使之以導電粒子於第1連接層之埋入率成為粒徑之表1所示之百分比之方式以單層排列。進而，自該導電粒子側對光自由基聚合性樹脂層照射波長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。
(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，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)以180℃、80MPa、5秒之條件構裝於0.5×50×30mm大小之康寧公司製造之玻璃配線基板(1737F)，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，對異向性導電膜之「構裝導電粒子捕捉率」、「導通可靠性」、「連接粒子個數」及「絕緣性」進行試驗評價。將所獲得之結果示於表1。
再者，於評價「絕緣性」時，係使用將0.5×1.5×13mm大小 之IC晶片(鍍金凸塊尺寸25×140μm、凸塊高度15μm、凸塊間間隔7.5μm)以180℃、80MPa、5秒之條件構裝於0.5×50×30mm大小之康寧公司製造之玻璃配線基板(1737F)而獲得的連接構造樣本體。
「構裝導電粒子捕捉率」
依據以下之算式求出“加熱、加壓後(實際構裝後)之連接構造樣本體之凸塊上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。
構裝導電粒子捕捉率(%)= {[加熱加壓後之凸塊上之粒子數]/[加熱加壓前之凸塊上之粒子數]}×100
「導通可靠性」
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，使用數位萬用表(Agilent Technologies(股))測定其導通電阻。實際使用上較理想為4Ω以下。
「連接粒子個數」
利用倍率50倍之電子顯微鏡觀察所獲得之連接構造樣本體之10mm見方之區域，將2個以上導電粒子連接成線狀或者塊狀而成之連接體記作一個連接粒子，並數出上述連接粒子之個數。例如，於2個導電粒子連接而成之連接粒子為2個，4個連接粒子連接而成之連接粒子為1個之情形時，連接粒子數為3個。若連接個數增大，則有構成連接粒子之導電粒子數亦增大之傾向，即，在凸塊間間隔所占之導電粒子其獨立性易受損，因此有短路之發生概率增大之傾向。
「絕緣性(短路之發生率)」
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。實際使用上較理想為100ppm以下。
如根據表1可知，實施例1~6之異向性導電膜為導電粒子於第1連接層之埋入率為80%以上，因此，連接粒子個數亦為10個以下，且關於構裝導電粒子捕捉率、導通可靠性、短路之發生率之各評價項目均顯示實際使用上為佳之結果。
相對於此，比較例1之異向性導電膜為導電粒子於第1連接層之埋入率為低於80%之75%，因此，連接粒子數增大，短路發生率增大為50ppm。
實施例7
於第1連接層形成時，以累計光量2000mJ/cm2照射紫外線，除此以外，與實施例1同樣地製成異向性導電膜。進而，自該異向性導電膜之第1 連接層側以累計光量2000mJ/cm2照射波長365nm之紫外線，藉此，獲得自第1連接層之兩面照射過紫外線之實施例7之異向性導電膜。使用該異向性導電膜，與實施例1之異向性導電膜同樣地製成連接構造樣本體並進行評價，結果獲得大致相同之實際使用上並無問題之結果，關於構裝導電粒子捕捉率有進而改善之傾向。
實施例8~12、比較例2~3
使導電粒子藉由調整利用橡膠輥之反覆抵壓次數而以導電粒子對於第1連接層之埋入率成為粒徑之表2所示之百分比之方式以單層排列，除此以外，重複實施例1之操作，藉此取得異向性導電膜，進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，與實施例1同樣地對異向性導電膜之「構裝導電粒子捕捉率」、「導通可靠性」及「絕緣性(短路發生率)」進行試驗評價，進而，如以下說明般，對「第1連接層側之「黏著力」」及「接著強度(晶片剪切強度)」進行試驗評價。將所獲得之結果示於表2。
如根據表2可知，實施例8~12之異向性導電膜由於導電粒子於第1連接層之埋入率為1%以上且20%以下，因此，關於黏著力、接著強度、構裝導電粒子捕捉率、導通可靠性、絕緣性(短路發生率)之各評價項目均顯示實際使用上為佳之結果。
相對於此，比較例2之異向性導電膜由於導電粒子於第1連接層之埋入率超過20%，因此，與實施例8~12之異向性導電膜相比，黏著力及接著強度變差。又，短路發生率亦增加約2.5倍。比較例3之異向性導電膜由於導電粒子於第1連接層之埋入率低於1%，因此，與實施例8~12之異向性導電膜相比，構裝導電粒子捕捉率降低，又，絕緣性之評價指標即短路發生率亦增加約7.5倍。
實施例13
於第1連接層形成時，以累計光量2000mJ/cm2照射紫外線，除此以 外，與實施例8同樣地製成異向性導電膜。進而，自該異向性導電膜之第1連接層側，以累計光量2000mJ/cm2照射波長365nm之紫外線，藉此，獲得自第1連接層之兩面照射過紫外線之實施例13之異向性導電膜。使用該異向性導電膜，與實施例8之異向性導電膜同樣地製成連接構造樣本體並進行評價，結果獲得大致相同之實際使用上並無問題之結果，關於構裝導電粒子捕捉率有進而改善之傾向。
[產業上之可利用性]
本發明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，異向性導電連接用之導電粒子以於第1連接層之埋入率成為80%以上之方式以單層排列。因此，可將導電粒子良好地固定於第1連接層，而顯示良好之構裝導電粒子捕捉率、導通可靠性、連接粒子個數、絕緣性。又，本發明之異向性導電膜之另一態樣中，異向性導電連接用之導電粒子以於第1連接層之埋入率成為1%以上且20%以下之方式以單層排列。因此，第1連接層顯示良好之黏著性及接著強度，且顯示良好之導通可靠性、絕緣性(短路發生率)、構裝導電粒子捕捉率。因此，該等本發明之異向性導電膜可用於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。
1‧‧‧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‧‧‧第1連接層之區域
3‧‧‧第2連接層
4‧‧‧導電粒子
La‧‧‧導電粒子之粒徑
Lb‧‧‧導電粒子埋入第1連接層中之深度

Claims (16)

  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，且導電粒子於第1連接層之埋入率為80%以上或1%以上且20%以下。
  2. 如申請專利範圍第1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。
  3. 如申請專利範圍第2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。
  4. 如申請專利範圍第1或2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。
  5. 如申請專利範圍第4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，且進而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1至5項中任一項之異向性導電膜，其中，於第1連接層中，位於導電粒子與第1連接層之最外表面之間的區域之第1連接層之硬化率低於位於相互鄰接之導電粒子間的區域之第1連接層之硬化率。
  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，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。
  8. 一種申請專利範圍第1項之異向性導電膜之製造方法，具有以下之步驟(A)~(C)：步驟(A)使導電粒子以導電粒子於第1連接層之埋入率成為80%以上或成為1%以上且20%以下之方式以單層排列於光聚合性樹脂層的步驟；步驟(B)藉由對排列有導電粒子之光聚合性樹脂層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。
  9. 如申請專利範圍第8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。
  10. 一種申請專利範圍第1項之異向性導電膜之製造方法，具有以下之步驟(AA)~(DD)：步驟(AA) 使導電粒子以導電粒子於第1連接層之埋入率成為80%以上或成為1%以上且20%以下之方式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連接層之步驟；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，使暫時第1連接層正式硬化而形成第1連接層之步驟。
  11. 如申請專利範圍第10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。
  12. 如申請專利範圍第8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。
  13. 如申請專利範圍第8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80%以上或1%以上且20%以下之埋入率單層地排列。
  14. 如申請專利範圍第10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。
  15. 如申請專利範圍第10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80%以上或1%以上且20%以下之埋入率單層地排列。
  16. 一種連接構造體，其係利用申請專利範圍第1至7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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