TW201800478A - 異向性導電膜 - Google Patents

異向性導電膜 Download PDF

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Publication number
TW201800478A
TW201800478A TW106104604A TW106104604A TW201800478A TW 201800478 A TW201800478 A TW 201800478A TW 106104604 A TW106104604 A TW 106104604A TW 106104604 A TW106104604 A TW 106104604A TW 201800478 A TW201800478 A TW 201800478A
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Taiwan
Prior art keywords
anisotropic conductive
conductive film
anion
film according
compound
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TW106104604A
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English (en)
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TWI804460B (zh
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林慎一
徳久憲司
山口恵津子
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迪睿合股份有限公司
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    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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Abstract

一種使用脂環式環氧化合物之陽離子聚合性異向性導電膜，其確保與以往同等之硬化溫度與連接可靠性，並且具有比以往更加優異之保管壽命性，該異向性導電膜含有：含有成膜用成分與陽離子聚合性成分之黏合劑組成物、陽離子聚合起始劑及導電粒子。該異向性導電膜使用四級銨鹽系熱酸產生劑作為陽離子聚合起始劑，含有脂環式環氧化合物與低極性氧環丁烷化合物作為陽離子聚合成分。

Description

異向性導電膜
本發明係關於一種異向性導電膜。
以往，將IC晶片等電子零件安裝於配線基板時，廣泛使用導電粒子分散於含有聚合性化合物之絕緣性之黏合劑組成物之異向性導電膜。於此種異向性導電膜中，為了實現低溫快速硬化性，提出使用與通用之環氧丙基醚系化合物相比陽離子聚合反應性較高之脂環式環氧化合物作為聚合性化合物，並且使用藉由熱而產生質子之鋶鹽系熱酸產生劑作為不會由氧導致聚合阻礙、顯示暗反應性之聚合起始劑(專利文獻1~3)。此種含有脂環式環氧化合物與鋶鹽系熱酸產生劑之以往之異向性導電膜顯示相對低溫(例如100℃左右)之硬化溫度。
專利文獻1：日本專利特開平9-176112號公報
專利文獻2：日本專利特開2008-308596號公報
專利文獻3：國際公開2012/018123號
然而，關於如上所述之異向性導電膜，存在由於商業交易之國際化等而自製造至實際使用之時間變長之問題，又，存在有時在未配備空調之倉庫進行保管等問題，存在以下顧慮：自暫貼性或壓痕等觀點而言，其保存穩定性(保管壽命性)降低，或者自密接特性等觀點而言，其連接可靠性降低。
本發明之課題在於，對於使用脂環式環氧化合物之陽離子聚合性異向性導電膜，能夠確保與以往同等之硬化溫度與連接可靠性，並且實現比以往更加優異之保管壽命性。
本發明人發現，除脂環式環氧化合物以外，還以特定比例併用低極性氧環丁烷化合物作為陽離子聚合性化合物，並且，使用四級銨鹽系熱酸產生劑代替鋶鹽系熱酸產生劑作為陽離子聚合起始劑，藉此能夠確保與以往同等之硬化溫度與連接可靠性，並且實現比以往更加優異之保管壽命性，從而完成本發明。
即，本發明提供一種異向性導電膜，其含有：含有成膜用成分與陽離子聚合性成分之黏合劑組成物、陽離子聚合起始劑及導電粒子；陽離子聚合起始劑係四級銨鹽系熱酸產生劑，陽離子聚合性成分含有脂環式環氧化合物與低極性氧環丁烷化合物。
又，本發明提供一種第1電子零件與第2電子零件以上述異向性導電膜異向性導電連接之連接結構體。
本發明之異向性導電膜含有：含有成膜用成分與陽離子聚合性成分之黏合劑組成物、陽離子聚合起始劑及導電粒子，且使用四級銨鹽系熱酸產生劑作為陽離子聚合起始劑，含有脂環式環氧化合物與低極性氧環丁烷化合物作為陽離子聚合性成分。因此，能夠確保與以往同等之硬化溫度與連接可靠性，並且實現比以往更加優異之保管壽命性。
以下，詳細說明本發明之一例。
<異向性導電膜>
本發明之異向性導電膜含有：含有成膜用成分與陽離子聚合性成分之黏合劑組成物、陽離子聚合起始劑及導電粒子。
(黏合劑組成物)
於本發明中，含有導電粒子並將其保持之黏合劑組成物含有成膜用成分與陽離子聚合性成分。
(成膜用成分)
成膜用成分係用於使異向性導電膜成膜，具有膜形成能力之成分。作為此種成膜用成分，可列舉：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，可併用該等之2種以上。於該等之中，自成膜 性、加工性、連接可靠性之觀點而言，能夠較佳地使用苯氧基樹脂。
黏合劑組成物中之成膜用成分之摻合比例較佳為10~70質量%，更佳為20~50質量%。若處於該範圍，則能夠發揮充分之膜形成能力。
(陽離子聚合性成分)
陽離子聚合性成分係使異向性導電膜硬化之成分，含有脂環式環氧化合物與低極性氧環丁烷化合物。黏合劑組成物中之陽離子聚合性成分之摻合量較佳為10~80質量%，更佳為20~60質量%。若處於該範圍，則能夠提供具有更高之硬化速度之黏合劑組成物。
(脂環式環氧化合物)
使用脂環式環氧化合物之原因在於利用比通用之環氧丙基醚型環氧化合物高之反應性，賦予異向性導電膜良好之低溫快速硬化性。作為此種脂環式環氧化合物，可較佳地列舉於分子內具有2個以上之環氧基者。該等可為液狀，亦可為固體狀。具體而言，可列舉：二環氧丙基六氫雙酚A、3',4'-環氧環己烯羧酸3,4-環氧環己烯基甲酯、二環氧聯環己烷等。其中，自能夠確保硬化物之透光性，且快速硬化性亦優異之方面而言，能夠較佳地使用二環氧丙基六氫雙酚A、尤佳為二環氧聯環己烷。
(低極性氧環丁烷化合物)
於本發明中，與脂環式環氧化合物併用低極性氧環丁烷化合物。低極性氧環丁烷化合物係偶極矩為3.0d以下之氧環丁烷化合物，表面張力相對較低，能夠賦予異向性導電膜之膜良好之流平性，結果能夠提高異向性導電膜之保管壽命性。另一方面，低極性氧環丁烷化合物具有提高來源於脂 環式環氧化合物之異向性導電膜之藉由示差掃描熱量計(DSC)測得之反應起始溫度與反應結束溫度的作用。作為此種低極性氧環丁烷化合物，可列舉：3-乙基-3-(2-乙基己氧基甲基)氧環丁烷、3-乙基-3-羥基甲基氧環丁烷、二[1-乙基(3-氧環丁基(oxetanyl))]甲基醚、4,4'-雙[(3-乙基-3-氧環丁基)甲氧基甲基]聯苯等。其中，就表面張力較低、潤濕性優異之方面而言，較佳為3-乙基-3-(2-乙基己氧基甲基)氧環丁烷，尤佳為4,4'-雙[(3-乙基-3-氧環丁基)甲氧基甲基]聯苯。
脂環式環氧化合物與低極性氧環丁烷化合物之摻合比例以質量基準計，較佳為25：75~60：40，更佳為45：55~60：40，特佳為50：50~55：45。若較該範圍增加低極性氧環丁烷化合物之摻合量，則有使反應起始溫度與反應結束溫度上升之傾向，相反，若減少則有保管壽命降低之傾向。因此，藉由調整脂環式環氧化合物與低極性氧環丁烷化合物之摻合比例，能夠控制異向性導電膜之反應起始溫度與反應結束溫度，進而，藉由調整反應時之升溫速度等，亦能夠控制反應時間。
黏合劑組成物根據需要可含有：雙酚A型環氧樹脂、雙酚F型環氧樹脂、酚醛清漆型環氧樹脂、該等之改質環氧樹脂等其他環氧樹脂、矽烷偶合劑、填充劑、軟化劑、促進劑、抗老化劑、著色劑(顏料、染料)、有機溶劑、離子捕捉劑等。又，根據需要，可含有(甲基)丙烯酸酯化合物與自由基聚合起始劑。此處，作為(甲基)丙烯酸酯化合物，可使用以往周知之(甲基)丙烯酸酯單體。例如，可使用單官能(甲基)丙烯酸酯系單體、二官能以上之多官能(甲基)丙烯酸酯系單體。此處，(甲基)丙烯酸酯包括丙烯酸酯與甲基丙烯酸酯。又，作為自由基聚合起始劑，可包含有機過氧化物、偶 氮雙異丁腈等周知之自由基聚合起始劑。
(導電粒子)
本發明之異向性導電膜為了可進行異向性導電連接，於黏合劑組成物中含有導電粒子。作為導電粒子，可自用於以往公知之異向性導電膜者中適當選擇並使用。可列舉例如鎳、鈷、銀、銅、金、鈀等金屬粒子，焊料等合金粒子，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，為了能夠應對配線高度之差異，又，為了抑制導通電阻之上升，且抑制短路之發生，較佳為2.5μm以上且30μm以下，更佳為3μm以上且9μm以下。導電粒子之粒徑可藉由一般之粒度分佈測量裝置進行測量，又，亦可使用粒度分佈測量裝置求出其平均粒徑。
再者，於導電粒子為金屬被覆樹脂粒子之情形時，關於樹脂芯粒子之粒子硬度(20%K值；壓縮彈性變形特性K20)，為了獲得良好之連接可靠性，較佳為100~1000kgf/mm2，更佳為200至500kgf/mm2。關於壓縮彈性變形特性K20，例如，可使用微型壓縮試驗機(MCT-W201，島津製作所股份有限公司)於測量溫度20℃進行測量。
關於導電粒子於異向性導電膜中之豐度，為了抑制導電粒子捕捉效率之降低，且抑制短路之產生，較佳為每1平方mm為50個以上且100000個以下，更佳為200個以上且70000個以下。該豐度之測量可藉由利用光學顯微鏡觀察材料之薄膜而進行。再者，於異向性導電連接前，由於異向性導電膜中之導電粒子存在於黏合劑組成物中，故而存在難以利用光學顯微鏡觀察之情況。於此種情形時，亦可觀察異向性導電連接後之異向 性導電膜。於該情形時，可考慮連接前後之膜厚變化而算出豐度。
再者，導電粒子於異向性導電膜中之豐度可以質量基準進行表示。於該情形時，關於其豐度，於將異向性導電膜之總質量設為100質量份時，於其100質量份中較佳為1質量份以上且30質量份以下、更佳為3質量份以上且10質量份以下之量。
(陽離子聚合起始劑)
本發明之異向性導電膜含有四級銨鹽系熱酸產生劑而非鋶鹽系熱酸產生劑作為陽離子聚合起始劑。其原因係為了提高保管壽命性。作為此種四級銨鹽系熱酸產生劑，可列舉四級銨陽離子與六氟銻酸根陰離子、六氟磷酸根陰離子、三氟甲磺酸根陰離子、全氟丁磺酸根陰離子、二壬基萘磺酸根陰離子、對甲苯磺酸根陰離子、十二烷基苯磺酸根陰離子、或四(五氟苯基)硼酸根陰離子之鹽等。又，作為四級銨陽離子，可列舉NR1R2R3R4+表示之陽離子。其中，R1、R2、R3及R4為直鏈、支鏈或環狀之碳數1~12的烷基或芳基，可分別具有羥基、鹵素、烷氧基、胺基、酯基等。
作為四級銨鹽系熱酸產生劑之具體例，可列舉由King Industries,lnc.製造之CXC-1612、CXC-1733、CXC-1738、TAG-2678、CXC-1614、TAG-2689、TAG-2690、TAG-2700、CXC-1802-60、CXC-1821等。該等可自楠本化成股份有限公司購得。
本發明之異向性導電膜的層厚較佳為3~50μm，更佳為5~20μm。
(異向性導電膜之製造)
本發明之異向性導電膜可藉由將導電粒子與陽離子聚合起始劑溶解於 甲苯等有機溶劑中加至上述黏合劑組成物中製成塗料，並利用公知之成膜化方法將該塗料成膜化而製造。
再者，本發明之異向性導電膜可為單層，但為了減少導電粒子之使用量而降低製造成本卻不降低異向性導電連接時之粒子捕捉性，且省去底部填充劑之填充操作，亦可積層絕緣性樹脂層。於該情形時，本發明之異向性導電膜成為導電粒子含有層/絕緣性樹脂層之2層結構。此種絕緣性樹脂層基本上可由在異向性導電膜使用之黏合劑組成物中不含導電粒子而摻合陽離子聚合起始劑而得之組成物形成。
本發明之異向性導電膜自反應速度控制之觀點而言，較佳將利用示差掃描熱量計測得之反應波峰之反應起始溫度調整至60~80℃，又，將反應結束溫度調整至155~185℃。該等之調整可藉由調整脂環式環氧化合物與低極性氧環丁烷化合物之摻合比例等進行。
<連接結構體>
本發明之異向性導電膜可較佳應用於將IC晶片、IC模組、FPC等第1電子零件與塑膠基板、玻璃基板、剛性基板、陶瓷基板、FPC等第2電子零件進行異向性導電連接時。利用此種本發明之異向性導電膜將第1電子零件與第2電子零件進行異向性導電連接所得之連接結構體亦為本發明之一部分。再者，作為使用異向性導電膜之電子零件之連接方法，可利用公知之方法。
實施例
以下，藉由實施例對本發明進行更加具體之說明。
實施例1
(導電粒子含有層之形成)
將苯氧基樹脂(YP-50，新日鐵住金化學股份有限公司)60質量份、作為脂環式環氧化合物之二環氧聯環己烷(Celloxide8000，大賽璐股份有限公司)10質量份、低極性氧環丁烷化合物(OXBP，宇部興產股份有限公司)20質量份、陽離子熱聚合起始劑(四級銨鹽系熱酸產生劑，商品名CXC-1612，楠本化成股份有限公司)2質量份及平均粒徑3μm之導電性粒子(鍍Ni/Au樹脂粒子，AUL704，積水化學工業股份有限公司)50質量份添加於甲苯中，以固形物成分成為50質量%之方式製備混合液。
藉由將所得之混合液以乾燥厚度成為6μm之方式塗佈於厚度為50μm之聚對酞酸乙二酯剝離膜(PET剝離膜)上，並於60℃之烘箱中乾燥5分鐘而形成導電粒子含有層。
(絕緣性樹脂層之形成)
除不使用導電粒子以外，將與形成導電粒子含有層時使用之原材料相同之原材料添加至甲苯，以固形物成分成為50質量%之方式製備混合液。
藉由將所得之混合液以乾燥厚度成為12μm之方式塗佈於厚度為50μm之PET剝離膜上，並於60℃之烘箱中乾燥5分鐘而形成絕緣性樹脂層。
(異向性導電膜之製作)
藉由於導電粒子含有層以60℃、5MPa層壓絕緣性樹脂層，而獲得由厚度為50μm之一對PET剝離膜夾持之異向性導電膜。
實施例2~4
除如表1所示變更導電粒子含有層及絕緣性樹脂層中之脂環式環氧化 合物(Celloxide8000，大賽璐股份有限公司)與作為低極性氧環丁烷化合物之4,4'-雙[(3-乙基-3-氧環丁基)甲氧基甲基]聯苯(OXBP，宇部興產股份有限公司)之摻合量(比率)以外，與實施例1同樣地獲得異向性導電膜。
比較例1~4
除如表1所示將導電粒子含有層及絕緣性樹脂層中之陽離子熱聚合起始劑更換為鋶鹽系熱酸產生劑(SI-60L，三新化學工業股份有限公司)以外，與實施例1~4同樣地製得異向性導電膜。
實施例5~13、比較例5
除如表1所示變更導電粒子含有層及絕緣性樹脂層中之脂環式環氧化合物(Celloxide8000，大賽璐股份有限公司)與低極性氧環丁烷化合物(OXBP，宇部興產股份有限公司)之摻合量(比率)以外，與實施例1同樣地製得異向性導電膜。
《評價》
針對各實施例及比較例中所得之異向性導電膜如以下所說明般對「保管壽命特性」、「硬化溫度」、「密接特性」及「反應時間」進行試驗或者測量，並進行評價。
<保管壽命特性>
將由一對PET剝離膜夾持之異向性導電膜放入至設定為濕度40%、溫度25℃或30℃之恆溫恆濕室中，放入後每24小時進行取樣，實施以下之暫貼評價及壓接評價，自該等之評價結果綜合性評價保管壽命特性。將所得之結果示於表1。
(暫貼評價)
剝離異向性導電膜之導電粒子含有層側的PET剝離膜，自導電粒子含有層側將異向性導電膜貼附於毛坯玻璃，製作毛坯玻璃與異向性導電膜之積層體。將該積層體以其毛坯玻璃側與設定為45℃之加熱板接觸之方式載置，自異向性導電膜側以手施加壓力，然後，冷卻至室溫。冷卻後，自積層體剝離絕緣性樹脂層側之PET剝離膜，確認是否異向性導電膜未自毛坯玻璃剝離，而僅剝離PET剝離膜。
(壓接評價)
於試驗用IC晶片與試驗用基板之間，以絕緣性樹脂層配置於IC晶片側之方式夾持異向性導電膜，進行加熱加壓(120℃、60MPa、5秒)，製得評價用連接物。確認製得之連接物之壓痕狀態，確認壓痕是否未變淺、未消失而殘存。
(保管壽命特性評價)
於暫貼評價中，將異向性導電膜自毛坯玻璃剝離之時間點設定為保管壽命。又，即便於暫貼評價中異向性導電膜未自毛坯玻璃剝離之情形時，亦將壓接評價中壓痕變淺(消失)之時間點設為保管壽命。
<硬化溫度>
於試驗用IC晶片與試驗用基板之間，以絕緣性樹脂層配置於IC晶片側之方式夾持異向性導電膜，進行加熱加壓(80℃、90℃、100℃、110℃或者120℃、60MPa、5秒)，獲得評價用連接物。對該連接物中之異向性導電膜之反應率如以下說明般進行測量，自其測量結果確定硬化溫度。將所得之結果示於表1。
(反應率測量)
用手捏住評價用連接物之IC晶片並剝下，露出經硬化之異向性導電膜，對異向性導電膜進行取樣。將所得之樣品以濃度成為0.1g/mL之方式溶解於乙腈。另外將硬化前之異向性導電膜以成為相同濃度之方式溶解於乙腈，使用HPLC-MS(WaterS公司)，根據以下之條件確認各單體之波峰強度。根據硬化後之波峰強度之減少量求出於各溫度之反應率，將反應率成為80%以上之溫度設為硬化溫度。
溶劑：於水/乙腈混合溶液(90/10)60質量份中混合乙腈40質量份而得之混合溶劑
流量：0.4mL/min
管柱：10cm、40℃C
注入量：5μL
解析波：210-410nm
<密接特性>
於試驗用IC晶片與試驗用基板之間，以絕緣性樹脂層配置於IC晶片側之方式夾持異向性導電膜，進行加熱加壓(120℃、60MPa、5秒)，獲得評價用連接物。對該連接物使用ETAC公司之型號EHS-411M實施高壓蒸煮試驗(PCT)。具體而言，關於所得之評價用連接物，將連接物放入至設定為121℃、2atm、飽和水蒸氣環境之條件的恆溫恆濕槽中，每24小時進行以下之密接評價。將所得之結果示於表1。
(密接評價)
進行PCT試驗中放入之連接物的外觀確認，目測觀察於異向性導電膜與IC晶片或基板之層間是否產生剝離。
等級 基準
○：IC壓接後，即使於48小時之PCT中亦未觀察到剝離之情形
△：IC壓接後，於24小時之PCT中觀察到剝離，但是於48小時之PCT試驗中未觀察到剝離之情形
×：IC壓接後，於進行PCT之前已經觀察到剝離，或者於24小時之PCT中觀察到剝離之情形
<反應時間>
將自所得之異向性導電膜切出之約5mg的樣品收納至鋁盤(TA Instruments Inc.)，將其放置於DSC測量裝置(Q2000，TA Instruments Inc.)，自30℃至250℃以10℃/分鐘之升溫速度進行示差掃描熱量計(DSC)測量。自所得之DSC曲線圖讀取發熱波峰上升之時間點的溫度作為反應起始溫度，讀取發熱波峰變為基準線之時間點的溫度作為反應結束溫度。又，根據以下之式算出反應時間。將所得之結果示於表1。
反應時間(分鐘)=(反應結束溫度(℃)-反應起始溫度(℃))/10[℃/分鐘]
Figure TW201800478AD00001
《評價結果之考察》
自表1之結果(實施例1與比較例1之對比、實施例2與比較例2之對比、實施例3與比較例3之對比、實施例4與比較例4之對比)可知，若使用四級銨鹽系熱酸產生劑代替鋶鹽系熱酸產生劑，則即使脂環式環氧化合物與低極性氧環丁烷化合物之間之摻合比有所變化，亦可不改變硬化溫度或作為連接可靠性之評價指標的密接特性而大幅度提高保管壽命。
又，自實施例1、5~7及比較例5之對比可知，隨著低極性氧環丁烷化合物相對於脂環式環氧化合物之摻合比例增加，有保管壽命提高之傾向，但是若相對地減少脂環式環氧化合物之摻合量，則有密接特性下降之傾向。相反，自實施例8~13之對比可知，隨著低極性氧環丁烷化合物相對於脂環式環氧化合物之摻合比例減少，有保管壽命下降之傾向。
再者，自於實施例1、實施例5~13、比較例5中進行之DSC測量結果之對比可知，若增加低極性氧環丁烷化合物之摻合量，則有使反應起始溫度與反應結束溫度上升之傾向。
[產業上之可利用性]
使用脂環式環氧化合物之陽離子聚合性之本發明之異向性導電膜可確保與使用鋶鹽系熱酸產生劑之以往之異向性導電膜同等之硬化溫度與連接可靠性，並可實現比以往更加優異之保管壽命性，因此對將IC晶片等電子零件向配線基板進行異向性導電連接有用。

Claims (9)

  1. 一種異向性導電膜，其含有：含有成膜用成分與陽離子聚合性成分之黏合劑組成物、陽離子聚合起始劑及導電粒子；陽離子聚合起始劑係四級銨鹽系熱酸產生劑，陽離子聚合性成分含有脂環式環氧化合物與低極性氧環丁烷化合物。
  2. 如申請專利範圍第1項之異向性導電膜，其中，脂環式環氧化合物與低極性氧環丁烷化合物之摻合比例以質量基準計為25：75~60：40。
  3. 如申請專利範圍第1項之異向性導電膜，其中，脂環式環氧化合物與低極性氧環丁烷化合物之摻合比例以質量基準計為45：55~60：40。
  4. 如申請專利範圍第1至3項中任一項之異向性導電膜，其中，四級銨鹽系熱酸產生劑係四級銨陽離子與六氟銻酸根陰離子、六氟磷酸根陰離子、三氟甲磺酸根陰離子、全氟丁磺酸根陰離子、二壬基萘磺酸根陰離子、對甲苯磺酸根陰離子、十二烷基苯磺酸根陰離子、或者四(五氟苯基)硼酸根陰離子之鹽。
  5. 如申請專利範圍第4項之異向性導電膜，其中，四級銨陽離子係NR1R2R3R4+表示之陽離子，R1、R2、R3及R4係直鏈、支鏈或環狀之碳數1~12的烷基或芳基。
  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，脂環式環氧化合物係二環氧丙基六氫雙酚A或二環氧聯環己烷，低極性氧環丁烷化合物係3-乙基-3-(2-乙基己氧基甲基)氧環丁烷或4,4'-雙[(3-乙基-3-氧環丁基)甲氧基甲基]聯苯。
  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，成膜用 成分係苯氧基樹脂。
  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，藉由示差掃描熱量計測得之反應波峰之反應起始溫度為60~80℃，反應結束溫度為155~185℃。
  9. 一種連接結構體，第1電子零件與第2電子零件係以申請專利範圍第1至8項中任一項之異向性導電膜異向性導電連接。
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