TWI548718B - A circuit-connecting material, and a method of manufacturing the same - Google Patents

A circuit-connecting material, and a method of manufacturing the same Download PDF

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Publication number
TWI548718B
TWI548718B TW102107556A TW102107556A TWI548718B TW I548718 B TWI548718 B TW I548718B TW 102107556 A TW102107556 A TW 102107556A TW 102107556 A TW102107556 A TW 102107556A TW I548718 B TWI548718 B TW I548718B
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Taiwan
Prior art keywords
adhesive layer
adhesive
mass
parts
melt viscosity
Prior art date
Application number
TW102107556A
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English (en)
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TW201343872A (zh
Inventor
Hiroshi Hamachi
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Dexerials Corp
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Publication of TW201343872A publication Critical patent/TW201343872A/zh
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Publication of TWI548718B publication Critical patent/TWI548718B/zh

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/51—Phosphorus bound to oxygen
    • C08K5/52—Phosphorus bound to oxygen only
    • C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02—Electrically-conducting adhesives
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C08K5/0025—Crosslinking or vulcanising agents; including accelerators
    • C—CHEMISTRY; METALLURGY
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    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
    • C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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Description

電路連接材料、及使用其之構裝體之製造方法
本發明係關於一種分散有導電性粒子之電路連接材料、及使用其之構裝體之製造方法。本申請案係基於2012年3月12日於日本提出申請之日本專利申請案編號之日本專利特願2012-054831且主張其優先權者，該申請案係藉由參照而引用於本申請案中。
先前，異向性導電膜(ACF，Anisotrcpic Conductive Film)被用於將半導體等零件安裝於印刷基板。例如於LCD(Liquid Crystal Display)面板之製造中，用於將控制像素之驅動IC(積體電路)接合於玻璃基板之所謂玻璃覆晶技術(COG，Chip-On-Glass)等。
又，近年來，液晶面板中，於連接面形成有IZO(Indium Zinc Oxide)、ITO(Indium Tin Oxide)等穿透度較高之透明導電膜，且於配線之周圍表面形成有SiNx等透明絕緣膜者不斷普及。
對此種液晶面板進行異向性導電連接之情形時，可使用調配有磷酸酯化合物以提高與金屬配線即透明導電膜的密接性，並且調配有矽烷偶合劑以提高與無機物之透明絕緣膜的密接性之異向性導電膜(例如，參照專利文獻1、2)。
然而，若如專利文獻1、2之技術般同時調配磷酸酯化合物 與矽烷偶合劑，則於保管期間磷酸酯作為酸觸媒而發揮作用，使矽烷偶合劑水解，導致壓接時對透明絕緣膜之密接性下降。
[專利文獻1]日本特開2004-43603號公報
[專利文獻2]日本特開2009-277769號公報
本發明係鑒於上述先前之實際情況而提出者，本發明提供一種具有優異之儲存穩定性的電路連接材料、及使用其之構裝體之製造方法。
本案發明者進行努力研究，結果發現藉由將磷酸酯化合物與矽烷偶合劑分開調配於雙層結構之電路連接材料的各層，可改善儲存穩定性。
即，本發明之電路連接材料之特徵在於具有：第1接著層，其含有矽烷偶合劑及導電性粒子；及第2接著層，其含有磷酸酯化合物。
又，本發明之構裝體之製造方法之特徵在於具有如下步驟：於第1電子零件之電極上，將具有第1接著層與第2接著層之異向性導電膜、以及第2電子零件以上述第1接著層位於上述第1電子零件上的方式依序配置之步驟，上述第1接著層含有矽烷偶合劑及導電性粒子，上述第2接著層含有磷酸酯化合物；及利用壓接頭自上述第2電子零件之上表面進行按壓之步驟。
本發明藉由將磷酸酯化合物與矽烷偶合劑分開調配於雙層結構之電路連接材料的各層，而可防止矽烷偶合劑水解，可獲得優異之儲存穩定性。又，因含有矽烷偶合劑之第1接著層中含有導電性粒子，故壓接時可提高與第1電子零件之密接性，進而可提高導電性粒子之粒子捕捉率。
10‧‧‧連接部
11‧‧‧透明導電膜
12‧‧‧透明絕緣膜
圖1係用以說明藉由矽烷偶合劑而提高對無機物之密接性的圖。
圖2係表示液晶面板之連接部之一部分的平面圖。
以下，一面參照圖式一面對本發明之實施形態以下述順序詳細地進行說明。
1.電路連接材料及其製造方法
2.構裝體之製造方法
3.實施例
<1.電路連接材料及其製造方法>
圖1係用以說明藉由矽烷偶合劑而提高對無機物之密接性的圖。如圖1所示，矽烷偶合劑於一分子中具有有機官能基與水解基，壓接時與無機材料之羥基進行脫水縮合，藉此可提高與無機材料之密接性。
由於長期保管，該矽烷偶合劑藉由空氣中之水分進行水解而部分縮合從而生成低聚物，於壓接之前經基不斷減少導致密接力減小。又，於磷酸酯化合物等酸觸媒存在下，矽烷偶合劑之水解受到促進。
針對於此，本實施形態之電路連接材料具有含有矽烷偶合劑及導電性粒子之第1接著層、與含有磷酸酯化合物之第2接著層。藉此，可防止矽烷偶合劑與磷酸酯化合物接觸，可抑制矽烷偶合劑之水解。因此，本實施形態之電路連接材料具有優異之儲存穩定性。
第1接著層中，於含有矽烷偶合劑之接著劑組成物分散有導電性粒子。藉此，例如若將第1接著層配置於塗佈有氮化矽膜之玻璃基板且進行壓接，則可對氮化矽膜獲得較高之密接力，進而，可獲得導電性粒子之高粒子捕捉率。
作為矽烷偶合劑，可列舉：甲基丙烯酸系、乙烯基系、環氧系、苯乙烯基系、丙烯酸系、胺基系、脲基系、巰基系、硫化物系、異氰酸酯系等。具體而言，可列舉：3-甲基丙烯醯氧基丙基三甲氧基矽烷、乙烯基三甲氧基矽烷、2-(3,4-環氧環己基)乙基三甲氧基矽烷、對苯乙烯基三甲氧基矽烷、3-丙烯醯氧基丙基三甲氧基矽烷、N-2-(胺基乙基)-3-胺基丙基甲基二甲氧基矽烷、3-脲基丙基三乙氧基矽烷、3-巰基丙基甲基二甲氧基矽烷、雙(三乙氧基矽烷基丙基)四硫化物、3-異氰酸酯基丙基三乙氧基矽烷等。該等可單獨使用，亦可組合2種以上而使用。該等中，本實施形態中可較佳地使用甲基丙烯酸系矽烷偶合劑。又，矽烷偶合劑之添加量相對於接著劑組成物100質量份，通常為0.01~5質量份。
作為導電性粒子，例如可使用鎳、金、銅等金屬粒子，對樹脂芯粒子實施鍍鎳、鍍銅、鍍金、鍍鈀等所成者等。又，關於導電性粒子之平均粒徑，就連接可靠性之觀點而言，較佳為1~20 μm，更佳為2~10 μm。又，關於接著劑組成物中之導電性粒子之平均粒子密度，就連接可靠 性及絕緣可靠性之觀點而言，較佳為1000~50000個/mm2，更佳為5000~30000個/mm2。
又，第1接著層之接著劑組成物含有膜形成樹脂、聚合性樹脂、及聚合起始劑。
膜形成樹脂相當於平均分子量為10000以上之高分子量樹脂，就膜形成性之觀點而言，平均分子量較佳為10000~80000左右。作為膜形成樹脂，可列舉：苯氧基樹脂、聚酯胺酯樹脂、聚酯樹脂、聚胺酯樹脂、丙烯酸系樹脂、聚醯亞胺樹脂、丁醛樹脂等各種樹脂；該等可單獨使用，亦可組合2種以上而使用。該等中，就膜形成狀態、連接可靠性等觀點而言，可較佳地使用苯氧基樹脂。膜形成樹脂之含量相對於接著劑組成物100質量份，通常為30~80質量份，較佳為40~70質量份。
聚合性樹脂為自由基聚合性樹脂、陽離子聚合性樹脂等，可根據用途而適當選擇。
自由基聚合性樹脂為具有藉由自由基而進行聚合之官能基的物質，可列舉：環氧丙烯酸酯、丙烯酸胺酯、聚酯丙烯酸酯等，該等可單獨使用，亦可組合2種以上而使用。該等中，本實施形態中可較佳地使用環氧丙烯酸酯。自由基聚合性樹脂之含量相對於接著劑組成物100質量份，通常為10~60質量份，較佳為20~50質量份。
使用自由基聚合性樹脂時之自由基聚合起始劑可使用公知者，其中，可較佳地使用有機過氧化物。作為有機過氧化物，可列舉：過氧縮酮類、過氧化二醯基類、過氧化二碳酸酯類、過氧酯類、過氧化二烷基類、過氧化氫類、過氧化矽烷基類等，該等可單獨使用，亦可組合2種 以上而使用。該等中，本實施形態中可較佳地使用過氧縮酮類。自由基聚合起始劑之含量相對於自由基系接著劑組成物100質量份，通常為0.1~30質量份，較佳為1~20質量份。
陽離子聚合性樹脂可使用單官能性環氧化合物、含雜環之環氧樹脂、脂肪族系環氧樹脂等。尤佳為單獨或混合使用雙酚A型環氧樹脂、雙酚F型環氧樹脂、萘型環氧樹脂、酚醛清漆型環氧樹脂等環氧樹脂。
作為使用陽離子聚合性樹脂時之陽離子硬化劑，可使用陽離子種使環氧樹脂末端之環氧基開環而使環氧樹脂彼此自交聯者。作為此種陽離子硬化劑，可列舉：芳香族鋶鹽、芳香族重氮鹽、錪鹽、鏻鹽、硒鹽等鎓鹽。尤其是芳香族鋶鹽於低溫下之反應性優異，且適用期較長，因此作為陽離子硬化劑較佳。
繼而，對第2接著層進行說明。第2接著層為含有磷酸酯化合物之接著劑組成物。藉由磷酸酯化合物，例如可對於形成有IZO(Indium Zinc Oxide)、ITO(Indium Tin Oxide)等金屬配線即透明導電膜的液晶面板獲得較高之密接力。
作為磷酸酯化合物，可列舉具有磷酸酯骨架之磷酸(甲基)丙烯酸酯等，具體而言，例如可列舉：單(2-甲基丙烯醯氧基乙基)酸式磷酸酯(mono(2-methacryloxyethyl)acid phosphate)、二(2-甲基丙烯醯氧基乙基)酸式磷酸酯、二苯基(2-丙烯醯氧基乙基)磷酸酯、二苯基(2-甲基丙烯醯氧基乙基)磷酸酯、苯基(2-丙烯醯氧基乙基)磷酸酯等。該等可單獨使用，亦可組合2種以上而使用。該等中，本實施形態中可較佳地使用單(2-甲基丙烯醯氧基乙基)酸式磷酸酯。磷酸酯化合物之含量相對於組成物100質量份，通常為 0.01~5質量份。
又，第2接著層之接著劑組成物與第1接著層同樣地含有膜形成樹脂、聚合性樹脂、及聚合起始劑。又，膜形成樹脂、聚合性樹脂、及聚合起始劑較佳為使用與第1接著層相同者，且使第1接著層與第2接著層之熔融黏度、最低熔融黏度到達溫度等之差較小。
具體而言，第1接著層之熔融黏度與第2接著層之熔融黏度之差較佳為1000 Pa．s以下。又，第1接著層之最低熔融黏度到達溫度與第2接著層之最低熔融黏度到達溫度之差較佳為15℃以下。藉此，例如於將液晶面板與COF(Chip On Film，覆晶膜)壓接時，第1接著層與第2接著層可良好地摻混，使磷酸酯化合物作用於液晶面板側之配線與COF側之配線兩者。
繼而，對由上述電路連接材料所構成之異向性導電膜之製造方法進行說明。本實施形態之異向性導電膜之製造方法係於含有矽烷偶合劑及導電性粒子之第1接著層上，形成含有磷酸酯化合物之第2接著層。
具體而言，該製造方法具有如下步驟：形成含有矽烷偶合劑及導電性粒子之第1接著層之步驟；形成含有磷酸酯化合物之第2接著層之步驟；將第1接著層與第2接著層貼附之步驟。
於形成第1接著層之步驟中，使膜形成樹脂、聚合性樹脂、聚合起始劑、矽烷偶合劑、導電性粒子溶解於溶劑。作為溶劑，可使用甲苯、乙酸乙酯等、或該等之混合溶劑。製備第1接著層之樹脂組成物後，使用棒式塗佈機、塗佈裝置等而塗佈於脫模基材上。脫模基材例如由將聚矽氧等脫模劑塗佈於PET(Poly Ethylene Terephthalate，聚對苯二甲酸乙二 酯)、OPP(Oriented Polypropylene，延伸聚丙烯)、PMP(Poly-4-methylpentene-1，聚-4-甲基戊烯)、PTFE(Polytetrafluoroethylene，聚四氟乙烯)等之積層結構所構成，可防止異向性導電材料中之樹脂乾燥，並且維持樹脂之形狀。
繼而，利用熱烘箱、加熱乾燥裝置等而將塗佈於脫模基材上之異向性導電材料乾燥。藉此，可獲得厚度5~50 μm左右之第1接著層。
又，形成第2接著層之步驟與第1接著層相同，使膜形成樹脂、聚合性樹脂、聚合起始劑、磷酸酯化合物溶解於溶劑而製備第2接著層之樹脂組成物後，將其塗佈於脫模片，使溶劑揮發而獲得第2接著層。
繼而，於將第1接著層與第2接著層貼附之步驟中，剝離第2接著層之脫模片後貼附於第1接著層上。
藉由以上述方式將第1接著層與第2接著層貼附，可獲得於脫模基材上依序積層有第1接著層與第2接著層之異向性導電膜。
再者，於上述實施形態中，係將第1接著層與第2接著層貼附而製造異向性導電膜，但並不限定於此，亦可於形成一接著層後，塗佈另一接著層之樹脂組成物且使其乾燥而進行製造。
<2.構裝體之安裝方法>
繼而，對使用上述電路連接材料之電子零件之安裝方法進行說明。本實施形態之電子零件之安裝方法具有如下步驟：於第1電子零件之電極上，將具有第1接著層與第2接著層之異向性導電膜、以及第2電子零件以第1接著層位於第1電子零件上的方式依序配置之步驟，上述第1接著層含有矽烷偶合劑及導電性粒子，上述第2接著層含有磷酸酯化合物；及利用壓接頭自第2電子零件之上表面進行按壓之步驟。藉此，可將第1電子零件 之電極與第2電子零件之電極經由導電性粒子而連接，且使異向性導電膜硬化。
此處，作為第1電子零件，可列舉於玻璃基板塗佈有IZO(Indium Zinc Oxide)膜之IZO塗佈玻璃、於玻璃基板塗佈有SiNx(氮化矽)膜之SiNx塗佈玻璃等。又，作為第2電子零件，可列舉COF(Chip On Film)、IC(Integrated Circuit)等。
圖2係表示液晶面板之連接部之一部分的平面圖。如圖2所示，於液晶面板之連接部10，形成有IZO(Indium Zinc Oxide)、ITO(Indium Tin Oxide)等透明導電膜11，於其周圍表面形成有SiNx等透明絕緣膜12。
於本實施形態中，由於係使含有矽烷偶合劑及導電性粒子之第1接著層接觸於液晶面板之連接部10上而進行壓接，故而可對透明絕緣膜12獲得較高之密接力，進而，可獲得導電性粒子之高粒子捕捉率。又，由於第1接著層與第2接著層良好地摻混，故而可使磷酸酯化合物作用於液晶面板之透明導電膜11。
[實施例] <3.實施例>
以下，對本發明之實施例進行說明。此處，製作具有含有矽烷偶合劑及導電性粒子之第1接著層、與含有磷酸酯化合物之第2接著層的異向性導電膜，進行儲存穩定性加速試驗。又，研究第1接著層與第2接著層之熔融黏度及最低熔融黏度到達溫度對接著強度之影響。再者，本發明並不限定於該等實施例。
儲存穩定性加速試驗、接著強度之測定、熔融黏度及最低熔 融黏度到達溫度之測定係以下述方式進行。
[儲存穩定性加速試驗]
利用30℃-80%RH之烘箱，對異向性導電膜進行8小時膜老化。然後，使用老化後之異向性導電膜製作構裝體，測定接著強度。
[接著強度之測定]
使用拉伸試驗機(產品編號：RTC1201，AND公司製造)，對玻璃基板與COF(Chip On Film)之構裝體的初期接著強度進行測定。將測定速度設為50 mm/sec，測定於90度方向上提拉COF時之接著強度。
[熔融黏度及最低熔融黏度到達溫度之測定]
將異向性導電膜重疊成500 μm厚，使用熔融黏度計(HAAKE Rheostress RS-150，Thermo Fisher Scientific公司製造)，於升溫溫度10℃/min、頻率1 Hz、加壓壓力1 N、測定溫度範圍30~180℃之條件下進行測定。
<3.1關於儲存穩定性> [實施例1] (第1接著層之製作)
於由以固形物成分換算為70質量份之苯氧基樹脂(品名：YP-50，東都化成公司製造)、及30質量份自由基聚合性樹脂(品名：EB-600，Daicel-Cytec公司製造)所構成之組成物中，使平均粒徑5 μm之導電性粒子(品名：AUL705，積水化學工業公司製造)以成為粒子密度10000個/mm2之方式分散。繼而，加入反應起始劑(品名：Perhexa C，日本油脂公司製造)2質量份、及矽烷偶合劑(品名：KBM-503，信越化學工業製造)2質量份而製備。使用棒式塗佈機將該接著劑組成物塗佈於PET膜上，利用烘 箱進行乾燥，製作厚度10 μm之第1接著層。
(第2接著層之製作)
將由以固形物成分換算為60質量份之苯氧基樹脂(品名：YP-50，東都化成公司製造)、40質量份自由基聚合性樹脂(品名：EB-600，Daicel-Cytec公司製造)、2質量份反應起始劑(品名：Perhexa C，日本油脂公司製造)、及2質量份磷酸酯丙烯酸酯(品名：P-2M，共榮化學公司製造)所構成之接著劑組成物，使用棒式塗佈機塗佈於PET膜上，並利用烘箱進行乾燥，製作厚度10 μm之第2接著層。
(異向性導電膜之製作)
將厚度10 μm之第1接著層與厚度10 μm之第2接著層貼附，而製作雙層結構之異向性導電膜。
(構裝體之製作)
將切割成1.5 mm寬之異向性導電膜，使用150 μm厚之緩衝材料(聚四氟乙烯)，利用1.5 mm寬工具之暫時壓接機，於70℃-1 MPa-1 sec之條件下暫時壓接於評價用玻璃基板(塗佈有250 nm之IZO(Indium Zinc Oxide)之玻璃)。繼而，於80℃-0.5 MPa-0.5 sec之條件下，利用上述壓接機將評價用COF(50 μmP，Cu8 μmt-鍍Sn，38 μmt)暫時固定，最後於190℃-2 MPa-10 Sec之條件下，利用使用1.5 mm寬工具之正式壓接機進行壓接，製作構裝體。
(評價結果)
將實施例1之評價結果示於表1。於實施例1中，第1接著層及第2接著層之熔融黏度分別為1830 Pa．s、1320 Pa．s，第1接著層及第2接著層之最 低熔融黏度到達溫度分別為117℃、110℃。又，儲存穩定性之加速試驗前及加速試驗後之接著強度分別為8.0 N/cm、7.8 N/cm。
[比較例1] (第1接著層)
於由苯氧基樹脂(品名：YP-50，東都化成公司製造)70質量份、自由基聚合性樹脂(品名：EB-600，Daicel-Cytec公司製造)30質量份所構成之組成物中，使平均粒徑5 μm之導電性粒子(品名：AUL705，積水化學工業公司製造)以成為粒子密度10000個/mm2之方式分散。繼而，加入反應起始劑(品名：Perhexa C，日本油脂公司製造)2質量份、矽烷偶合劑(品名：KBM-503，信越化學工業製造)2質量份、及磷酸酯丙烯酸酯(品名：P-2M，共榮化學公司製造)2質量份而製備，並使用棒式塗佈機將該接著劑組成物塗佈於PET膜上，並利用烘箱進行乾燥，製作厚度10 μm之第1接著層。
(第2接著層)
將由以固形物成分換算為60質量份之苯氧基樹脂(品名：YP-50，東都化成公司製造)、40質量份自由基聚合性樹脂(品名：EB-600，Daicel-Cytec公司製造)、2質量份反應起始劑(品名：Perhexa C，日本油脂公司製造)、2質量份矽烷偶合劑(品名：KBM-503，信越化學工業製造)及2質量份磷酸酯丙烯酸酯(品名：P-2M，共榮化學公司製造)所構成之接著劑組成物，使用棒式塗佈機塗佈於PET膜上，並利用烘箱進行乾燥，製作厚度10 μm之第2接著層。
除第1接著層及第2接著層以外，以與實施例1相同之方式 製作異向性導電膜及構裝體。
(評價結果)
將比較例1之評價結果示於表1。於比較例1中，第1接著層及第2接著層之熔融黏度分別為1830 Pa．s、1320 Pa．s，第1接著層及第2接著層之最低熔融黏度到達溫度分別為117℃、110℃。又，儲存穩定性之加速試驗前及加速試驗後之接著強度分別為7.9 N/cm、2.3 N/cm。
如表1所示，於第1接著層及第2接著層兩者中均調配有矽烷偶合劑及磷酸酯化合物之比較例1中，加速試驗後接著強度下降。另一方面，將磷酸酯化合物與矽烷偶合劑分開調配於第1接著層及第2接著層之各者中之實施例1中，加速試驗後接著強度未下降。因此，可知藉由實施例1可獲得優異之儲存穩定性。
<3.2關於熔融黏度之差> [實施例2] (第2接著層)
將由以固形物成分換算為50質量份之苯氧基樹脂(品名：YP-50，東都化成公司製造)、50質量份自由基聚合性樹脂(品名：EB-600，Daicel-Cytec公司製造)、2質量份反應起始劑(品名：Perhexa C，日本油脂公司製造)、及2質量份磷酸酯丙烯酸酯(品名：P-2M，共榮化學公司製造)所構成之接著劑組成物，使用棒式塗佈機塗佈於PET膜上，並利用烘箱進行乾燥，製作厚度10 μm之第2接著層。
除第2接著層以外，以與實施例1相同之方式製作異向性導電膜及構裝體。
(評價結果)
將實施例2之評價結果示於表2。於實施例2中，第1接著層及第2接著層之熔融黏度分別為1830 Pa．s、830 Pa．s，第1接著層及第2接著層之最低熔融黏度到達溫度分別為117℃、112℃。又，儲存穩定性之加速試驗前及加速試驗後之接著強度分別為8.1 N/cm、7.9 N/cm。
[比較例2] (第2接著層)
將由以固形物成分換算為60質量份之苯氧基樹脂(品名：YP-70，東都化成公司製造)、40質量份自由基聚合性樹脂(品名：EB-600，Daicel-Cytec公司製造)、2質量份反應起始劑(品名：Perhexa C，日本油脂公司製造)、及2質量份磷酸酯丙烯酸酯(品名：P-2M，共榮化學公司製造)所構成之接著劑組成物，使用棒式塗佈機塗佈於PET膜上，並利用烘箱進行乾燥， 製作厚度10 μm之第2接著層。
除第2接著層以外，以與實施例1相同之方式製作異向性導電膜及構裝體。
(評價結果)
將比較例2之評價結果示於表2。於比較例2中，第1接著層及第2接著層之熔融黏度分別為1830 Pa．s、530 Pa．s，第1接著層及第2接著層之最低熔融黏度到達溫度分別為117℃、108℃。又，儲存穩定性之加速試驗前及加速試驗後之接著強度分別為2.8 N/cm、2.5 N/cm。
如表2所示，第1接著層與第2接著層之熔融黏度之差較大的比較例2中，於加速試驗前無法獲得較高之接著強度。另一方面，藉由如實施例1、2般使第1接著層與第2接著層之熔融黏度之差為1000 Pa．s以下，第1接著層與第2接著層可良好地摻混，而獲得較高之接著強度。
<3.3關於最低熔融黏度到達溫度之差> [實施例3] (第2接著層)
將由以固形物成分換算為60質量份之苯氧基樹脂(品名：YP-50，東都化成公司製造)、40質量份自由基聚合性樹脂(品名：EB-600，Daicel-Cytec公司製造)、3質量份反應起始劑(品名：Perhexa C，日本油脂公司製造)、及2質量份磷酸酯丙烯酸酯(品名：P-2M，共榮化學公司製造)所構成之接著劑組成物，使用棒式塗佈機塗佈於PET膜上，並利用烘箱進行乾燥，製作厚度10 μm之第2接著層。
除第2接著層以外，以與實施例1相同之方式製作異向性導電膜及構裝體。
(評價結果)
將實施例3之評價結果示於表3。於實施例3中，第1接著層及第2接著層之熔融黏度分別為1830 Pa．s、1320 Pa．s，第1接著層及第2接著層之最低熔融黏度到達溫度分別為117℃、102℃。又，儲存穩定性之加速試驗前及加速試驗後之接著強度分別為8.2 N/cm、8.0 N/cm。
[比較例3] (第2接著層)
將由以固形物成分換算為60質量份之苯氧基樹脂(品名：YP-50，東都化成公司製造)、40質量份自由基聚合性樹脂(品名：EB-600，Daicel-Cytec公司製造)、5質量份反應起始劑(品名：Perhexa C，日本油脂公司製造)、及2質量份磷酸酯丙烯酸酯(品名：P-2M，共榮化學公司製造)所構成之接著劑組成物，使用棒式塗佈機塗佈於PET膜上，並利用烘箱進行乾燥， 製作厚度10 μm之第2接著層。
除第2接著層以外，以與實施例1相同之方式製作異向性導電膜及構裝體。
(評價結果)
將比較例3之評價結果示於表3。於比較例3中，第1接著層及第2接著層之熔融黏度分別為1830 Pa．s、1320 Pa．s，第1接著層及第2接著層之最低熔融黏度到達溫度分別為117℃、97℃。又，儲存穩定性之加速試驗前及加速試驗後之接著強度分別為3.2 N/cm、2.8 N/cm。
[比較例4] (第2接著層)
將由以固形物成分換算為60質量份之苯氧基樹脂(品名：YP-70，東都化成公司製造)、40質量份自由基聚合性樹脂(品名：EB-600，Daicel-Cytec公司製造)、5質量份反應起始劑(品名：Perhexa C，日本油脂公司製造)、及2質量份磷酸酯丙烯酸酯(品名：P-2M，共榮化學公司製造)所構成之接著劑組成物，使用棒式塗佈機塗佈於PET膜上，並利用烘箱進行乾燥，製作厚度10 μm之第2接著層。
除第2接著層以外，以與實施例1相同之方式製作異向性導電膜及構裝體。
(評價結果)
將比較例4之評價結果示於表3。於比較例4中，第1接著層及第2接著層之熔融黏度分別為1830 Pa．s、530 Pa．s，第1接著層及第2接著層之最低熔融黏度到達溫度分別為117℃、98℃。又，儲存穩定性之加速試驗前及 加速試驗後之接著強度分別為3.2 N/cm、2.8 N/cm。
如表3所示，第1接著層與第2接著層之最低熔融黏度到達溫度之差較大的比較例3中，於加速試驗前無法獲得較高之接著強度。進而，第1接著層與第2接著層之熔融黏度之差較大的比較例4中於加速試驗前亦無法獲得較高之接著強度。另一方面，藉由如實施例1~3般使第1接著層與第2接著層之最低熔融黏度到達溫度之差為15℃以下，第1接著層與第2接著層可良好地摻混，可獲得較高之接著強度。

Claims (7)

  1. 一種電路連接材料，其具有：第1接著層，其含有矽烷偶合劑及導電性粒子，且不含磷酸酯化合物；第2接著層，其含有磷酸酯化合物，且不含矽烷偶合劑。
  2. 如申請專利範圍第1項之電路連接材料，其中上述第1接著層之熔融黏度與上述第2接著層之熔融黏度之差為1000Pa．s以下。
  3. 如申請專利範圍第1項或第2項之電路連接材料，其中上述第1接著層之最低熔融黏度到達溫度與第2接著層之最低熔融黏度到達溫度之差為15℃以下。
  4. 如申請專利範圍第1項或第2項之電路連接材料，其中上述第1接著劑及上述第2接著劑含有自由基聚合性樹脂、及自由基聚合起始劑。
  5. 如申請專利範圍第3項之電路連接材料，其中上述第1接著劑及上述第2接著劑含有自由基聚合性樹脂、及自由基聚合起始劑。
  6. 一種構裝體之製造方法，其具有如下步驟：於第1電子零件之電極上，將具有第1接著層與第2接著層之異向性導電膜、以及第2電子零件以上述第1接著層位於上述第1電子零件上的方式依序配置之步驟，上述第1接著層含有矽烷偶合劑及導電性粒子且不含磷酸酯化合物，上述第2接著層含有磷酸酯化合物且不含矽烷偶合劑；及利用壓接頭自上述第2電子零件之上表面進行按壓之步驟。
  7. 如申請專利範圍第6項之構裝體之製造方法，其中上述第1電子零件為塗佈有氮化矽膜之玻璃基板。
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