TWI658114B - 異方性導電膜組成物、異方性導電膜以及使用所述異方性導電膜的連接結構 - Google Patents

異方性導電膜組成物、異方性導電膜以及使用所述異方性導電膜的連接結構 Download PDF

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TWI658114B
TWI658114B TW105140285A TW105140285A TWI658114B TW I658114 B TWI658114 B TW I658114B TW 105140285 A TW105140285 A TW 105140285A TW 105140285 A TW105140285 A TW 105140285A TW I658114 B TWI658114 B TW I658114B
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conductive film
anisotropic conductive
weight
compound
resin
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TW105140285A
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TW201720888A (zh
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高連助
權純榮
金智軟
金荷娜
朴永祐
徐賢柱
許健寧
黃慈英
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南韓商三星Ｓｄｉ股份有限公司
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    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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Abstract

本發明提供異方性導電膜組成物、使用其製備的異方性 導電膜以及使用所述膜的連接結構。異方性導電膜包含：黏合劑樹脂；包括脂環族環氧化合物和氧雜環丁烷化合物的可固化化合物；季銨催化劑；以及導電粒子，異方性導電膜具有15%或小於15%的熱量變化率，以差示掃描量熱法(DSC)所測量和方程式1所計算：熱量變化率(%)=[(H0-H1)/H0]×100---(1)，其中H0是異方性導電膜的DSC熱量，如在25℃下和0小時的時間點所測量，並且H1是異方性導電膜的DSC熱量，如在40℃下靜置24小時後所測量。異方性導電膜在低溫下實現快速固化，同時展現極佳儲存穩定性和可靠性。

Description

異方性導電膜組成物、異方性導電膜以及使用 所述異方性導電膜的連接結構
本發明是有關於一種異方性導電膜組成物、使用所述異方性導電膜組成物製備的異方性導電膜以及使用所述異方性導電膜的連接結構。
相關申請案的交叉引用-本發明主張2015年12月07日在韓國智慧財產權局提交的韓國專利申請第10-2015-0173398號的權益，所述專利申請的全部公開內容以引用的方式併入本文中。
一般來說，異方性導電膜(anisotropic conductive film，ACF)是指通過使導電粒子分散於如環氧樹脂的樹脂中製備的膜狀黏著劑，並且由異方性黏著劑聚合物膜形成，所述異方性導電膜在膜的厚度方向上展現導電特性並且在其表面方向上展現絕緣特性。
當配置於待連接的電路板之間的異方性導電膜在特定條 件下進行加熱/壓縮時，電路板的重疊電路端線經由導電粒子彼此電連接。另外，相鄰電極之間的空間用絕緣黏合樹脂填充以使導電粒子彼此隔離，從而使得相鄰電極可以彼此電絕緣。
這類異方性導電膜可以在製造平板顯示器，如液晶顯示器和有機發光二極體顯示器時用於將驅動積體電路(integrated circuit,IC)連接到玻璃基板。
最近，由於顯示器面板厚度減小，不斷需要更薄的玻璃基板。然而，當經由異方性導電膜將驅動IC安裝於玻璃基板上時，玻璃基板在加熱和壓縮期間容易彎曲。玻璃基板彎曲導致漏光，從而造成顯示器故障。玻璃基板越薄，彎曲越嚴重，並且使得故障率越高。
為了防止玻璃基板彎曲，需要可以在5秒或小於5秒內，在150℃或小於150℃的低溫下快速固化的異方性導電膜。雖然可以使用具有高反應性的可固化化合物和固化劑來實現此需要，但使用固化化合物和固化劑由於其高反應性而導致儲存穩定性下降並且需要過量穩定劑。日本專利公開案第2012-171980 A號(2012年9月10日)揭示了採用脂環族環氧化合物和氧雜環丁烷化合物作為可固化化合物以及具有特定結構的鋶基潛在陽離子催化劑的異方性導電膜。然而，此異方性導電膜由於脂環族環氧化合物、氧雜環丁烷化合物以及鋶基陽離子催化劑之間的較高反應性而具有較低儲存穩定性的問題。
因此，需要可以在150℃或小於150℃的溫度下快速固 化，同時展現極佳儲存穩定性的異方性導電膜。
本發明提供一種異方性導電膜，其可以解決傳統異方性導電膜所存在的問題。
本發明提供一種異方性導電膜，包括：黏合劑樹脂、包括脂環族環氧化合物以及氧雜環丁烷化合物的可固化化合物、季銨催化劑、以及導電粒子。異方性導電膜具有15%或小於15%的熱量變化率，以差示掃描量熱法所測量以及方程式1所計算：熱量變化率(%)=[(H0-H1)/H0]×100---(1)，其中H0是異方性導電膜以差示掃描量熱法測定的熱量，在25℃下以及0小時的時間點所測量，以及H1是異方性導電膜以差示掃描量熱法測定的熱量，在40℃下靜置24小時後所測量。
本發明還提供一種異方性導電膜組成物，包括：黏合劑樹脂、包括脂環族環氧化合物以及氧雜環丁烷化合物的可固化化合物季銨催化劑以及導電粒子。
本發明還提供連接結構，包括：第一連接構件、第二連接構件以及異方性導電膜。第一連接構件包括第一電極。第二連接構件包括第二電極。異方性導電膜配置於第一連接構件與第二連接構件之間以將第一電極連接到第二電極。異方性導電膜是如前述的異方性導電膜或使用如前述異方性導電膜組成物製備的異方性導電膜。
基於上述，本發明的異方性導電膜具有低熱量變化率和因此高儲存穩定性，展現低DSC放熱起始溫度和低DSC放熱峰值溫度，並且提供其間相對較小的差異，從而在低溫下實現快速固化。
為讓本發明的上述特徵和優點能更明顯易懂，下文特舉實施例，並配合所附圖式作詳細說明如下。
3‧‧‧導電粒子
10‧‧‧異方性導電膜
30‧‧‧連接結構
50‧‧‧第一連接構件
60‧‧‧第二連接構件
70‧‧‧第一電極
80‧‧‧第二電極
圖1是根據本發明的一個實施例的連接結構的剖面圖。
在下文中，將詳細描述本發明的實施例。本文中將省略對所屬領域的技術人員顯而易知的細節描述。
本發明的一種態樣是有關於一種異方性導電膜組成物，包含：黏合劑樹脂；包含脂環族環氧化合物和氧雜環丁烷化合物的可固化化合物；季銨催化劑以及導電粒子。
黏合劑樹脂
黏合劑樹脂的實例可以包含聚醯亞胺樹脂、聚醯胺樹脂、苯氧基樹脂(phenoxy resin)、聚甲基丙烯酸酯樹脂、聚丙烯樹脂、聚氨基甲酸酯樹脂、聚酯樹脂、聚酯氨基甲酸酯樹脂、聚乙烯醇縮丁醛樹脂、苯乙烯-丁二烯-苯乙烯(styrene-butadiene-styrene，SBS)樹脂和其環氧化化合物、苯乙 烯-乙烯/丁烯-苯乙烯(styrene-ethylene/butylene-styrene，SEBS)樹脂和其經修飾的化合物、丙烯腈丁二烯橡膠(acrylonitrile butadiene rubber，NBR)和其氫化化合物以及其組合。具體地說，黏合劑樹脂可以是苯氧基樹脂，更尤其芴苯氧基樹脂。作為芴苯氧基樹脂(fluorene phenoxy resin)，可以使用(但不限於)含有芴結構的任何苯氧基樹脂。
就固體含量來說，按異方性導電膜組成物的總量計，黏合劑樹脂可以20重量%到60重量%的量存在。具體地說，就固體含量來說，按異方性導電膜組成物的總量計，黏合劑樹脂可以25重量%到40重量%，例如25重量%、26重量%、27重量%、28重量%、29重量%、30重量%、31重量%、32重量%、33重量%、34重量%、35重量%、36重量%、37重量%、38重量%、39重量%或40重量%的量存在。
脂環族環氧化合物
異方性導電膜組成物包含脂環族環氧化合物作為可固化化合物中的一種。因為脂環族環氧化合物具有存在於脂肪族環附近的環氧結構，所述脂環族環氧化合物允許快速開環反應並且因此展現比其它環氧化合物更好的固化反應性。作為脂環族環氧化合物，可以使用(但不限於)包含直接與脂肪族環偶合或經由另一連接位點與其偶合的環氧結構的任何脂環族環氧化合物。在一個實施例中，異方性導電膜組成物可以包含由式1到4表示的脂環族環氧化合物：
在式2到4中，n、s、t、u、v、m以及f可以各自獨立地為1到50的整數，並且R可以是烷基、乙醯基、烷氧基或羰基。更具體地說，n、s、t、u、v、m以及f可以各自獨立地為1到25的整數， 並且R可以是烷基、乙醯基或烷氧基。
在本發明的實施例中，脂環族環氧化合物可以單獨或以其組合形式使用。
氧雜環丁烷化合物
除脂環族環氧化合物以外，異方性導電膜組成物還包含氧雜環丁烷化合物作為可固化化合物。如本文所使用，氧雜環丁烷化合物是指含有氧雜環丁烷環的碳基化合物。歸因於氧雜環丁烷環的開環反應，氧雜環丁烷化合物具有良好的固化反應性。確切地說，每分子含有1到4個氧雜環丁烷環的氧雜環丁烷化合物可以用於抑制組成物在固化後裂化。具體地說，含有一個氧雜環丁烷環的氧雜環丁烷化合物可以由式5表示： 其中R1是氫原子；C1到C6烷基，如甲基、乙基、丙基以及丁基；C1到C6氟烷基；丙烯基(allyl group)；芳基；呋喃基或噻吩基。R2是C1到C6烷基，如甲基、乙基、丙基或丁基；C2到C6烯基(alkenyl)，如1-丙烯基、2-丙烯基、2-甲基-1-丙烯基、2-甲基-2-丙烯基、1-丁烯基、2-丁烯基或3-丁烯基；含有芳香族環的基團，如苯基、苄基(benzyl)、氟苄基、甲氧基苄基(methoxybenzyl)或苯氧基乙基(phenoxyethyl)；C2到C6烷基羰基(alkylcarbonyl)，如乙基羰基、丙基羰基或丁基羰基；C2到C6烷氧羰基 (alkoxycarbonyl)，如乙氧基羰基、丙氧基羰基或丁氧基羰基；或C2到C6 N-烷基氨甲醯基(N-alkylcarbamoyl group)，如乙基氨甲醯基(ethylcarbamoyl)、丙基氨甲醯基、丁基氨甲醯基或戊基氨甲醯基。
具體地說，含有兩個氧雜環丁烷環的氧雜環丁烷化合物可以由式6表示： 其中R1與式5中的R1相同。R3可以由以下中選出：直鏈或支鏈伸烷基(alkylene group)，如伸乙基、伸丙基或伸丁基；直鏈或支鏈聚(伸烷氧基)(poly(alkyleneoxy)group)；直鏈或支鏈不飽和烴基團，如伸丙烯基、甲基伸丙烯基或伸丁烯基；羰基；含有羰基的伸烷基；含有羧基的伸烷基；含有氨甲醯基的伸烷基；以及由式7到19表示的官能團中的任一個： 其中R4是氫原子；C1到C4烷基，如甲基、乙基、丙基或丁基；C1到C4烷氧基，如甲氧基、乙氧基、丙氧基或丁氧基；鹵素原子，如氯原子或溴原子；硝基；氰基；巰基；低級烷基羧基；羧基或氨甲醯基。
其中R5是氧原子、硫原子、亞甲基(methylene group)、胺基、磺醯基、雙(三氟甲基)亞甲基或二甲基亞甲基。
其中R6是氫原子；C1到C4烷基，如甲基、乙基、丙基或丁基；C1到C4烷氧基，如甲氧基、乙氧基、丙氧基或丁氧基；鹵素原子，如氯原子或溴原子；硝基；氰基；巰基；低級烷基羧基；羧基或氨甲醯基。
其中R7是氧原子、硫原子、亞甲基、胺基、磺醯基、雙(三氟甲基)亞甲基、二甲基亞甲基、苯基甲基亞甲基或二苯基亞甲基。
在式11和12中，R8是氫原子；C1到C4烷基，如甲基、乙基、丙基或丁基；C1到C4烷氧基，如甲氧基、乙氧基、丙氧基或丁氧基；鹵素原子，如氯原子或溴原子；硝基；氰基；巰基；低級烷基羧基；羧基或氨甲醯基。在一些實施例中，R8還可以包含2到4個在萘環中經取代的取代基。
其中n在0到10範圍內。
在一些實施例中，含有兩個氧雜環丁烷環的氧雜環丁烷化合物可以是由式19表示的化合物的混合物並且具有不同的n值。
除前述化合物以外，含有兩個氧雜環丁烷環的氧雜環丁烷化合物可以是由式20表示的化合物： 其中R1與式5中的R1相同。
具體地說，含有3到4個氧雜環丁烷環的氧雜環丁烷化合物可以是由式21表示的化合物： 其中R1與式5中的R1相同，並且m是3或4。R9可以是C1到C12支鏈伸烷基，如由式22、式23以及式24表示的基團；或由式25表示的支鏈聚(伸烷氧基)。
其中R10是低級烷基，如甲基、乙基或丙基。
其中n是1到10的整數。
在本發明的實施例中，可以單獨或以其組合形式使用上述氧雜環丁烷化合物。
包含脂環族環氧化合物和氧雜環丁烷化合物作為可固化化合物的異方性導電膜組成物由於化合物的高反應性可以在低溫下實現快速固化。在一些實施例中，就固體含量來說，按異方性導電膜組成物的總重量計，包含脂環族環氧化合物和氧雜環丁烷化合物的可固化化合物可以10重量%到40重量%，尤其15重量%到40重量%，例如15重量%、16重量%、17重量%、18重量%、19重量%、20重量%、21重量%、22重量%、23重量%、24重量%、25重量%、26重量%、27重量%、28重量%、29重量%、30重量%、31重量%、32重量%、33重量%、34重量%、35重量%、36重量%、37重量%、38重量%、39重量%或40重量%的量存在。另外，脂環族環氧化合物與氧雜環丁烷化合物的重量比可以在1：9到9：1範圍內。
其它可固化化合物
在一些實施例中，異方性導電膜組成物可以更包含額外可固化化合物以及脂環族環氧化合物和氧雜環丁烷化合物。額外可固化化合物可以包含至少一種由以下所構成的族群中選出的可固化化合物：含有環氧基的倍半矽氧烷(epoxy group-containing silsesquioxane)化合物、含有氧雜環丁烷基團的倍半矽氧烷化合物、苯酚酚醛環氧(phenol novolac epoxy)化合物以及甲酚酚醛環氧(cresol novolac epoxy)化合物。含有環氧基或氧雜環丁烷基 團的倍半矽氧烷化合物可以具有多面體寡聚倍半矽氧烷(polyhedral oligomeric silsesquioxane，POS)結構、無規結構、梯狀結構或部分籠狀結構。
當此類含有多官能基團的可固化化合物更包含於組成物中時，有可能改進粒子捕獲率，同時防止在高溫和高濕度下可靠性測試之後異方性導電膜的體積膨脹。
季銨催化劑
異方性導電膜組成物包含季銨催化劑。具體地說，作為季銨催化劑，可以使用由式26表示的化合物。
其中，R11、R12、R13以及R14各自獨立地為經取代或未經取代的C1到C6烷基和C6到C20芳基中的一個，並且M是Cl-、BF4 -、PF6 -、N(CF3SO2)2-、CH3CO2 -、CF3CO2 -、CF3SO3 -、HSO4 -、SO4 2-、SbF6 -以及B(C6F5)4 -中的一個。在式26中，例如由M的價數決定，季銨的許多部分可以被調整，以提供中性電荷(neutral charge)。
具體地說，R11、R12、R13以及R14可以各自獨立地為由以下中選出的一個：甲基、乙基、丙基、異丙基、丁基、異丁基、仲丁基、叔丁基、戊基、正戊基、叔戊基、異戊基、己基、環己基、苯基、蒽基(anthryl)以及菲基(phenanthryl)。如本文所使 用，術語“經取代的”意指化合物中的氫原子經由以下中選出的取代基取代：例如烷基、烷氧基、氨基、鹵素原子以及硝基。
季銨催化劑在特定溫度下促進脂環族環氧化合物的開環反應並且因此使得脂環族環氧化合物和氧雜環丁烷化合物在150℃或小於150℃的溫度下快速固化。此外，與一般用作陽離子催化劑的鋶基陽離子催化劑相比，季銨催化劑在小於固化溫度的溫度下，例如在室溫下展現較低反應性，並且因此可以延遲脂環族環氧化合物的開環反應，從而提供極佳儲存穩定性。
具體地說，在式26中，M可以是SbF6 -和B(C6F5)4 -中的一個。更具體地說，M可以是B(C6F5)4 -，其對於生態環較友善。
當季銨化合物催化劑與脂環族環氧化合物和氧雜環丁烷化合物一起使用時，有可能減小異方性導電膜組成物的放熱起始溫度與放熱峰值溫度之間的溫度差，以差示掃描量熱法(DSC)所測量，從而使得組成物快速固化。
就固體含量來說，按異方性導電膜組成物的總重量計，季銨催化劑可以1重量%到10重量%，例如1重量%、2重量%、3重量%、4重量%、5重量%、6重量%、7重量%、8重量%、9重量%或10重量%的量存在。
穩定劑
在一些實施例中，異方性導電膜組成物可以包含穩定劑以調節組成物的固化溫度。穩定劑用以延遲脂環族環氧化合物的開環反應，從而調節固化溫度。
在一個實施例中，由式27表示的化合物可以用作穩定劑： 其中R15到R19各自獨立地為氫原子、烷基、乙醯基、烷氧基羰基、苯甲醯基或苄氧羰基(benzyloxycarbonyl)，R20和R21各自獨立地為烷基、苄基、鄰甲基苄基、間甲基苄基、對甲基苄基或萘甲基(naphthylmethyl)，並且X1是烷基硫酸。
在本發明的實施例中，可以使用少量穩定劑，因為穩定劑僅用於微調固化溫度。舉例來說，按季銨催化劑的重量計，穩定劑可以小於5重量%，尤其超過0重量%到小於5重量%，例如1重量%、2重量%、3重量%、4重量%的量包含於異方性導電膜組成物中。
導電粒子
導電粒子不受特定限制並且可以由所屬領域中使用的典型導電粒子中選出。導電粒子的實例可以包含：包含Au、Ag、Ni、Cu的金屬粒子和焊料；碳粒子；通過塗布聚合樹脂粒子獲得的粒子，如聚乙烯、聚丙烯、聚酯、聚苯乙烯、聚乙烯醇以及其經修飾的樹脂，其中金屬包含Au、Ag、Ni等；以及經由通過用金屬塗布聚合樹脂粒子獲得的粒子表面的絕緣處理獲得的絕緣粒子。導電粒子可以具有例如1微米到20微米，尤其1微米到10微米， 例如1微米、2微米、3微米、4微米、5微米、6微米、7微米、8微米、9微米或10微米的粒子大小，取決於電路間距。
在一個實施例中，就固體含量來說，按異方性導電膜的總重量計，導電粒子可以1重量%到20重量%的量存在。
當異方性導電膜具有導電層和介電層的雙層結構並且用於玻璃基板與IC之間的連接時，就固體含量來說，按導電層的重量計，導電粒子可以10重量%到50重量%，尤其15重量%到35重量%，例如15重量%、16重量%、17重量%、18重量%、19重量%、20重量%、21重量%、22重量%、23重量%、24重量%、25重量%、26重量%、27重量%、28重量%、29重量%、30重量%、31重量%、32重量%、33重量%、34重量%或35重量%的量存在，但導電粒子的量可以取決於待連接電路的電極區域和電極上粒子的所需數目變化。在此範圍內，可以易於在端線之間壓縮導電粒子以保持穩定連接可靠性，同時經由提高導電性來減小連接電阻。
無機填充劑
異方性導電膜組成物中包含的無機填充劑不受特定限制並且可以由所屬領域中使用的典型無機填充劑中選出。無機填充劑的實例可以包含(但不限於)氧化鋁、二氧化矽、二氧化鈦、氧化鋯、氧化鎂、氧化鈰、氧化鋅、氧化鐵、氮化矽、氮化鈦、氮化硼、碳酸鈣、硫酸鋁、氫氧化鋁、鈦酸鈣、滑石、矽酸鈣以及矽酸鎂。具體地說，無機填充劑可以是氧化鋁、二氧化矽、碳 酸鈣或氫氧化鋁。在一個實施例中，無機填充劑可以是氫氧化鋁或二氧化矽。確切地說，氫氧化鋁可以改進異方性導電膜組成物的可塗布性，調節異方性導電膜組成物的流動性，以及防止黏附體的腐蝕。
就固體含量來說，按異方性導電膜組成物的總重量計，無機填充劑可以5重量%到30重量%，例如5重量%、6重量%、7重量%、8重量%、9重量%、10重量%、11重量%、12重量%、13重量%、14重量%、15重量%、16重量%、17重量%、18重量%、19重量%、20重量%、21重量%、22重量%、23重量%、24重量%、25重量%、26重量%、27重量%、28重量%、29重量%或30重量%的量存在。在此範圍內，無機填充劑可以有效地分散導電粒子並且可以適當地調節異方性導電膜的流動性。
其它添加劑
在一個實施例中，異方性導電膜組成物可以更包含矽烷偶合劑。矽烷偶合劑可以包含(但不限於)至少一種由以下所構成的族群中選出的物質：例如可聚合含有氟基的矽化合物，如乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷以及(甲基)丙烯醯氧基丙基三甲氧基矽烷；含有環氧基的矽化合物，如3-縮水甘油氧基丙基三甲氧基矽烷、3-縮水甘油氧基丙基甲基二甲氧基矽烷以及2-(3,4-環氧環己基)-乙基三甲氧基矽烷；含有氨基的矽化合物，如3-氨基丙基三甲氧基矽烷、N-(2-氨基乙基)-3-氨基丙基三甲氧基矽烷以及N-(2-氨基乙基)-3-氨基丙基甲基二甲氧基矽烷；以及3-氯 丙基三甲氧基矽烷。
就固體含量來說，按異方性導電膜組成物的總重量計，矽烷偶合劑可以0重量%到10重量%，例如1重量%、2重量%、3重量%、4重量%、5重量%、6重量%、7重量%、8重量%、9重量%或10重量%的量存在。
異方性導電膜組成物可以更包含添加劑，如聚合抑制劑、抗氧化劑以及熱穩定劑以提供額外特性，而不影響其基本特性。就固體含量來說，按異方性導電膜組成物的總重量計，添加劑可以0.01重量%到2重量%，例如0.01重量%、0.05重量%、0.1重量%、0.5重量%、1.5重量%或2重量%的量存在。
聚合抑制劑的實例可以包含(但不限於)氫醌、氫醌單甲醚、對苯醌、吩噻嗪以及其混合物。抗氧化劑可以是酚類或羥基肉桂酸酯抗氧化劑。具體地說，抗氧化劑可以包含四[亞甲基(3,5-二-叔丁基-4-羥基肉桂酸酯)]甲烷、3,5-雙(1,1-二甲基乙基)-4-羥基苯丙酸硫代二-2,1-乙烷二基酯等。
本發明的另一種態樣是有關於一種異方性導電膜，包含：黏合劑樹脂；包含脂環族環氧化合物和氧雜環丁烷化合物的可固化化合物；季銨催化劑；以及導電粒子，並且熱量變化率為15%或小於15%，以差示掃描量熱法(DSC)所測量和方程式1所計算：熱量變化率(%)=[(H0-H1)/H0]×100---(1)，其中H0是異方性導電膜的DSC熱量，如緊接在其製造之後所測量，例如， 如在25℃下和0小時的時間點所測量，並且H1是異方性導電膜的DSC熱量，如在40℃下靜置24小時之後所測量。
因為黏合劑樹脂、包含脂環族環氧化合物和氧雜環丁烷化合物的可固化化合物以及季銨催化劑的細節與異方性導電膜組成物所述者相同，所以將省略其描述。
在一些實施例中，異方性導電膜可以更包含導電粒子、額外可固化化合物等。因為其細節與異方性導電膜組成物所述者相同，所以將省略其描述。
在一個實施例中，異方性導電膜可以更包含穩定劑。穩定劑與異方性導電膜組成物的穩定劑相同。就固體含量來說，按異方性導電膜的總重量計，穩定劑可以超過0重量%到小於5重量%，例如1重量%、2重量%、3重量%、4重量%的量存在。
熱量變化率
根據本發明的異方性導電膜可以具有15%或小於15%，尤其10%或小於10%的熱量變化率，如通過方程式1所計算：熱量變化率(%)=[(H0-H1)/H0]×100---(1)，其中H0是異方性導電膜的DSC熱量，如在25℃下和0小時的時間點所測量，並且H1是異方性導電膜的DSC熱量，如在40℃下靜置24小時之後所測量。
異方性導電膜的DSC熱量可以通過所屬領域中使用的任何典型方法測量。舉例來說，異方性導電膜的DSC熱量可以取決於溫度，根據異方性導電膜的卡路里計算，如在-50℃到250℃的 溫度範圍內，以10℃/分鐘的加熱速率，在氮氣氛圍下使用DSC(差示掃描量熱法計)(Q20，TA儀器)加熱所述異方性導電膜時所測量。在熱量變化率的上述範圍內，異方性導電膜具有良好儲存穩定性。
DSC放熱起始溫度和DSC放熱峰值溫度
根據本發明的異方性導電膜可以具有70℃到85℃的DSC放熱起始溫度和90℃到110℃的放熱峰值溫度。
在DSC圖上，DSC放熱起始溫度定義為熱量產生起始點與熱量產生結束點之間的基線與最高峰的切線相接時到DSC圖斜率由於DSC測量後熱量產生而開始增加時的溫度。DSC放熱峰值溫度定義為熱量的最高峰所處的溫度。
舉例來說，DSC放熱起始溫度和DSC放熱峰值溫度可以經由在-50℃到250℃的溫度範圍內，以10℃/分鐘的加熱速率，在氮氣氛圍下使用DSC(差示掃描量熱法計)(Q20，TA儀器)加熱異方性導電膜組成物的方法所測量。
在DSC放熱起始溫度和DSC放熱峰值溫度的上述範圍內，異方性導電膜可以在150℃或小於150℃，例如130℃到150℃的相對較低溫度下固化，並且可以歸因於DSC放熱起始溫度與DSC放熱峰值溫度之間的較小差值而快速固化。
可靠性後連接電阻(T1)
異方性導電膜可以具有0.5歐姆或小於0.5歐姆的可靠性後連接電阻，如在50℃到90℃的溫度下，在0.5兆帕到2兆帕的 壓力下初步壓縮0.5到2秒並且在100℃到150℃的溫度下，在50兆帕到90兆帕的壓力下主要壓縮4到7秒，繼而使異方性導電膜在85℃和85% RH下靜置500小時之後所測量。
在可靠性測試後連接電阻的此範圍內，異方性導電膜可以在連接可靠性和長期儲存穩定性方面展現改進的特性。
可靠性測試之後的連接電阻可以通過(但不限於)以下示例性方法測量。在此方法中，首先，將異方性導電膜放置在包含凸起面積為1,200平方微米並且厚度為2,000埃的氧化銦錫(indium tin oxide,ITO)電路的玻璃基板上，繼而在50℃到90℃的溫度下，在0.5兆帕到2兆帕的壓力下初步壓縮0.5到2秒，並且在去除離型膜之後，將凸起面積為1,200平方微米並且厚度為1.5T的IC晶片放置在異方性導電膜上，繼而在100℃到150℃的溫度下，在50兆帕到90兆帕的壓力下主要壓縮4到7秒，從而製備樣本。接著，通過4點探針方法，使用電阻計(2000萬用表(Multimeter)，吉時利儀器(Keithley Instruments))測量所製備樣本的4點之間的電阻值，從而發現初始連接電阻T0。接著，將樣本在85℃和85% RH下靜置500小時，繼而以相同方式測量電阻，從而發現可靠性測試後的連接電阻T1。此處，基於在通過電阻計施加1毫安培電流後所測量到的電壓計算電阻值，並且取平均值。
製造異方性導電膜的方法
製造異方性導電膜的方法不需要任何特定裝置或設備。 舉例來說，使包含如上文所闡述的組分的異方性導電膜組成物溶解於如甲苯的有機溶劑中，繼而以不會導致導電粒子粉碎的攪拌速度攪拌一定時間段。接著，將所得材料塗布到離型膜上，達到例如10微米到50微米的厚度，並且乾燥一定時間段以使甲苯等揮發，從而獲得異方性導電膜。
本發明的另一種態樣是有關於一種連接結構，包含：第一連接構件，包含第一電極；第二連接構件，包含第二電極；以及異方性導電膜，配置於第一連接構件與第二連接構件之間以將第一電極連接到第二電極，其中異方性導電膜可以是根據本發明的實施例的異方性導電膜。
第一連接構件或第二連接構件包含用於電連接的電極。具體地說，第一連接構件或第二連接構件可以是玻璃或塑膠基板、印刷線路板、陶瓷線路板、柔性線路板、半導體矽晶片、積體電路(integrated circuit，IC)晶片或驅動器IC晶片，對於LCD，其用氧化銦錫(indium tin oxide，ITO)或氧化銦鋅(indium zinc oxide，IZO)電極形成。更具體地說，第一連接構件和第二連接構件中的一個可以是IC晶片或驅動器IC晶片，並且另一個可以是玻璃基板。
參看圖1，根據本發明的一個實施例的連接結構30包含：第一連接構件50，包含第一電極70；以及第二連接構件60，包含第二電極80，其中第一連接構件和第二連接構件可以經由異方性導電膜10彼此連接，所述異方性導電膜10配置於第一連接 構件50與第二連接構件60之間並且包含將第一電極70連接到第二電極80的導電粒子3，以將第一電極70連接到第二電極80，其中所述異方性導電膜10可以是如上文所闡述的異方性導電膜10。
隨後，將詳細描述本發明的實例以及比較例。然而，應理解，本發明不限於以下實例。
為清楚起見，將省略對所屬領域的技術人員顯而易知的細節描述。
雖然實例和比較例中製造的異方性導電薄膜中的每一個是用於將玻璃基板連接到典型的顯示器面板的IC的異方性導電膜並且具有含有導電粒子的導電層和介電層的雙層結構，但應理解，本發明不限於此並且異方性導電膜可以具有不同的層結構。
實例
實例1
-含有導電粒子的導電層
通過混合30重量%聯二苯芴苯氧基樹脂(FX-293，日本鋼鐵公司(Nippon Steel Corporation))、22.5重量%脂環族環氧化合物(Celloxide 2021P，大賽璐(DAICEL))、2.5重量%氧雜環丁烷化合物(OXT-221，東亞合成(TOAGOSEI))、5重量%季銨催化劑(CXC-1612，國王企業(KING INDUSTRY))、3重量%矽烷化合物(KBM-403，信越(SHINETSU))、2重量%氫氧化鋁(Al(OH)2)(奧德里奇化學公司(ALDRICH CHEMICALS))、10 重量%球狀二氧化矽(Sciqas，酒井(SAKAI)，平均粒子直徑：0.4微米)以及25重量%經過絕緣處理的導電粒子(N2EJB，平均粒子直徑：3微米，日本積水株式會社(Sekisui Co.,Ltd.,Japan))製備導電層組成物。
將導電層組成物塗布到離型膜上並且在60℃下在乾燥器中乾燥5分鐘以使溶劑揮發，從而獲得6微米厚的導電層。
-不含有導電粒子的介電層
除了不使用導電粒子以外，以與實例1相同的方式製備介電層組成物。將介電層組成物塗布到離型膜上並且在60℃下在乾燥器中乾燥5分鐘以使溶劑揮發，從而獲得12微米厚的介電層。
在40℃的溫度下，在1兆帕的壓力下，將導電膜層壓在介電層上，從而獲得具有雙層結構的異方性導電膜(厚度：18微米)，其中介電層堆疊在導電層上。
在實例2到7和比較例1到4中，以與實例1類似的方式製備具有雙層結構的異方性導電膜(厚度：18微米)，其中介電層堆疊在導電層上。在實例和比較例中的每一個中，使用除了不包含導電粒子以外與導電層組成物相同的組成物製備介電層。因此，在實例2到7和比較例1到4中，在下文中僅將描述含有導電粒子的導電層組成物之間的差異。
實例2到5
除了以總計25重量%的量使用脂環族環氧化合物(Celloxide 2021P，大賽璐)和氧雜環丁烷化合物(OXT-221，東 亞合成)並且分別將脂環族環氧化合物與氧雜環丁烷化合物的重量比(在實例1中為9：1)改變為7：3(實例2)、5：5(實例3)、3：7(實例4)以及1：9(實例5)以外，以與實例1相同的方式製備異方性導電膜組成物，並且使用各別異方性導電膜組成物獲得異方性導電膜。
實例6
除了將脂環族環氧化合物(Celloxide 2021P，大賽璐)和氧雜環丁烷化合物(OXT-221，東亞合成)的量分別改變為7.5重量%和7.5重量%並且使用10重量%苯酚酚醛環氧化合物(YDPN638，國都化工(KUKDO Chemical))以外，以與實例1相同的方式製備異方性導電膜組成物，並且使用異方性導電膜組成物獲得異方性導電膜。
實例7
除了將季銨催化劑(CXC-1612，國王工業)的量改變為4.8重量%並且使用0.2重量%由式27-1表示的化合物(SI-S，日本三信化工株式會社(Sanshin Chemical Industry Co.,Ltd.,Japan))作為穩定劑以外，以與實例1相同的方式製備異方性導電膜組成物，並且使用異方性導電膜組成物獲得異方性導電膜。
比較例1
除了使用鋶陽離子催化劑(San-aid SI-60L，日本三信化工株式會社)替代季銨催化劑以外，以與實例3相同的方式製備異方性導電膜組成物，並且使用異方性導電膜組成物獲得異方性導電膜。
比較例2
除了使用鋶陽離子催化劑(San-aid SI-60L，日本三信化工株式會社)替代季銨催化劑以外，以與實例6相同的方式製備異方性導電膜組成物，並且使用異方性導電膜組成物獲得異方性導電膜。
比較例3
除了不使用氧雜環丁烷化合物並且單獨使用25重量%脂環族環氧化合物(Celloxide 2021P，大賽璐)作為可固化化合物以外，以與實例3相同的方式製備異方性導電膜組成物，並且使用異方性導電膜組成物獲得異方性導電膜。
比較例4
除了不使用脂環族環氧化合物並且單獨使用25重量%氧雜環丁烷化合物(OXT-221，東亞合成)作為可固化化合物以外，以與實例3相同的方式製備異方性導電膜組成物，並且使用異方性導電膜組成物獲得異方性導電膜。
表1中示出了實例和比較例中使用的組分中的每一個的細節。
實驗實例1：計算異方性導電膜的DSC熱量變化率
以1毫克的量對實例1到6和比較例1到4中製備的異方性導電膜中的每一個進行取樣，通過測量異方性導電膜樣品的卡路里，同時在-50℃到250℃的溫度範圍內，以10℃/分鐘的加熱速率，在氮氣氛圍下使用DSC(差示掃描量熱計)(Q20，TA儀器)加熱樣品發現樣品的初始熱量(H0)和在40℃下靜置24小時之後的熱量(H1)，繼而根據方程式1計算異方性導電膜的熱量變化率：熱量變化率(%)=[(H0-H1)/H0]×100---(1)
實驗實例2：在DSC上測量放熱起始溫度和放熱峰值溫 度
使用差示掃描量熱計(DSC)(Q20，TA儀器)，同時在-50℃到250℃的溫度範圍內，以10℃/分鐘的加熱速率，在氮氣氛圍下加熱異方性導電膜，測量實例1到6和比較例1到4中製備的異方性導電膜中的每一個的DSC放熱起始溫度和放熱峰值溫度。在DSC圖上，DSC放熱起始溫度定義為熱量產生起始點與熱量產生結束點之間的基線與最高峰的切線相接時到DSC圖斜率由於DSC測量後熱量產生而開始增加時的溫度。DSC放熱峰值溫度定義為DSC圖上熱量的最高峰所處的溫度。
實驗實例3：測量初始凹痕均一性和可靠性後凹痕均一性
將實例和比較例中製備的異方性導電膜中的每一個放置在包含凸起面積為1,200平方微米並且厚度為2,000埃的ITO電路的玻璃基板(紐維科隆公司(Neoview Kolon,Inc.))上並且在70℃下在1兆帕下進行初步壓縮1秒。接著，在去除離型膜之後，將凸起面積為1,200平方微米並且厚度為1.5T(三星(Samsung)LSI)的IC晶片放置在異方性導電膜上，繼而在130℃下在70兆帕下主要壓縮5秒。接著，肉眼觀測到凹痕的均一性。
另外，在85℃和85% RH下，將樣本在高溫和高濕度箱中靜置500小時，繼而肉眼觀測凹痕均一性以評估可靠性。
具體地說，檢查IC晶片的兩個側面的凹痕是否與其中心區域中的凹痕一樣清晰。當凹痕為均一的並且第一行輸出端線上的凹痕與第二行輸出端線上的凹痕一樣清晰時，此結果得分為5， 並且當相比於其中心區域中的凹痕，IC晶片的兩個側面處的凹痕極不清楚或不可識別時，此結果得分為0。每個標準以0到5進行評分。
實驗實例4：測量初始連接電阻和可靠性後連接電阻
將實例和比較例中製備的異方性導電膜中的每一個放置在包含凸起面積為1,200平方微米並且厚度為2,000埃的ITO電路的玻璃基板上並且在70℃和1.0兆帕下進行初步壓縮1秒。接著，在去除離型膜之後，將凸起面積為1,200平方微米並且高度為15微米的IC晶片放置在異方性導電膜上，繼而在130℃下在70兆帕下主要壓縮5秒，從而製備5個樣本。
通過4點探針方法，使用具有4個探針的電阻計測量所製備樣本中的每一個的4點之間的電阻值。此處，基於在通過電阻計施加1毫安培電流後所測量到的電壓計算電阻值，並且取平均值。
首先，測量樣本的初始連接(T0)電阻。
接著，在85℃和85% RH下，將樣本放置于高溫和高濕度箱中500小時，繼而以相同方式測量電阻，從而發現可靠性測試之後的連接電阻(T1)。
實驗實例1到4的結果顯示於表2中。
表2
如表2中所示，可見包含脂環族環氧化合物和氧雜環丁烷化合物以及季銨催化劑的實例1到6的異方性導電膜具有低熱量變化率和因此高儲存穩定性，展現低DSC放熱起始溫度和低DSC放熱峰值溫度，並且提供其間相對較小的差異，從而在低溫下實現快速固化。另外，在可靠性測試之後，實例1到6的異方性導電膜在凹痕和連接電阻方面展現良好特性。
以上概述了多個實施例的特徵，使本領域具有通常知識者可更佳了解本發明的態樣。本領域具有通常知識者應理解，其可輕易地使用本發明作為設計或修改其他製程與結構的依據，以實行本文所介紹的實施例的相同目的及/或達到相同優點。本領域具有通常知識者還應理解，這種等效的配置並不悖離本發明的精神與範疇，且本領域具有通常知識者在不悖離本發明的精神與範疇的情況下可對本文做出各種改變、置換以及變更。

Claims (12)

  1. 一種異方性導電膜，包括：就固體含量來說，按所述異方性導電膜的總重量計，20重量%到60重量%的黏合劑樹脂；10重量%到40重量%的包括脂環族環氧化合物以及氧雜環丁烷化合物的可固化化合物，其中所述脂環族環氧化合物與所述氧雜環丁烷化合物的重量比在1：9到9：1範圍間；1重量%到10重量%的季銨催化劑；5重量%到30重量%的無機填充劑；以及1重量%到20重量%的導電粒子，所述導電粒子具有1微米到20微米的粒子大小，所述異方性導電膜具有15%或小於15%的熱量變化率，以差示掃描量熱法所測量以及方程式1所計算：熱量變化率(%)=[(H0-H1)/H0]×100---(1)，其中H0是所述異方性導電膜以差示掃描量熱法測定的熱量，在25℃下以及0小時的時間點所測量，以及H1是所述異方性導電膜以差示掃描量熱法測定的熱量，在40℃下靜置24小時後所測量，其中所述異方性導電膜具有70℃到85℃的差示掃描量熱法放熱起始溫度以及90℃到110℃的差示掃描量熱法放熱峰值溫度。
  2. 如申請專利範圍第1項所述的異方性導電膜，其中所述脂環族環氧化合物是由式1表示的脂環族環氧化合物：[式1]
  3. 如申請專利範圍第1項所述的異方性導電膜，其中所述氧雜環丁烷化合物是每分子含有1到4個氧雜環丁烷環的碳聚合物化合物。
  4. 如申請專利範圍第1項所述的異方性導電膜，其中所述季銨催化劑由式2表示：其中R11、R12、R13以及R14各自獨立地為經取代或未經取代的C1到C6烷基以及C6到C20芳基中的一個，以及M是Cl-、BF4 -、PF6 -、N(CF3SO2)2-、CH3CO2 -、CF3CO2 -、CF3SO3 -、HSO4 -、SO4 2-、SbF6 -以及B(C6F5)4 -中的一個。
  5. 如申請專利範圍第1項所述的異方性導電膜，其中所述黏合劑樹脂是聚醯亞胺樹脂、聚醯胺樹脂、苯氧基樹脂、聚甲基丙烯酸酯樹脂、聚丙烯樹脂、聚氨基甲酸酯樹脂、聚酯樹脂、聚酯氨基甲酸酯樹脂、聚乙烯醇縮丁醛樹脂、苯乙烯-丁二烯-苯乙烯樹脂以及其環氧化化合物、苯乙烯-乙烯/丁烯-苯乙烯樹脂以及其經修飾的化合物、丙烯腈丁二烯橡膠以及其氫化化合物或者其組合。
  6. 如申請專利範圍第5項所述的異方性導電膜，其中所述苯氧基樹脂是芴苯氧基樹脂。
  7. 如申請專利範圍第1項所述的異方性導電膜，所述無機填充劑包含由下列所選出的至少一種：氧化鋁、二氧化矽、二氧化鈦、氧化鋯、氧化鎂、氧化鈰、氧化鋅、氧化鐵、氮化矽、氮化鈦、氮化硼、碳酸鈣、硫酸鋁、氫氧化鋁、鈦酸鈣、滑石、矽酸鈣以及矽酸鎂。
  8. 如申請專利範圍第1項所述的異方性導電膜，更包括：就固體含量來說，按所述異方性導電膜的總重量計，超過0重量%到小於5重量%的量的穩定劑。
  9. 如申請專利範圍第1項所述的異方性導電膜，更包括至少一種可固化化合物由以下所構成的族群中選出的：含有環氧基的倍半矽氧烷化合物、含有氧雜環丁烷基團的倍半矽氧烷化合物、苯酚酚醛環氧化合物以及甲酚酚醛環氧化合物。
  10. 如申請專利範圍第1項所述的異方性導電膜，其中所述異方性導電膜具有0.5歐姆或小於0.5歐姆的可靠性後連接電阻，如在50℃到90℃的溫度下，在0.5兆帕到2兆帕的壓力下初步壓縮0.5到2秒，以及在100℃到150℃的溫度下，在50兆帕到90兆帕的壓力下主要壓縮4到7秒，繼而使所述異方性導電膜在85℃以及85% RH下靜置500小時之後所測量。
  11. 一種異方性導電膜組成物，包括：就固體含量來說，按所述異方性導電膜組成物的總重量計，20重量%到60重量%黏合劑樹脂；10重量%到40重量%的包括脂環族環氧化合物以及氧雜環丁烷化合物的可固化化合物，其中所述脂環族環氧化合物與所述氧雜環丁烷化合物的重量比在1：9到9：1範圍間；1重量%到10重量%的季銨催化劑；5重量%到30重量%的無機填充劑；以及1重量%到20重量%的導電粒子，所述導電粒子具有1微米到20微米的粒子大小，其中所述異方性導電膜組成物具有70℃到85℃的差示掃描量熱法放熱起始溫度以及90℃到110℃的差示掃描量熱法放熱峰值溫度。
  12. 一種連接結構，包括：第一連接構件，包括第一電極；第二連接構件，包括第二電極；以及異方性導電膜，配置於所述第一連接構件與所述第二連接構件之間以將所述第一電極連接到所述第二電極，其中所述異方性導電膜是根據申請專利範圍第1項所述的異方性導電膜或使用根據申請專利範圍第11項所述的異方性導電膜組成物製備的異方性導電膜。
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