CN103965793A - 各向异性导电膜和半导体装置 - Google Patents

各向异性导电膜和半导体装置 Download PDF

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Publication number
CN103965793A
CN103965793A CN201410037692.7A CN201410037692A CN103965793A CN 103965793 A CN103965793 A CN 103965793A CN 201410037692 A CN201410037692 A CN 201410037692A CN 103965793 A CN103965793 A CN 103965793A
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conductive film
anisotropic conductive
methyl
radical polymerization
condensation material
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CN201410037692.7A
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CN103965793B (zh
Inventor
高连助
奇惠秀
金二柱
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Guo Dujianduansucai
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Cheil Industries Inc
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B60—VEHICLES IN GENERAL
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    • B60N2/26—Seats specially adapted for vehicles; Arrangement or mounting of seats in vehicles for particular purposes or particular vehicles for children
    • B60N2/28—Seats readily mountable on, and dismountable from, existing seats or other parts of the vehicle
    • B60N2/2803—Adaptations for seat belts
    • B60N2/2806—Adaptations for seat belts for securing the child seat to the vehicle
    • B60N2/2809—Adaptations for seat belts for securing the child seat to the vehicle with additional tether connected to the top of the child seat and passing above the top of the back-rest
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Abstract

此处公开了各向异性导电膜和包括它的半导体装置，所述各向异性导电膜使用至少两种类型的自由基聚合材料制备以提供低透湿性和低吸湿性同时呈现优异的长期可靠性，所述至少两种类型的自由基聚合材料在其结构中具有不同数量的反应基团。具体地，使用自由基聚合材料制备各向异性导电膜以改善长期可靠性，所述自由基聚合材料包括具有一个或两个(甲基)丙烯酸酯反应基团的材料和具有至少三个(甲基)丙烯酸酯反应基团的材料。

Description

各向异性导电膜和半导体装置
技术领域
本发明涉及具有低透湿性和吸湿性同时呈现优异的长期可靠性的各向异性导电膜，以及使用所述各向异性导电膜连接的半导体装置。
背景技术
通常，各向异性导电膜(ACF)是指膜形粘合剂,其中诸如金属微粒(包括镍或金微粒)或金属涂覆的聚合物微粒的导电微粒分散在诸如环氧树脂的树脂中。各向异性导电膜由具有电各向异性和粘合性的聚合物层形成，并在膜的厚度方向呈现导电性能且在其表面方向呈现绝缘性能。
当各向异性导电膜被置于电路板之间并且在特定条件下经受加热和压制时，电路板的电路端子通过导电微粒电连接，并且绝缘粘合剂树脂填充相邻电路端子之间的空间以使导电微粒彼此分离，从而在电路端子之间提供高绝缘性。
对具有优异的长期可靠性的各向异性导电膜的需要日益增加，该各向异性导电膜可克服由于在产品使用中的连续电流和暴露于高温和高湿条件下所造成的问题。特别地，随着近来轻薄短小的IT装置的开发和平板显示器分辨率的增加，在相关领域中装置的电路宽度逐渐变窄，并且因此被置于电极之间以使电路连接的导电颗粒的数量下降，从而增加长期可靠性的重要性。
为了增强包括在各向异性导电膜中以连接电路元件的各向异性导电膜的长期可靠性，已在相关领域中研究无机颗粒的用途(韩国专利10-0652915等)。当将其加入用于各向异性导电膜的组合物时，无机颗粒可降低膜的透湿性和吸湿性。但是，无机颗粒劣化各向异性导电膜的固有粘合性，导致在膜与基板之间的界面处产生严重鼓泡，从而劣化长期可靠性。
因此，需要这样一种各向异性导电膜，其中通过调节膜的透湿性和吸湿性但不劣化各向异性导电膜的粘合性而使其具有优异的长期可靠性。
发明内容
本发明的目的是提供各向异性导电膜，所述各向异性导电膜使用至少两种类型的自由基聚合材料制备，以提供低透湿性和低吸湿性同时呈现优异的长期可靠性，所述自由基聚合材料在其结构中具有不同数量的反应基团。
具体地，本发明的目的在于提供各向异性导电膜，所述各向异性导电膜使用自由基聚合材料制备以提高长期可靠性，所述自由基聚合材料包括在其结构中具有一个或两个(甲基)丙烯酸酯反应基团的材料和在其结构中具有至少三个(甲基)丙烯酸酯反应基团的材料。
本发明提供各向异性导电膜，所述各向异性导电膜使用至少两种类型的自由基聚合材料制备以提供低透湿性和低吸湿性同时呈现优异的长期可靠性，所述至少两种类型的自由基聚合材料在其结构中具有不同数量的反应基团。
根据本发明的一个方面，各向异性导电膜包括：(a)粘结剂树脂；(b)第一自由基聚合材料和第二自由基聚合材料，所述第一自由基聚合材料在其结构中具有一个或两个(甲基)丙烯酸酯反应基团，所述第二自由基聚合材料在其结构中具有至少三个(甲基)丙烯酸酯反应基团；和(c)导电颗粒，其中所述膜具有170g/m2/24小时以下的透湿性或者2%以下的吸湿性。
根据本发明的实施方式的各向异性导电膜具有低透湿性和低吸湿性，并且因此，即使在高温和/或高湿的条件下使用较长一段时间后，在可靠性连接电阻、可靠性粘合强度或可靠性鼓泡性能的方面也呈现优异的可靠性。
作为电路的元件，由于所述各向异性导电膜的优异性能，因此使用所述各向异性导电膜制备的半导体装置而在较长一段时间内提供半导体效应。
附图说明
图1是半导体装置的截面图，包括具有第一电极70的第一连接元件50和具有第二电极80的第二连接元件60，其中第一连接元件50和第二连接元件60根据本发明的一个实施方式经由各向异性导电膜10彼此连接。当在包括第一电极70的第一连接元件50和包括第二电极80的第二连接元件60之间压制各向异性导电膜10时，第一电极70经由导电颗粒40电连接至第二电极80。
具体实施方式
此后，将更详细地描述本发明的实施方式。为清楚起见将省略对本领域技术人员显而易见的详情的描述。
本发明提供各向异性导电膜，所述各向异性导电膜使用至少两种类型的自由基聚合材料制备以提供低透湿性和低吸湿性同时呈现优异的长期可靠性，所述两种类型的自由基聚合材料在其结构中具有不同数量的反应基团。
根据本发明的一个实施方式，各向异性导电膜包括：(a)粘结剂树脂；(b)第一自由基聚合材料和第二自由基聚合材料，所述第一自由基聚合材料在其结构中具有一个或两个(甲基)丙烯酸酯反应基团，所述第二自由基聚合材料在其结构中具有至少三个(甲基)丙烯酸酯反应基团；和(c)导电颗粒，其中所述膜具有170g/m2/24小时以下的透湿性和2%以下的吸湿性。
接下来，将更详细地描述根据本发明的实施方式的各向异性导电膜的各组分。此处，每种组分的含量是基于各向异性导电膜组合物的总重量。此外，在制备各向异性导电膜时，将每种组分溶解于有机溶剂中并沉积在离型膜上，随后以预定时间干燥以使有机溶剂蒸发。因此，固体各向异性导电膜也可含有各向异性导电膜组合物的各组分。
(a)粘结剂树脂
在本发明中，可不加限制地使用通常用于本领域中的任何粘结剂树脂。
粘结剂树脂的实例可包括丙烯腈-丁二烯橡胶(NBR)树脂、聚氨酯树脂、丙烯酸树脂、聚酯聚氨酯树脂等。
此处，丙烯腈-丁二烯橡胶树脂是指通过丙烯腈和丁二烯的乳液聚合而制备的共聚物。在该共聚物中，丙烯腈和丁二烯的含量无具体限制，并且可不加限制地使用任何聚合方法。丙烯腈-丁二烯橡胶树脂可具有50,000g/mol至1,000,000g/mol的重均分子量，而不限于此。
此处，聚氨酯树脂是指具有氨基甲酸酯键的聚合物树脂，并且可通过例如异佛尔酮二异氰酸酯、聚丁二醇等的聚合制备，而不限于此。聚氨酯树脂可具有10,000g/mol至200,000g/mol的重均分子量，而不限于此。
此处，丙烯酸树脂可通过丙烯酰基单体和/或可与其聚合的其它单体的聚合而制备。例如，丙烯酸树脂可通过至少一种选自由含C2至C10烷基的(甲基)丙烯酸酯、(甲基)丙烯酸、乙酸乙烯酯和由其修饰的丙烯酸单体组成的组中的单体的聚合而制备。可不加限制地使用任何聚合方法。丙烯酸树脂可具有10,000g/mol至200,000g/mol的重均分子量，而不限于此。
如此处所用，聚酯聚氨酯树脂可以是通过聚酯多元醇和二异氰酸酯的反应而制备的树脂。
聚酯多元醇是指具有多个酯基和多个羟基的聚合物。聚酯多元醇可通过二羧酸和二醇的缩合而获得。
二羧酸的实例可包括脂族或芳族二羧酸，例如邻苯二甲酸、对苯二甲酸、间苯二甲酸、己二酸、癸二酸、琥珀酸、戊二酸、辛二酸、壬二酸、十二烷二羧酸、六氢苯二甲酸、四氯苯二甲酸、1,5-萘二羧酸、富马酸、马来酸、衣康酸、柠康酸、中康酸和四氢苯二甲酸，而不限于此。
二醇的实例可包括二元醇类，例如乙二醇、1,2-丙二醇、己二醇、新戊二醇、二乙二醇、三乙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、二丙二醇、二丁二醇、2-甲基-1,3-戊二醇、2,2,4-三甲基-1,3-戊二醇和1,4-环己烷二甲醇，而不限于此。
二异氰酸酯可包括芳族、脂环族或脂族二异氰酸酯，例如异佛尔酮二异氰酸酯(IPDI)、4,4'-联苯基甲烷二异氰酸酯(MDI)、1,6-六亚甲基二异氰酸酯(HDI)、二甲苯二异氰酸酯、氢化联苯基甲烷二异氰酸酯、萘二异氰酸酯、2,4-甲苯二异氰酸酯和2,6-甲苯二异氰酸酯，而不限于此。
聚酯聚氨酯树脂可具有10,000g/mol至200,000g/mol，具体地50,000g/mol至100,000g/mol的重均分子量，而不限于此。
这些粘结剂树脂可单独或与两种或更多种具有不同重均分子量的粘结剂树脂组合地使用。当使用两种或更多种具有不同重均分子量的粘结剂树脂时，可能防止在仅使用具有高重均分子量的粘结剂的情况下发生的膜硬化过度的问题和在仅使用具有低重均分子量的粘结剂的情况下发生的膜形成困难的问题。此外，与仅使用具有中等重均分子量的粘结剂的情况相比，根据本发明的各向异性导电膜组合物可通过具有不同重均分子量的粘结剂树脂之间的互补而形成具有优异的性能的各向异性导电膜。
在一个实施方式中，粘结剂树脂可以是树脂组合物，包括丙烯腈-丁二烯橡胶树脂、聚氨酯树脂和丙烯酸树脂。
在一些实施方式中，树脂组合物可包括1重量%(wt%)至10wt%的丙烯腈-丁二烯橡胶树脂、20wt%至40wt%的聚氨酯树脂和10wt%至30wt%的丙烯酸树脂。在该组分含量范围内时，树脂组合物可提供优异的成膜性和粘合性。
在一些实施方式中，基于各向异性导电膜以固体含量计的总量，粘结剂树脂可以30wt%至80wt%、具体地40wt%至70wt%，例如50wt%至70wt%的量存在。在该范围内，粘结剂树脂可提供优异的成膜性和粘合性。
(b)自由基聚合材料
在本发明的实施方式中，自由基聚合材料包括第一自由基聚合材料和第二自由基聚合材料，所述第一自由基聚合材料在其结构中具有一个或两个(甲基)丙烯酸酯反应基团，所述第二自由基聚合材料在其结构中具有至少三个(甲基)丙烯酸酯反应基团。
此处，第一自由基聚合材料的实例可包括(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸异癸酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸C12-C15烷基酯、(甲基)丙烯酸正硬脂酯、(甲基)丙烯酸正丁氧基乙酯、(甲基)丙烯酸丁氧基二乙二醇酯、(甲基)丙烯酸甲氧基三乙二醇酯、(甲基)丙烯酸甲氧基聚乙二醇酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸四氢糠酯、(甲基)丙烯酸苄酯、(甲基)丙烯酸2-苯氧乙酯、(甲基)丙烯酸异冰片酯、(甲基)丙烯酸2-羟乙酯、(甲基)丙烯酸2-羟丙酯、(甲基)丙烯酸2-羟丁酯、(甲基)丙烯酸4-羟丁酯、(甲基)丙烯酸二甲基氨基乙酯、(甲基)丙烯酸二乙基氨基乙酯、(甲基)丙烯酸、2-(甲基)丙烯酰氧乙基琥珀酸、2-(甲基)丙烯酰氧乙基六氢邻苯二甲酸酯、2-(甲基)丙烯酰氧乙基-2-羟丙基邻苯二甲酸酯、(甲基)丙烯酸缩水甘油酯、2-(甲基)丙烯酰氧乙基酸式磷酸酯、二(甲基)丙烯酸乙二醇酯、二(甲基)丙烯酸二乙二醇酯、二(甲基)丙烯酸三乙二醇酯、二(甲基)丙烯酸1,4-丁烷二醇酯、二(甲基)丙烯酸新戊二醇酯、二(甲基)丙烯酸1,6-己二醇酯、二(甲基)丙烯酸1,9-壬二醇酯、二(甲基)丙烯酸1,10-癸二醇酯、二(甲基)丙烯酸甘油酯、(甲基)丙烯酸2-羟基-3-丙烯酰氧基丙酯、二(甲基)丙烯酸二羟甲基三环癸烷基酯、(甲基)丙烯酸三氟乙酯、(甲基)丙烯酸全氟辛基乙酯、丙烯酸异戊酯、双酚A的环氧乙烷加合物的二(甲基)丙烯酸酯、双酚A的环氧丙烷加合物的二(甲基)丙烯酸酯、三羟甲基丙烷-苯甲酸-(甲基)丙烯酸酯、双酚A二(甲基)丙烯酸二缩水甘油酯、甲苯二异氰酸酯和(甲基)丙烯酸2-羟基-3-苯氧基丙酯的加合物，而不限于此。这些可单独或以其组合使用。
在一些实施方式中，基于各向异性导电膜以固体含量计的总量，第一自由基聚合材料可以5wt%至40wt%、具体地7wt%至40wt%，例如10wt%至40wt%的量存在。在该范围内，第一自由基聚合材料可允许固化产物整体形成充分的丙烯酸酯固化结构并且可防止固化产物的硬度过度增加以及剥离强度和粘合性的劣化。
此外，第二自由基聚合材料的实例可包括三(甲基)丙烯酸酯三羟甲基丙酯、环氧乙烷改性的三羟甲基丙烷的三(甲基)丙烯酸酯、三(甲基)丙烯酸季戊四醇酯、四(甲基)丙烯酸季戊四醇酯、六(甲基)丙烯酸二季戊四醇酯、三(甲基)丙烯酸季戊四醇酯和六亚甲基二异氰酸酯的加合物、三(甲基)丙烯酸季戊四醇酯和甲苯二异氰酸酯的加合物、三(甲基)丙烯酸季戊四醇酯和异佛尔酮二异氰酸酯的加合物、和五(甲基)丙烯酸二季戊四醇酯和六亚甲基二异氰酸酯的加合物，而不限于此。这些可单独或以其组合使用。
在一些实施方式中，基于各向异性导电膜以固体含量计的总量，第二自由基聚合材料可以1wt%至20wt%、具体地1wt%至15wt%，例如1wt%至10wt%的量存在。在该范围内，第二自由基聚合材料可充分增加固化速率并且可通过三维固化结构提供高可靠性。此外，在该范围内，第二自由基聚合材料可防止固化产物的硬化过度增加、剥离强度和粘合性的劣化、以及由于组合物的反应性过度增加造成的储存稳定性的劣化。
在一些实施方式中，基于各向异性导电膜以固体含量计的总量，自由基聚合材料的总含量可为6wt%至60wt%、具体地10wt%至50wt%，例如20wt%至40wt%。在该范围内，自由基聚合材料可允许固化产物整体形成充分的丙烯酸酯固化结构并且可防止固化产物的硬度过度增加以及剥离强度和粘合性的劣化。
在一些实施方式中，第一自由基聚合材料和第二自由基聚合材料可以以1至10、具体地1至7，例如1至5，更具体地，2至4的重量比(第一自由基聚合材料/第二自由基聚合材料)混合。
在第一自由基聚合材料与第二自由基聚合材料的重量比的该范围内，自由基聚合材料可与粘结剂形成致密网状交联，而不是线状交联，从而提供低透湿性和低吸湿性，同时保持在连接电阻、粘合性、鼓泡性能等方面的优异的可靠性。
(c)导电颗粒
在本发明中，可不加限制地使用本领域通常已知的任何导电颗粒。
导电颗粒的实例可包括金属颗粒，例如金(Au)、银(Ag)、镍(Ni)、铜(Cu)和焊料颗粒；碳颗粒；树脂颗粒，例如聚乙烯、聚丙烯、聚酯、聚苯乙烯、聚乙烯醇和其涂有金属(例如金(Au)、银(Ag)、镍(Ni)等)的改性的树脂颗粒；和绝缘导电颗粒，所述导电颗粒通过在金属涂敷的聚合物树脂颗粒上进一步涂敷绝缘颗粒而获得，而不限于此。这些可单独或以其组合使用。
根据电路的节距，导电颗粒可具有各种平均粒径，并且如果需要，导电颗粒的平均粒径可在1μm至30μm的范围内。
在一些实施方式中，基于各向异性导电膜以固体含量计的总量，导电颗粒可以0.1wt％至约30wt％，具体地1wt％至20wt％，更具体地1wt％至10wt％的量存在。在该含量范围内，各向异性导电膜可通过防止连接和/或分离中的故障而呈现优异的连接特性。
在其它实施方式中，除了(a)、(b)和(c)组分外，各向异性导电膜可进一步包括无机颗粒。当无机颗粒被进一步包括于各向异性导电膜的组合物中时，所述无机颗粒可在将各向异性导电膜向电极压制时均匀地分散压力，并且可降低各向异性导电膜的透湿性和吸湿性，同时改善粘合性和连接可靠性。
无机颗粒的实例可包括至少一种类型的陶瓷颗粒，所述陶瓷颗粒选自二氧化硅、Al2O3、TiO2、ZnO、MgO、ZrO2、PbO、Bi2O3、MoO3、V2O5、Nb2O5、Ta2O5、WO3和In2O3，而不限于此。
二氧化硅颗粒可具有0.01μm至10μm，具体地0.05μm至5μm，更具体地0.1μm至1μm的平均粒径，而不限于此。
基于各向异性导电膜以固体含量计的总量，二氧化硅颗粒可以0.1wt%至20wt%，具体地0.1wt%至10wt%的量存在。在该范围内，无机颗粒可使施加于电极的压力均匀分散并且可降低各向异性导电膜的透湿性和吸湿性，同时改善粘合性和连接可靠性。
各向异性导电膜可进一步包括固化引发剂。
在本发明中，可不加限制地使用本领域已知的任何典型的固化引发剂。固化引发剂的实例可包括基于过氧化物(有机过氧化物)类引发剂和偶氮类引发剂，而不限于此。
过氧化物类引发剂的实例可包括过氧化乙酰丙酮、过氧化甲基环己烷、过氧化甲乙酮、1,1-双(叔丁基过氧化)环己烷、1,1-双(叔丁基过氧化)-2-甲基环己烷、1,1-双(叔丁基过氧化)-3,3,5-三甲基环己烷、正丁基-4,4-双(叔丁基过氧化)戊酸酯、2,2-双(叔丁基过氧化)丁烷、叔丁基过氧化氢、萜烷过氧化氢、1,1,3,3-四甲基丁基过氧化氢、α',α'-双(叔丁基过氧化)二异丙苯、2,5-二甲基-2,5-双(叔丁基过氧化)己烷、2,5-二甲基-2,5-双(叔丁基过氧化)-3-已炔、过氧化苯甲酰、月桂基过氧化物、硬脂酰过氧化物、琥珀酸过氧化物、3,5,5-三甲基己酰过氧化物、过氧化二碳酸二-2-乙氧基乙酯、过氧化二碳酸二异丙酯、过氧化二碳酸二-3-甲氧丁酯、过氧化二碳酸二-2-乙基己酯、双(4-叔丁基环己基)过氧化二碳酸酯、过氧乙酸叔丁酯、叔丁基过氧化-2-乙基己基单碳酸酯、叔丁基过氧化单碳酸异丙酯、过氧化月桂酸叔丁酯、叔丁基过氧马来酸、过氧化新癸酸叔丁酯、过氧化-2-乙基己酸叔丁酯、过氧化新戊酸叔丁酯、过氧化苯甲酸叔丁酯、过氧化-间-甲苯甲酸叔丁酯/苯甲酸叔丁酯、过氧化-3,3,5-三甲基己酸叔丁酯、α',α'-双(新癸酰基过氧化)二异丙苯、枯基过氧新癸酸酯、1-环己基-1-甲基乙基过氧化新癸酸酯、2,5-二甲基-2,5-双(间甲苯酰基过氧化)己烷(2,5-二甲基-2,5-双(间甲苯酰基过氧化)己烷)、2,5-二甲基-2,5-双(2-乙基己酰基过氧化)己烷、2,5-二甲基-2,5-双(苯甲酰基过氧化)己烷、叔己基过氧化异丙基单碳酸酯、过氧化新癸酸叔己酯、过氧化-2-乙基己酸叔己酯、过氧化三甲基乙酸叔己酯、过氧化-2-乙基己酸1,1,3,3-四甲基丁酯和3,3',4,4'-四(叔丁基过氧化羰基)二苯甲酮，而不限于此。这些可单独或以其组合使用。
偶氮类引发剂的实例可包括2,2'-偶氮双(4-甲氧基-2,4-二甲基戊腈)、二甲基2,2'-偶氮双(2-甲基丙酸酯)和2,2'-偶氮双(N-环己基-2-甲基丙酸酯)，而不限于此。这些可单独或以其组合使用。
在一些实施方式中，基于各向异性导电膜以固体含量计的总重量，固化引发剂可以0.1wt%至20wt%，具体地0.1wt%至15wt%，更具体地1wt%至10wt%的量存在。在该含量范围内，组合物可在短时间内被充分固化并且具有良好的相容性，从而允许有效形成各向异性导电膜。
在其它实施方式中，为了向膜提供其它性能而不劣化膜的基本性能，各向异性导电膜可进一步包括添加剂，例如聚合抑制剂、抗氧化剂、热稳定剂、固化加速剂、偶联剂等。可以根据膜的目的和预期作用以各种方式确定这些添加剂的加入量，并且所述各种方式是本领域技术人员所熟知的。
未特别限定一种制备根据本发明的实施方式的各向异性导电膜的方法，并且可不加限制地使用本领域已知的任何典型的方法。
不需要特殊装置或设备来形成各向异性导电膜。例如，各向异性导电膜可通过如下制备：将粘合剂树脂溶解于有机溶剂中，加入各向异性导电膜的其它组分，以不会引起导电微粒的粉碎的速率将混合物搅拌特定时间，将混合物涂布于离型膜上至适合的厚度(例如，10μm至50μm)，并经充分的时间干燥混合物以使有机溶剂蒸发。因此，各向异性导电膜可包括各向异性导电膜和离型膜。
根据本发明的各向异性导电膜可具有170g/m2/24小时以下，具体地160g/m2/24小时以下，更具体地150g/m2/24小时以下的透湿性。在该范围内，即使在高温和/或高湿下使用较长一段时间后，各向异性导电膜也可在粘合性、连接电阻等方面呈现优异的可靠性。
可不加限制地通过本领域已知的任何方法测量透湿性。例如，将各向异性导电膜切成具有5cm的直径和200μm的厚度的样品，并且在200℃固化1小时。此后，在将固化的样品放置在含有20g氯化钙的瓶子的入口处，密封瓶子并且测量和记录瓶子的初始重量。此后，将瓶子置于85℃和85%RH(相对湿度)下24小时并且从样品表面除去水分，随后测量瓶子的重量。最后，记录重量增量。
根据本发明的各向异性导电膜可具有2%以下，具体地1.5%以下，更具体地1.2%以下的吸湿性。在该范围内，即使在高温和/或高湿下使用较长一段时间后，各向异性导电膜也可在粘合性、连接电阻、鼓泡性能等方面呈现优异的可靠性。
可不加限制地通过本领域已知的任何方法测量吸湿性。例如，将各向异性导电膜切成具有2cm×2cm x200μm(长度、宽度、厚度)的尺寸的样品并且在200℃固化1小时，随后测量样品的初始重量。此后，将样品置于85℃和85%RH下24小时并且从样品表面除去水分，随后测量样品的重量。最后，记录重量增量。
在一些实施方式中，各向异性导电膜可具有400gf/cm以上，具体地450gf/cm以上，更具体地500gf/cm以上，例如530gf/cm以上的可靠性粘合强度。可靠性粘合强度是指在从各向异性导电膜中去除离型膜的情况下，在经受预压制和主压制并置于85℃和85%RH下500小时后测量的粘合强度。
预压制可在60℃至80℃的条件下在1.0Mpa至4.0Mpa进行1秒至3秒，并且主压制可在170℃至200℃的条件下在2.5MPa至7Mpa进行1秒至7秒。例如，可靠性粘合强度可通过以下方法测量：将所制备的各向异性导电膜置于室温(25℃)下1小时并且使用金属电极玻璃(Mo/Al/Mo结构，Samsung Electronics Co.,Ltd.)和COF(Samsung Electronics Co.,Ltd.)制备多个样品，所述多个样品通过在约70℃的测量温度在1MPa的条件下预压制1秒，随后在从各向异性导电膜去除离型膜的情况下，在185℃和4.5MPa下主压制4秒而制备。将每个样品置于85℃和85%RH下500小时，随后使用剥离强度测试仪H5KT(Tinius Olsen)以90°的剥离角和50mm/min的剥离速率测量平均剥离强度。
在一些实施方式中，各向异性导电膜中包括的各向异性导电膜可具有3Ω以下，具体地2.6Ω以下的可靠性连接电阻。可靠性连接电阻是指在从所述各向异性导电膜去除离型膜的情况下，在经受预压制和主压制以及置于85℃和85%RH下500小时后测量的连接电阻。在该范围内，即使在高温和/或高湿的条件下使用较长一段时间后，各向异性导电膜也具有低电阻，从而提供优异的可靠性。
例如，可靠性连接电阻强度可通过以下方法测量：将所制备的各向异性导电膜置于室温(25℃)下1小时，并且通过在70℃的所测量温度的条件下在1MPa预压制1秒，随后在从各向异性导电膜去除离型膜的情况下在185℃和4.5MPa下主压制4秒连接各向异性导电膜与COF(Samsung Electronics Co.,Ltd.)而制备每种各向异性导电膜的10个样品，所述COF通过形成图案而制备，因此允许在涂有厚ITO层的0.5t无图案玻璃板上进行4探针测量。在将每种各向异性导电膜的10个样品置于85℃和85%RH下500小时以评估在高温和高湿条件下的可靠性后，测量每个样品的可靠性连接电阻(根据ASTM D117)并且计算平均值。
在一些实施方式中，各向异性导电膜中包括的各向异性导电膜可具有20%以下，具体地15%以下的可靠性鼓泡面积。可靠性鼓泡面积是指在从中去除离型膜的情况下，在预压制和主压制后以及置于85℃和85%RH下500小时后所测量的鼓泡面积。在该范围内，各向异性导电膜即使在高温和/或高湿的条件下使用较长一段时间后也具有窄鼓泡面积，从而提供优异的粘合性和可靠性。
例如，可靠性鼓泡面积可通过以下方法测量：将所制备的各向异性导电膜置于室温(25℃)下1小时，且通过在70℃的所测量温度的条件下在1MPa预压制1秒，随后在从各向异性导电膜去除离型膜的情况下在185℃和4.5MPa下主压制4秒，并使用金属电极玻璃(Mo/Al/Mo结构，Samsung Electronics Co.,Ltd.)和COF(SamsungElectronics Co.,Ltd.)制备多个样品。
将每种各向异性导电膜的10个样品置于85℃和85%RH下500小时以评估在高温和高湿条件下的可靠性，并且使用光学显微镜对每个样品的10个点进行拍照。此后，使用图像分析仪测量鼓泡面积与电极间的空间的面积的比率，并且计算平均值。
根据本发明的另一实施方式，半导体装置包括：具有第一电极的第一连接元件；具有第二电极的第二连接元件；以及根据本发明的各向异性导电膜，其被置于第一连接元件和第二连接元件中并且将第一电极和第二电极彼此电连接。
参照图1，根据该实施方式的半导体装置包括具有第一电极70的第一连接元件50；具有第二电极80的第二连接元件60；和包括导电颗粒40的各向异性导电膜10。当压制置于具有第一电极70的第一连接元件50和具有第二电极80的第二连接元件60之间的各向异性导电膜10时，第一电极70和第二电极80经由导电微粒40彼此连接。在该实施方式中，第一连接元件50和第二连接元件60可具有在材料、厚度、尺寸和相互连接性方面类似的结构。第一连接元件50和第二连接元件60可具有约20μm至约100μm的厚度。
在另一个实施方式中，第一连接元件和第二连接元件在材料、厚度、尺寸和相互连接性方面可具有不同结构和功能。第一连接元件或第二连接元件可由玻璃、PCB(印刷电路板)、fPCB、COF、TCP、ITO玻璃等形成，而不限于此。第一电极或第二电极可以是突出电极或平板电极。当第一电极和第二电极是突出电极时，这些电极可具有约2.50μm至约10μm的高度(H)，约50μm至约100μm的宽度(W)，以及约50μm至约110μm的电极间空隙(G)。优选地，电极具有约2.50μm至约9μm的高度(H)，约50μm至约100μm的宽度(W)，以及约60μm至约100μm的电极间空隙(G)。
当第一电极和第二电极是平板电极时，这些电极可具有约至约的厚度，并且可可由ITO、铜、硅、IZO等形成，而不限于此。
平板电极可具有至的厚度，并且突出电极可具有约6μm至约10μm的高度。此处，当绝缘层具有4μm至12μm的厚度时，可确保充分的粘附性。更优选地，平板电极具有的厚度并且突出电极具有8μm的高度。此处，绝缘层具有6μm至10μm的厚度。
根据本发明，可不加限制地使用本领域已知的任何方法制备半导体装置。
接下来，将参考一些实施例更详细地描述本发明。但是，应理解，提供了这些实施例仅用于进行阐述并且不应以任何方式被解释为限制本发明。
实施例1
通过混合以下试剂制备用于各向异性导电膜的组合物：5wt%的丙烯腈-丁二烯橡胶树脂(N-34,Nippon Zeon)、35wt%的聚氨酯树脂(NPC7007T,Nanux)、20wt%的丙烯酸树脂(AOF-7003,Aekyung Chemical)、13wt%的丙烯酸4-羟丁酯、13wt%的二羟甲基三环癸烷二丙烯酸酯、8wt%的三丙烯酸季戊四醇酯、3wt%的导电颗粒(3μm的平均粒径，Sekisui)和3wt%的月桂基过氧化物。
将组合物以不粉碎导电颗粒的搅拌速率在室温(25℃)搅拌60分钟。使用组合物在经硅酮脱模表面处理的聚乙烯基膜上形成35μm厚的膜，并且使用铸刀以用于膜的形成。将膜在60℃干燥5分钟。
实施例2
以与实施例1中相同的方式制备实施例1各向异性导电膜，区别在于使用10wt%的丙烯酸4-羟丁酯、10wt%的二羟甲基三环癸烷二丙烯酸酯和9wt%的三丙烯酸季戊四醇酯，并且另外使用5wt%的二氧化硅颗粒(0.5μm,Denka)。
实施例3
以与实施例1中相同的方式制备各向异性导电膜，区别在于使用26wt%的二羟甲基三环癸烷二丙烯酸酯替代丙烯酸4-羟丁酯。
对比例1
以与实施例1中相同的方式制备各向异性导电膜，区别在于使用9wt%的丙烯酸4-羟丁酯和25wt%的二氧化硅颗粒(0.5μm,Denka)而不使用二羟甲基三环癸烷二丙烯酸酯和三丙烯酸季戊四醇酯。
对比例2
以与实施例1中相同的方式制备各向异性导电膜，区别在于使用17wt%的丙烯酸4-羟丁酯和17wt%的二羟甲基三环癸烷二丙烯酸酯而不使用三丙烯酸季戊四醇酯。
对比例3
以与实施例1中相同的方式制备各向异性导电膜，区别在于使用7wt%的丙烯酸4-羟丁酯、7wt%的二羟甲基三环癸烷二丙烯酸酯和20wt%的三丙烯酸季戊四醇酯。
对比例4
以与实施例1中相同的方式制备各向异性导电膜，区别在于使用16wt%的丙烯酸4-羟丁酯、16wt%的二羟甲基三环癸烷二丙烯酸酯和2wt%的季戊四醇三丙烯酸酯。
实施例1至3和对比例1至4中制备的各向异性导电膜的组合物示于表1中。
表1
实验例1：透湿性的测量
如下测量实施例1至3和对比例1至4中制备的每种各向异性导电膜的透湿性。
将每种各向异性导电膜切成具有5cm的直径和200μm的厚度的样品，并且在200℃固化1小时。此后，在将固化的样品放置在含有20g氯化钙的瓶子的入口处，密封瓶子并且测量和记录瓶子的初始重量。
此后，将瓶子置于85℃和85%RH下24小时并且从样品表面除去水分，随后测量瓶子的重量。最后，记录重量增量。
实验例2：吸湿性的测量
如下测量实施例1至3和对比例1至4中制备的每种各向异性导电膜的吸湿性。
将每种各向异性导电膜切成具有2cm×2cm x200μm(长度、宽度、厚度)的尺寸的样品并且在200℃固化1小时，随后测量样品的初始重量。
此后，将样品置于85℃和85%RH下24小时并且从样品表面除去水分，随后测量样品的重量。最后，记录重量增量。
实验例3：可靠性连接电阻的测量
如下测量实施例1至3和对比例1至4中制备的每种各向异性导电膜的可靠性连接电阻。
将每种各向异性导电膜置于室温(25℃)下1小时，并且通过通过在70℃的所测量温度的条件下在1MPa预压制1秒，随后在从各向异性导电膜去除离型膜的情况下在185℃和4.5MPa下主压制4秒连接各向异性导电膜与COF(Samsung Electronics Co.,Ltd.)而制备每种各向异性导电膜的10个样品，所述COF通过形成图案而制备，因此允许在涂有厚ITO层的0.5t无图案玻璃板上进行4探针测量。
在将每种各向异性导电膜的10个样品置于85℃和85%RH下500小时以评估在高温和高湿条件下的可靠性后，测量每个样品的可靠性连接电阻(根据ASTM D117)并且计算平均值。
实验例4：可靠性粘合强度的测量
如下测量实施例1至3和对比例1至4中制备的每种各向异性导电膜的可靠性粘合强度。
将每种各向异性导电膜置于室温(25℃)下1小时，并且通过在70℃的所测量温度的条件下在1MPa预压制1秒，随后在从各向异性导电膜去除离型膜的情况下在185℃和4.5MPa下主压制4秒使用金属电极玻璃(Mo/Al/Mo结构，Samsung Electronics Co.,Ltd.)与COF(Samsung Electronics Co.,Ltd.)而制备每种各向异性导电膜的10个样品。
将10个样品中的每个置于85℃和85%RH下500小时以评估在高温和高湿条件下的可靠性，随后使用剥离强度测试仪H5KT(Tinius Olsen)以90°的剥离角和50mm/min的剥离速率测量平均剥离强度。
实验例5：可靠性鼓泡面积的测量
如下测量实施例1至3和对比例1至4中制备的每种各向异性导电膜的可靠性鼓泡面积。
将每种各向异性导电膜置于室温(25℃)下1小时，并且通过在70℃的所测量温度的条件下在1MPa预压制1秒，随后在从各向异性导电膜去除离型膜的情况下在185℃和4.5MPa下主压制4秒连接各向异性导电膜与COF(Samsung Electronics Co.,Ltd.)而制备每种各向异性导电膜的10个样品，所述COF通过形成图案而制备，因此允许在涂有厚ITO层的0.5t无图案玻璃板上进行4探针测量。
在将每种各向异性导电膜的10个样品置于85℃和85%RH下500小时以评估在高温和高湿条件下的可靠性，并且使用光学显微镜对每个样品的10个点进行拍照。此后，使用图像分析仪测量鼓泡面积与电极间的空间的面积的比率，并且计算平均值。
实验例1至5的测量结果示于表2中。
表2
性能 E1 E2 E3 CE1 CE2 CE3 CE4
透湿性(g/m2/24小时) 130 110 140 130 260 220 210
吸湿性(%) 1.2 0.9 1.2 1.1 2.3 2.2 2.2
可靠性连接电阻(Ω) 2.4 2.3 2.4 2.8 3.8 2.7 3.4
可靠性粘合强度(gf/cm) 550 550 540 320 350 390 360
可靠性鼓泡面积(%) 10 12 10 35 22 19 20
尽管已经公开了一些实施方式，但是对于本领域技术人员显而易见的是，实施方式仅以说明的方式被给出，并且可在不背离本发明的精神和范围的情况下作出各种修改、改变、变更和等效的实施方式。本发明的范围应当仅受所附权利要求限制。

Claims (13)

1.一种各向异性导电膜，包括：
(a)粘结剂树脂；(b)第一自由基聚合材料和第二自由基聚合材料，所述第一自由基聚合材料在其结构中具有一个或两个(甲基)丙烯酸酯反应基团，所述第二自由基聚合材料在其结构中具有至少三个(甲基)丙烯酸酯反应基团；和(c)导电颗粒；
其中所述各向异性导电膜具有170g/m2/24小时以下的透湿性和2%以下的吸湿性。
2.根据权利要求1所述的各向异性导电膜，其中所述各向异性导电膜具有400gf/cm以上的可靠性粘合强度，其中在60℃至80℃的条件下在1.0Mpa至4.0Mpa预压制1秒至3秒，并在从预压制后的各向异性导电膜去除离型膜的情况下在170℃至200℃的条件下在2.5MPa至7Mpa主压制1秒至7秒，且将所述各向异性导电膜置于85℃的温度和85%的相对湿度下500小时后，测量所述可靠性粘合强度。
3.根据权利要求1所述的各向异性导电膜，其中所述各向异性导电膜具有3Ω以下的可靠性连接电阻，其中在60℃至80℃的条件下在1.0Mpa至4.0Mpa预压制1秒至3秒，并在从预压制后的各向异性导电膜去除离型膜的情况下在170℃至200℃的条件下在2.5MPa至7Mpa主压制1秒至7秒，且将所述各向异性导电膜置于85℃的温度和85%的相对湿度下500小时后，测量所述可靠性连接电阻。
4.根据权利要求1所述的各向异性导电膜，其中所述各向异性导电膜具有20%以下的可靠性鼓泡面积，其中在60℃至80℃的条件下在1.0Mpa至4.0Mpa预压制1秒至3秒，并在从预压制后的各向异性导电膜去除离型膜的情况下在170℃至200℃的条件下在2.5MPa至7Mpa主压制1秒至7秒，且将所述各向异性导电膜置于85℃的温度和85%的相对湿度下500小时后，测量所述可靠性鼓泡面积。
5.根据权利要求1所述的各向异性导电膜，其中以固体含量计，所述各向异性导电膜包括：30wt%至80wt%的(a)粘结剂树脂；6wt%至60wt%的(b)自由基聚合材料；和0.1wt%至20wt%的(c)导电颗粒。
6.根据权利要求1所述的各向异性导电膜，其中所述第一自由基聚合材料与所述第二自由基聚合材料的重量比在1至10的范围内。
7.根据权利要求1所述的各向异性导电膜，其中所述(a)粘结剂树脂包括至少两种类型的具有不同重均分子量的树脂。
8.根据权利要求7所述的各向异性导电膜，其中所述(a)粘结剂树脂包括至少两种类型的树脂，所述至少两种类型的树脂选自由丙烯腈-丁二烯橡胶树脂、聚氨酯树脂和丙烯酸树脂组成的组中。
9.根据权利要求1所述的各向异性导电膜，其中所述第一自由基聚合材料包括选自由(甲基)丙烯酸羟丁酯、(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸2-羟丙酯和(甲基)丙烯酸缩水甘油酯组成的组中的至少一种。
10.根据权利要求1所述的各向异性导电膜，其中所述第二自由基聚合材料包括选自由三(甲基)丙烯酸季戊四醇酯、三(甲基)丙烯酸酯三羟甲基丙酯、环氧乙烷改性的三羟甲基丙烷的三(甲基)丙烯酸酯、四(甲基)丙烯酸季戊四醇酯和六(甲基)丙烯酸二季戊四醇酯的至少一种。
11.根据权利要求1所述的各向异性导电膜，其中所述各向异性导电膜进一步包括无机颗粒。
12.根据权利要求11所述的各向异性导电膜，其中基于各向异性导电膜以固体含量计的总重量，所述无机颗粒以0.1wt%至20wt%的量存在。
13.一种半导体装置，包括：
包括第一电极的第一连接元件；
包括第二电极的第二连接元件；和
根据权利要求1至12中任一项所述的各向异性导电膜，所述各向异性导电膜被置于所述第一连接元件和所述第二连接元件之间并将所述第一电极连接至所述第二电极。
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