CN101407700B - 胶粘剂膜组合物、胶粘剂膜以及划片晶粒粘结膜 - Google Patents

胶粘剂膜组合物、胶粘剂膜以及划片晶粒粘结膜 Download PDF

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CN101407700B
CN101407700B CN200810161497XA CN200810161497A CN101407700B CN 101407700 B CN101407700 B CN 101407700B CN 200810161497X A CN200810161497X A CN 200810161497XA CN 200810161497 A CN200810161497 A CN 200810161497A CN 101407700 B CN101407700 B CN 101407700B
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adhesive film
resin
weight
cured resin
composition
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CN101407700A (zh
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洪容宇
郑基成
金完中
任首美
金相珍
丁畅范
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Cheil Industries Inc
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Cheil Industries Inc
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Abstract

本发明涉及一种半导体装配用胶粘剂膜组合物、胶粘剂膜以及划片晶粒粘结膜。该组合物包含具有羟基、羧基或环氧基的弹性体树脂，成膜树脂，与硅烷偶联剂预反应的酚醛固化树脂，环氧树脂，固化促进剂以及填料。酚醛固化树脂与硅烷偶联剂预反应以预先除去挥发性组分例如醇、湿气和挥发性反应副产物。通过除去挥发性组分可以使胶粘剂膜中空隙和气泡的形成降至最少。因此，该组合物的应用可以赋予胶粘剂膜高的可靠性。

Description

胶粘剂膜组合物、胶粘剂膜以及划片晶粒粘结膜
相关申请的交叉引用
根据U.S.C.§119的规定，该非临时申请要求2007年10月8日提出的第2007-100947号韩国专利申请的优先权，在此将其所有内容并入作为参考。
技术领域
所述公开涉及用于半导体装配的胶粘剂膜组合物，包含与硅烷偶联剂预反应的酚醛固化树脂(在下文中，简单地称其为“预反应酚醛固化树脂”)以及使用该组合物制备的胶粘剂膜。更具体地，该固化树脂与硅烷偶联剂预先反应以预先除去挥发性组分例如醇和水分，从而使在胶粘剂膜中所形成的空隙和气泡降至最少。
背景技术
银(Ag)浆主要用来将半导体元器件粘结到支撑元件或器件上。随着最近半导体元器件小型化和大容量的趋势，用于半导体元器件的支撑元件需要尺寸更小并且更精细。现在所使用的银浆受到许多缺点的困扰，例如，由半导体元器件的凸出或倾斜导致的不完全的引线接合，形成气泡和难于控制厚度。由于这些缺点，存在着使用胶粘剂膜代替银浆的增长趋势。
典型的用于半导体装配的胶粘剂膜与划片膜(dicing film)一起使用。划片膜是指在一系列的半导体晶片制造方法中的划片期间用来固定半导体晶圆的薄膜。划片是将半导体晶片切割成单个晶片的工艺。在划片之后，进行包括膨胀、粘附晶粒、引线接合和烘箱固化的工艺。粘附晶粒是将晶粒贴附到PCB或引线框架上的工艺，引线接合是将金属线与晶片和连接端子通过金线或铝线连接的工艺，以及烘箱固化是在晶粒粘合之后在烘箱中使一部分的胶粘剂元件固化从而将晶粒固定在PCB或引线框架上的工艺。
划片膜通常通过以下方式来生产：将UV固化胶粘剂或一般的可固化压敏胶粘剂涂敷到作为基膜的氯乙烯或聚烯烃膜之上并在其上粘附PET覆盖膜。另一方面，用于半导体装配的一般胶粘剂膜以如下方式使用：将胶粘剂膜贴附于半导体晶圆上，然后覆盖除去了覆盖膜的划片膜并且在胶粘剂膜之上展开，通过划片将所形成的结构切割成片。
目前应用于半导体装配的用于划片晶粒粘合的胶粘剂膜是胶粘剂膜和已经预先除去了覆盖膜的划片膜的层压物。然后，将半导体晶圆贴附到该层压物上，接着通过划片切割成片。然而在这种情况下，存在如下的困难，在随后的拾取步骤中晶粒胶粘剂膜必须与晶粒同时被剥离，而不像传统的划片膜仅仅是为了划片。另外，在贴附晶粒胶粘剂膜到半导体晶圆背面时有可能会产生气泡。
进行软熔(reflowing)以使半导体封装贴装到基板上。如果胶粘剂膜层失去了其耐软熔性和耐温度循环性的话，就会有半导体封装内附着于晶片上的胶粘剂膜可能分层或晶片易于产生裂纹的危险。
通过增加胶粘剂膜组合物中的固化组分的含量可以获得用于半导体装配的胶粘剂膜的高可靠性。然而，增加固化组分的含量会导致如下缺点：为了提高中间层的粘合强度而在室温下保持一较长的时间时，此时胶粘剂膜层会与划片膜的压敏胶粘剂层相互影响，从而导致在拾取步骤中拾取成功率低。在处理期间随着固化组分含量的增加，能与湿气反应的羟基的数目也在增加。结果，挥发性组分大量产生，导致在粘附晶粒、引线接合、烘箱固化以及其他的处理步骤中形成空隙和气泡，它们是低可靠性的成因。另外，固化组分含量的增加导致膜拉伸强度的下降。拉伸强度下降的胶粘剂膜在预切割期间将产生变形，从而导致断裂、产生毛边或碎片，其中预切割步骤是将所述膜切割成与半导体晶圆相应的尺寸的工艺。
发明内容
此处公开了用于半导体装配的胶粘剂膜组合物，其包含具有羟基、羧基或环氧基的弹性体树脂，成膜树脂，环氧树脂，与硅烷偶联剂预反应的酚醛固化树脂，固化促进剂以及填料。
该胶粘剂膜组合物涉及与硅烷偶联剂预反应的酚醛固化树脂在胶粘剂膜生产中的应用。更具体地，该酚醛固化树脂与硅烷偶联剂预先反应以预先除去挥发性组分，例如在多个随后处理步骤中可能产生的醇和水分，结果使得在胶粘剂膜中所形成的空隙和气泡降至最少，从而获得胶粘剂膜的高可靠性。另外，在半导体装配的粘附晶粒、引线接合和烘箱固化工艺中，由于残留的挥发性组分而形成的空隙和气泡可以被降至最少。
此处也公开了用于半导体装配的胶粘剂膜，其使用胶粘剂膜组合物而制备。
此处也公开了包含胶粘剂膜的划片晶粒粘合膜。
具体实施方式
下面，将对示例性实施方案进行详细说明。
应当理解的是当一元件或层被认为是在另一元件或层“之上”、“介于”、“位于”或在另一个元件或层“之间”，它可以是直接地在其它元件或层上、介于、位于或在其它元件或层之间，或者可能存在中间元件或中间层。
应当理解的是虽然此处所使用的术语第一、第二、第三等被用来描述多种元件、部件、区域、层和/或部位，但是这些元件、部件、区域、层和/或部位不应被这些术语所限制。这些术语仅用于将一种元件、部件、区域、层或部位区别于另一种元件、部件、区域、层或部位。因此，下面所论述的第一元件、部件、区域、层或部分可被称为第二元件、部件、区域、层或部分，而没有偏离本发明的教示。
除非文中另外清楚地指出，此处所使用的单数形式“一种”以及“该”同时也包含了复数形式。应当进一步理解的是说明中使用的术语“含有”和/或“包含”，表示存在所述特征、整数、步骤、操作、元件和/或组分，但并没有排除另外的一种或多种的其他特征、整数、步骤、操作、元件、部件和/或它们的组的存在。
除另有说明外，在此使用的语句“基于胶粘剂膜组合物的总量的重量份”、“基于组合物的总量的重量份”、“基于胶粘剂膜组合物的总量的重量百分比”和“基于组合物的总量的重量百分比”未将溶剂计算在内。因此，在这里，“基于胶粘剂膜组合物的总量”的引用要点并不包括溶剂。举例来说，当一种组合物由两组分A和B组成，且基于胶粘剂膜组合物的总量A为35重量份、B为65重量份时，在该组合物中添加10重量份溶剂会产生如下结果：基于该胶粘剂膜组合物的总量，该组合物仍然含有35重量份的A和65重量份的B。
除非另有定义，此处使用的所有的术语(包括技术术语和科学术语)具有与发明所属领域的普通技术人员通常所理解的相同的含义。应当更进一步理解的是术语(诸如通常所使用的词典中的定义)应当理解为具有在与其相关的技术范围内相一致的含义，以及不会被理解为理想化的或过度形式上的意义，除非在此是这样表述的。
根据一实施方案，提供了胶粘剂膜组合物，其包含具有羟基、羧基或环氧基的弹性体树脂，成膜树脂，环氧树脂，与硅烷偶联剂预反应的酚醛固化树脂，固化促进剂以及填料。
特别地，基于组合物的总重量，胶粘剂膜组合物含有5～60％重量的弹性体树脂，5～60％重量的成膜树脂，5～40％重量的环氧树脂，3～25％重量的预反应酚醛固化树脂，0.01～10％重量的固化促进剂，以及3～60％重量的填料。
胶粘剂膜组合物可以进一步含有酚醛固化树脂，基于组合物的总重量，其用量为该另外的酚醛固化树脂和预反应的酚醛固化树脂用量的和为3～30％重量。
组成胶粘剂膜组合物的单个组分的说明如下。
弹性体树脂
弹性体树脂是一橡胶组分，能够赋予膜足够的强度从而易于处理膜，并且对于所形成的膜具有合适的粘结强度是所必需的。弹性体树脂优选包含羟基、羧基或环氧基。弹性体树脂的重均分子量优选在50,000～5,000,000的范围内，更优选100,000～800,000。适合用于胶粘剂膜组合物的弹性体树脂的例子包括，但不局限于：丙烯腈基弹性体、丁二烯基弹性体、苯乙烯基弹性体、丙烯酸基弹性体、异戊二烯基弹性体、乙烯基弹性体、丙烯基弹性体、聚氨酯基弹性体和硅树脂基弹性体。这些弹性体树脂可以单独使用或以其两种或更多种的组合使用。
基于胶粘剂膜组合物的总重量，弹性体树脂的典型用量为5～60％重量。
成膜树脂
成膜树脂赋予膜足够的强度从而易于处理膜并且有助于形成具有合适粘结强度的膜。
成膜树脂的玻璃化转变温度(Tg)在-30℃～200℃，优选0℃～200℃的范围内。
成膜树脂是酚醛树脂或苯氧基树脂，其包含羟基、环氧基、苯氧基或烷基，并且优选具有200～500,000的重均分子量。
当成膜树脂具有以上定义范围内较高的玻璃化转变温度(Tg)时，其有可能为酚醛树脂或苯氧基树脂，其含有氢醌、2-溴氢醌、间苯二酚、邻苯二酚、双酚A、双酚F、双酚AD、双酚S、4，4′-二羟基联苯或二(4-羟苯基)醚、苯酚、甲酚、甲酚酚醛清漆或芴成分作为骨架。酚醛树脂或苯氧基树脂可以具有至少一个选自烷基、芳基、羟甲基、烯丙基、脂环基、卤素和硝基的基团。同时，可将至少一个选自直链烷基、支链烷基、烯丙基、取代的烯丙基、脂环基和烷氧羰基的基团引入到双酚骨架的中心碳原子上。
基于胶粘剂膜组合物的总重量，成膜树脂优选以5～60％重量的量存在。
与硅烷偶联剂预反应的酚醛固化树脂
预反应酚醛固化树脂可以通过硅烷偶联剂与酚醛固化树脂以1:5～100的摩尔比反应制备。特别地，胶粘剂膜组合物使用作为由硅烷偶联剂与酚醛固化树脂的反应所获得的反应产物的预反应酚醛固化树脂。
[硅烷偶联剂]
用于制备预反应酚醛固化树脂的硅烷偶联剂具有粘着增强剂的作用，用于提高在组合物中树脂对无机原料(例如硅)表面的粘合力。通常可使用含环氧基硅烷或含巯基的硅烷作为硅烷偶联剂。示例性的硅烷化合物包括：含环氧基硅烷，例如2-(3，4-环氧基环己基)乙基三甲氧基硅烷、3-环氧丙氧基三甲氧基硅烷、3-环氧丙氧丙基三甲氧基硅烷和3-环氧丙氧丙基三乙氧基硅烷；含胺的硅烷，例如N-2-(氨乙基)-3-氨丙基甲基二甲氧基硅烷、N-2-(氨乙基)-3-氨丙基三甲氧基硅烷、N-2-(氨乙基)-3-氨丙基三乙氧基硅烷、3-氨丙基三甲氧基硅烷、3-氨丙基三乙氧基硅烷、3-三乙氧基甲硅烷基-N-(1，3-二甲基亚丁基)丙胺和N-苯基-3-氨丙基三甲氧基硅烷；含巯基的硅烷，例如3-巯丙基甲基二甲氧基硅烷和3-巯丙基三乙氧基硅烷；和含异氰酸酯的硅烷，例如3-异氰酸酯基丙基三乙氧基硅烷。
[酚醛固化树脂]
可以使用任何公知的酚醛固化树脂，而没有任何特别的限制，来制备预反应酚醛固化树脂。酚醛固化树脂优选为在一个分子中具有两个或更多酚羟基的化合物。优选的酚醛固化树脂为双酚固化树脂，例如双酚A树脂、双酚F树脂和双酚S树脂，和酚醛树脂，例如苯酚酚醛清漆树脂、双酚A酚醛清漆树脂、甲酚酚醛清漆树脂、新酚(xylok)树脂和联苯树脂，当暴露于湿气时，以上所有的树脂都显示出优秀的耐电解腐蚀能力。
可商业提供的酚醛固化树脂的例子包括：简单的酚醛固化树脂，例如H-1、H-4、HF-1M、HF-3M、HF-4M和HF-45(Meiwa PlasticIndustries Ltd.(日本))；对二甲苯型固化树脂，例如MEH-78004S、MEH-7800SS、MEH-7800S、MEH-7800M、MEH-7800H、MEH-7800HH和MEH-78003H(Meiwa Plastic Industries Ltd.(日本))、KPH-F3065(KolonChemical Co.，Ltd.(韩国))；联苯型固化树脂，例如MEH-7851SS、MEH-7851S、MEH7851M、MEH-7851H、MEH-78513H和MEH-78514H(Meiwa Plastic Industries Ltd.(日本))和KPH-F4500(Kolon Chemical Co.，Ltd.(韩国))；以及三苯甲基型固化树脂，例如MEH-7500、MEH-75003S、MEH-7500SS、MEH-7500S和MEH-7500H(Meiwa Plastic Industries Ltd.(日本))。这些酚醛固化剂可以单独使用或以其两种或更多种的混合物来使用。
酚醛固化树脂优选由结构式1表示：
Figure G200810161497XD00081
其中每个R1和R2独立地为C1～C4烷基或氢原子，a和b各自独立地为0～4，以及n为0～7的整数。
结构式1的酚醛固化树脂在其分子结构中具有两个或更多个羟基，当暴露于湿气的时候由于其低吸水性，展示出出色的耐电化学腐蚀能力、良好的耐热性以及优越的耐软熔性。
结构式1的酚醛固化树脂优选具有的羟基当量为100～600g/eq，更优选170～300g/eq。如果酚醛固化树脂的羟基当量低于100g/eq，那么吸湿性会趋于增加并且耐软熔性趋于下降。同时，如果酚醛固化树脂的羟基当量高于600g/eq，那么玻璃化转变温度趋于降低并且耐热性趋于变差。
预处理酚醛固化树脂可以通过使硅烷偶联剂与酚醛固化树脂反应来制备，以去除挥发性组分例如醇和湿气。
用来制备预反应酚醛固化树脂的硅烷偶联剂(a)与酚醛固化树脂(b)的摩尔比优选为1:5(a/b)～1:100(a/b)。如果硅烷偶联剂的比例小于下限(即1:5)，偶联剂趋于发生凝胶。同时，如果硅烷偶联剂的比例大于上限(即1:100)，偶联剂便不能按照要求与酚醛固化树脂预反应。
通过使用预反应固化树脂可以使空隙和气泡的形成降至最少。预反应固化树脂优选具有约500至约6,000的重均分子量。
基于胶粘剂膜组合物的总重量，预反应酚醛固化树脂优选以3～25％重量的量存在，优选约4～25％重量，更优选约4～15％重量。使用的预反应固化树脂的量小于3％重量时，无法保证最终膜具有足够的粘结强度，与此同时，使用的预反应固化树脂的量超过25％重量时，最终膜的粘结强度趋于变差。
酚醛固化树脂
胶粘剂膜组合物可以进一步包含酚醛固化树脂。该另外的酚醛固化树脂不同于用来制备预反应酚醛固化树脂的酚醛固化树脂，因为其不提前与硅烷偶联剂反应。该另外的酚醛固化树脂的种类可以与用来制备预反应酚醛固化树脂的酚醛固化树脂相同。
酚醛固化树脂的使用量，基于组合物的总重量，优选以该另外的酚醛固化树脂和预反应酚醛固化树脂的总量计为3～30％重量。如果总量小于3％重量，将无法得到流动性和耐热性方面令人满意的结果。同时，如果总量大于30％重量，将无法得到抗湿性和耐软熔性方面令人满意的结果。
环氧树脂
环氧树脂被用作可固化的胶粘剂。环氧树脂优选具有100～1,500g/eq，更优选150～800g/eq，并且最优选150～400g/eq的环氧当量。所使用的环氧树脂具有的环氧当量低于100g/eq时，固化成品的粘合性能趋于劣化。同时，环氧树脂的环氧当量高于1,500g/eq时，玻璃化转变温度降低、耐热性变差。对于环氧树脂的状态没有特别的限制，只要环氧树脂是可交联的并且具有粘性。考虑到最终膜的形状，环氧树脂优选为固态或大体上为固态。环氧树脂优选具有至少一个官能团。
作为环氧树脂，可以列举双酚类环氧树脂、苯酚酚醛清漆类环氧树脂、邻甲酚酚醛清漆类环氧树脂、多官能团环氧树脂、胺类环氧树脂、杂环类环氧树脂、取代的环氧树脂或萘酚类环氧树脂。商业可用的双酚类环氧树脂的例子包括：Epiclon830-S、EpiclonEXA-830CRP、Epiclon EXA850-S、Epiclon EXA-850CRP和EpiclonEXA-835LV(Dainippon Ink and Chemicals Inc.(日本))；Epicoat807、Epicoat815、Epicoat825、Epicoat827、Epicoat828、Epicoat834、Epicoat1001、Epicoat1004、Epicoat1007和Epicoat1009(Yuka-Shell Epoxy Co.，Ltd.(日本))；DER-330，DER-301和DER-361(Dow Chemical)；以及Yd-128和YDF-170(Kukdo Chemical Co.，Ltd.(韩国))。商业可用的邻甲酚酚醛清漆类树脂的例子包括：YDCN-500-1P、YDCN-500-4P、YDCN-500-5P、YDCN-500-7P、YDCN-500-80P和YDCN-500-90P(Kukdo Chemical Co.，Ltd.(韩国))；以及EOCN-102S、EOCN-103S、EOCN-104S、EOCN-1012、EOCN-1025和EOCN-1027(Nippon Kayaku Co.，Ltd.(日本))。商业可用的多官能团环氧树脂的例子包括：Epon1031S(Yuka-Shell Epoxy Co.，Ltd.(日本))；Araldite0163(CIBA Specialty Chemicals)；以及Denacol EX-611、Denacol EX-614、Denacol EX-614B、Denacol EX-622、Denacol EX-512、Denacol EX-521、Denacol EX-421、Denacol EX-411和Denacol EX-321(Nagase ChemteX Corp.(日本))。商业可用的胺类环氧树脂的例子包括：Epicoat604(Yuka-ShellEpoxy Co.，Ltd.(日本))；YH-434(Tohto Kasei Co.，Ltd.(日本))；TETRAD-X和TETRAD-C(Mitsubishi Gas Chemical Company Inc.(日本))；以及ELM-120(Sumitomo Chemical Co.，Ltd.(日本))。商业可用的杂环环氧树脂为从CIBA Specialty Chemicals得到的商标为PT-810的产品。商业可用的取代的环氧树脂包括ERL-4234、ERL-4299、ERL-4221和ERL-4206(UCC)。商业可用的萘酚类环氧树脂包括：Epiclon HP-4032、EpiclonHP-4032D、Epiclon HP-4700和Epiclon4701(Dainippon Ink and Chemicals，Inc.(日本))。这些环氧树脂可以单独使用或以其两种或更多种的混合物来使用。
基于胶粘剂膜组合物的总重量，环氧树脂的典型用量为5～40％重量。
环氧树脂可以与预反应酚醛固化树脂或与预反应酚醛固化树脂和另外的酚醛固化树脂以环氧当量与羟基当量的比为0.6～1.4:1的比例混合。即，当单独使用预反应酚醛固化树脂或与另外的酚醛固化树脂同时使用时，环氧当量与羟基当量的比例优选调节为0.6～1.4:1，更优选0.8～1.2:1。如果比例超出了该范围(即0.6～1.4:1)，最终胶粘剂膜的粘性和可固化性趋于变差。
固化促进剂
固化促进剂是一种在半导体加工的过程中缩短固化时间使环氧树脂完全固化的催化剂。
固化促进剂可以为磷化氢、硼或咪唑类型。
适合在胶粘剂膜组合物中应用的磷化氢类固化促进剂为：三苯膦、三邻甲苯基膦、三间甲苯基膦、三对甲苯基膦、三-2，4-二甲苯基膦、三-2，5-二甲苯基膦、三-3，5-二甲苯基膦、三苄基膦、三(对甲氧基苯基)膦、三(对叔丁氧苯基)膦、二苯基环己基膦、三环己基膦、三丁基膦、三叔丁基膦、三正辛基膦、二苯膦基苯乙烯、二苯基次亚膦酰氯、三正辛基氧化膦、二苯基氧膦基氢醌、氢氧化四丁基鏻、醋酸四丁基鏻、六氟锑酸苄基三苯基鏻、四苯基硼酸四苯基鏻、四对甲苯基硼酸四苯基鏻、四苯基硼酸苄基三苯基鏻、四氟硼酸四苯基鏻、四对甲苯基硼酸对甲苯基三苯基鏻、三苯膦三苯基硼烷、1，2-二(二苯膦基)乙烷、1，3-二(二苯膦基)丙烷、1，4-二(二苯膦基)丁烷和1，5-二(二苯膦基)戊烷。适合用于胶粘剂膜组合物的硼类固化促进剂为：苯基硼酸、4-甲基苯基硼酸、4-甲氧基苯基硼酸、4-三氟甲氧基苯基硼酸、4-叔丁氧基苯基硼酸、3-氟-4-甲氧基苯基硼酸、吡啶-三苯基硼烷、四苯基硼酸2-乙基-4-甲基咪唑鎓、1，8-二氮杂双环[5.4.0]十一烯-7-四苯基硼酸盐、1，5-二氮杂双环[4.3.0]壬烯-5-四苯基硼酸盐以及三苯基(正丁基)硼酸锂。适合用于胶粘剂膜组合物中的咪唑类固化促进剂为：2-甲基咪唑、2-十一烷基咪唑、2-十七烷基咪唑、2-乙基-4-甲基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑、1-苄基-2-苯基咪唑、1，2-二甲基咪唑、1-氰乙基-2-甲基咪唑、1-氰乙基-2-乙基-4-甲基咪唑、1-氰乙基-2-十一烷基咪唑，1-氰乙基-2-苯基咪唑、偏苯三酸1-氰乙基-2-十一烷基咪唑鎓、偏苯三酸1-氰乙基-2-苯基咪唑鎓、2，4-二氨基-6-[2’-甲基咪唑基-(1’)]-乙基-s-三嗪、2，4-二氨基-6-[2’-十一烷基咪唑基-(1’)]-乙基-s-三嗪、2，4-二氨基-6-[2’-乙基-4’-甲基咪唑基-(1’)]-乙基-s-三嗪、2，4-二氨基-6-[2’-甲基咪唑基-(1’)]-乙基-s-三嗪、异氰脲酸二水加合物、2-苯基咪唑异氰脲酸加合物、2-甲基咪唑异氰脲酸二水加合物、2-苯基-4，5-二羟基甲基咪唑、2-苯基-4-甲基-5-羟基甲基咪唑、2，3-二氢-1H-吡咯[1，2-a]苯并咪唑、4，4’-亚甲基-二(2-乙基-5-甲基咪唑)、2-甲基咪唑啉、2-苯基咪唑啉、2，4-二氨基-6-乙烯基-1，3，5-三嗪、2，4-二氨基-6-乙烯基-1，3，5-三嗪异氰脲酸加合物、2，4-二氨基-6-甲基丙烯酰氧乙基-1，3，5-三嗪异氰脲酸加合物、1-(2-氰乙基)-2-乙基-4-甲基咪唑、1-氰乙基-2-甲基咪唑、1-(2-氰乙基)-2-苯基-4，5-二-(氰基乙氧基甲基)咪唑、1-乙酰基-2-苯肼、2-乙基-4-甲基咪唑啉、2-苄基-4-甲基咪唑啉、2-乙基咪唑啉、2-苯基咪唑啉、2-苯基-4，5-二羟基甲基咪唑啉、三聚氰胺以及双氰胺。这些固化促进剂可以单独使用或以其两种或更多种的组合来使用。
在一实施方案中，可以使用结构式2或3所示的固化促进剂：
Figure G200810161497XD00131
其中R1～R8每个独立地为氢原子、卤素原子或烷基；或
Figure G200810161497XD00132
与使用胺类固化剂或咪唑类固化促进剂相比，结构式2或3的固化促进剂的使用提高了固化的起始温度，从而便于获得均一的固化速率。另外，与胺类固化剂或咪唑类固化促进剂相比，结构式2或3所示的固化促进剂在室温下反应活性较小。所以，结构式2或3的固化促进剂在确保储藏稳定性时是有利的。当在胺类固化剂或咪唑类固化促进剂的存在下使用结构式1的酚醛树脂时，在室温下随着存储时间的延长，酚醛树脂会部分地固化，从而引起不均匀的固化物理性能，从而在半导体的装配过程中导致空洞的形成或较差的粘结强度。
相反，当在结构式2或3的固化促进剂的存在下使用结构式1的酚醛树脂时，可以阻止酚醛树脂的固化，从而在半导体装配的过程中减少由不均匀的固化物理性能所引起的缺陷。
另外，与使用了胺类固化剂或咪唑类固化促进剂的组合物相比，使用了固化促进剂的胶粘剂膜组合物具有较低的导电率，因此在加压蒸煮器测试(PCT)中获得了较好的可靠性。
基于胶粘剂膜组合物的总重量，固化促进剂的含量优选为0.01～10％重量，并且更优选为0.03～5％重量。固化促进剂的存在量小于0.01％重量，会导致环氧树脂的不充分交联，从而导致最终膜耐热性变坏。同时，如果固化促进剂的存在量超过10％重量，最终膜的储藏稳定性趋于变坏。
填料
填料是一种能赋予组合物触变性能，从而控制组合物的熔体粘度的组分。可以非强制选择性地使用任何无机或有机的填料。对于无机填料，能够使用金属组分，例如金、银、铜或镍粉，或非金属组分，例如氢氧化铝、氢氧化镁、碳酸钙、碳酸镁、硅酸钙、硅酸镁、氧化钙、氧化镁、氧化铝、氮化铝、二氧化硅、氮化硼、二氧化钛、玻璃、氧化铁、陶瓷等。有机填料可以是碳基填料、橡胶基填料、聚合物基填料等。对于填料的形状和大小没有特别的限制。主要使用球形的二氧化硅或无定形二氧化硅作为无机填料。填料的平均粒径优选在5nm～10μm之间，更优选在10nm～3μm之间。
基于胶粘剂膜组合物的固态总重量，填料的使用量优选3～60％重量，更优选5～30％重量。如果混入的填料的量低于3％重量，那么添加填料的增强效果可以忽略不计。同时，如果混入的填料的量大于60％重量，对附着物的粘合性趋于变差。
硅烷偶联剂
胶粘剂膜组合物可以进一步含有偶联剂。该另外的硅烷偶联剂的种类可以与用来制备预反应酚醛固化树脂的硅烷偶联剂相同，在此省略对它的描述。
基于胶粘剂膜组合物的总重量，该另外的硅烷偶联剂的量优选为0.01～10％重量，更优选0.30～5％重量。
有机溶剂
胶粘剂膜组合物可以进一步地含有有机溶剂以获得低粘度。低粘度有利于膜的形成。对于有机溶剂的种类没有特别的限制。考虑到在成膜期间有机溶剂的挥发性，有机溶剂可以选自甲苯、二甲苯、丙二醇单甲醚醋酸酯、苯、丙酮、丁酮、四氢呋喃、二甲基甲酰胺、环己酮以及它们的混合物。
成膜后残留的有机溶剂的含量限定为1％或更少。在半导体的装配过程中，当晶粒贴附于印刷电路板(PCB)时，在有机溶剂中的挥发性组分的量残留过多的话，会导致空隙的形成。
有机溶剂构成胶粘剂膜组合物中的余量，基于胶粘剂膜组合物的总重量，可以以5～85％重量的量存在。
胶粘剂膜组合物可用于生产半导体装配用胶粘剂膜，无需使用专门的仪器或设备。可以使用本领域中任何已知的方法形成胶粘剂膜而没有限制，例如，由以下方法形成。首先，将弹性体树脂、成膜树脂、环氧树脂、固化树脂、固化促进剂、硅烷偶联剂、预反应固化树脂、填料等溶于有机溶剂。然后，使用珠磨机对溶液进行充分的揉捻，涂敷到经剥离处理的聚对苯二甲酸乙二醇酯膜上，然后加热干燥以形成具有适当涂层厚度的胶粘剂膜。胶粘剂膜的厚度优选调节到5～200μm，更优选10～100μm。厚度小于5μm时难以获得足够的粘结强度。同时，厚度大于200μm时经济上不理想。
根据另一实施方案，划片晶粒粘合膜包含使用胶粘剂膜组合物制备的胶粘剂膜。特别地，划片晶粒粘合膜通过随后将压敏胶粘剂(‘PSA’)层和胶粘剂膜层层压到基膜上制备，其中胶粘剂膜层是胶粘剂膜。
可以使用一般的PSA组合物制备PSA层。优选地，PSA层包含PSA聚合物粘合剂、紫外线可固化丙烯酸酯和光引发剂，其中紫外线可固化丙烯酸酯以相对于100重量份聚合物胶粘剂为20～150重量份的量存在，并且光引发剂以相对于100重量份紫外线可固化丙烯酸酯为0.1～5重量份的量存在。基膜优选是可透射辐射的。当使用对紫外线照射的辐射可固化的压敏胶粘剂施覆基膜时，基膜可以由高光透射性材料形成。可用于基膜的聚合物材料的例子有：聚烯烃的均聚物和共聚物，例如聚乙烯、聚丙烯、丙烯-乙烯共聚物、乙烯-丙烯酸乙酯共聚物、乙烯-丙烯酸甲酯共聚物和乙烯-醋酸乙烯脂共聚物，聚碳酸酯、聚甲基丙烯酸甲酯、聚氯乙烯以及聚氨酯共聚物。基膜的厚度需考虑到多种因素来决定，例如拉伸强度、伸长率和辐射穿透性。基膜最好具有50～200μm的厚度。
为了更好地理解示例性的实施方案，通过下列实施例进行更详细地描述。然而给出这些实施例仅仅是为了进行说明，不应看作是对实施方案的限制。
实施例
[制备实施例1]
在120～140℃下将8.0摩尔的酚醛清漆类酚醛树脂(羟基当量＝106，HF-1M，Meiwa Plastic Industries Ltd.(日本))完全溶于四颈圆底烧瓶中。在130℃下静置溶液，然后向其中加入0.2摩尔的三苯膦。将混合物充分地搅拌30分钟。将1.0摩尔的3-环氧丙氧丙基三甲氧基硅烷(分子量＝236，KBM-403，Shin-Etsu Chemical Co.，Ltd.(日本))缓慢地滴加到烧瓶中。在130～150℃下，让所得混合物反应4个小时。在反应完成以后，将反应混合物冷却到室温。使用混合器磨碎反应产物，防水存储。在此时，醇作为硅烷偶联剂与酚醛树脂反应的副产物和湿气同时保留在树脂中，并且通过冷凝器使用真空泵将其他的挥发性组分从反应产物中分离出来。
[实施例1～6和对比例1～3]
将制备实施例1中制备的预反应固化树脂用来制备胶粘剂膜组合物(实施例1～6)。将示于表1(实施例1～6)和表2(对比例1～3)中的组分放入到1L的装有高速搅拌器的圆柱形烧瓶中，以4000rpm分散20分钟分别制备胶粘剂膜组合物。使用珠磨机将每种组合物研磨得很细，研磨30分钟。研磨重复至少两次。使用50μm的囊式过滤器过滤粉末，使用涂覆器将其涂敷到经过剥离处理的聚对苯二甲酸乙二醇酯(PET)膜上至厚度为20μm，然后在90～120℃下干燥20分钟获得胶粘剂膜。
表1
Figure G200810161497XD00171
表2
Figure G200810161497XD00181
注释：(1)：羟值＝13mgKOH/g，酸值＝63mgKOH/g，Tg＝38℃，重 均分子量＝690,000，KLS-1045，Fujikura Kasei Co.，Ltd(日本)
(2)：平均分子量＝60,000，E4275，JER
(3)：当量＝205，YDCN-500-4P，Kukdo Chemical Co.，Ltd.(韩国)
(4)：当量＝106，HF-1M，Meiwa Plastic Industries Ltd.(日本)
(5)：TPP，HOKKO
(6)：Aerosil-200，Degussa
(7)：SO-25R，Admatech
(8)：3-环氧丙氧丙基三甲氧基硅烷，KBM-403，Shin-Etsu ChemicalCo.，Ltd.(日本)
(9)：在作为有机溶剂的环己酮中测量
胶粘剂膜的物理性能的评价
对实施例1～6和对比例1～3中所制备的胶粘剂膜的物理性能进行评价，结果显示在表3和表4中。在胶粘剂膜实施完耐软熔性和耐温度循环性测试之后，通过超声波扫描显微镜(SAT)观察胶粘剂膜的分层和裂纹。测量胶粘剂膜的晶粒剪切强度，结果显示在表3和表4中。
(1)挥发性气体含量：将1g的每种膜溶于50g的1，4-二噁烷，静置6个小时，使其通过0.45μm的囊式过滤器获得样品。以500:1的比例在样品中加入作为校准物的乙基卡必醇。通过气相色谱(GC，Agilent5890)以下列条件来测量混合物中挥发性气体的含量：
柱：DB-1(长度＝30m，ID＝0.53mm，膜厚度＝0.88μm)
首次停留时间：3分钟(40℃)，
加热速率：10℃/分钟从40℃至280℃
第二次停留时间：10分钟(280℃)
流动速率：10ml/分钟
结果显示在表3和表4中。
(2)起泡测试：在胶粘剂膜上按照下列程序模拟粘附晶粒和引线接合步骤。首先，将530μm厚的涂有二氧化硅膜的晶圆切割成晶片(大小＝10mmx10mm)，然后在60℃下与每个胶粘剂膜层压。将层压物切割仅仅留下其粘合部分。将玻璃载片(大小＝20mmx20mm)放置到120℃和150℃的热板上之后，将晶片短暂地暴露于相应的玻璃载片一小段时间，从而来评价挥发性组分是否蒸发形成气泡。由于气泡的形成，如果形成的空隙超过膜粘合面积的10％或更多，那么该膜被评定为“差的”。
(3)耐软熔性测试：将每个胶粘剂膜贴在100μm厚的涂有二氧化硅膜的晶圆上，然后切割成具有不同尺寸的晶片(8mmx8mm，10mmx10mm)。将该晶片贴附于MCP封装上以形成双层的结构。在175℃下用环氧模塑化合物(EMC)(SG-8500BC，Cheil Industries(韩国))模塑使最终结构成型60秒，在175℃下二次固化2小时以获得测试片。允许测试片在85℃、85RH％的环境下吸收湿气168个小时，在最高温度260℃下进行三次软熔。然后，使用超声波扫描显微镜(SAT)来观察测试片的分层和裂纹。结果显示在表3和表4中。当观察到15％或更多的测试片分层并开裂时，该测试片被被判为“差”。
(4)晶粒剪切强度：530μm厚的涂有二氧化硅膜的晶圆被切割成5mmx5mm大小的晶片。在60℃下将晶片与各自的胶粘剂膜层压。将每个层压物切割，仅仅留下其粘合部分。将晶片(5mmx5mm)置于较低的晶片(10mmx10mm)之上，在120℃的热板上以1kgf力压1秒钟以使其贴附于较低的晶片上，然后在175℃下固化2个小时。允许所获得的测试片在85℃、85RH％的环境下吸收湿气168个小时，在最高温度260℃下软熔三次。其后，在250℃下以100μm/秒的速率测量上面晶片的晶粒剪切强度。结果显示在表3和表4中。
表3
Figure G200810161497XD00201
表4
Figure G200810161497XD00211
从表3和表4的结果可以看出，与通过直接添加不与酚醛固化树脂预反应的硅烷偶联剂来制备的对比例1～3的胶粘剂膜相比，用与硅烷偶联剂预反应的酚醛固化树脂来制备的实施例1～6的胶粘剂膜显示出低挥发性气体含量和较好的耐软熔性。
起泡测试结果显示，高挥发性气体含量将导致对比例1～3的胶粘剂膜形成较多的气泡。另外，耐软熔性测验结果显示，由于在对比例1～3的胶粘剂膜中有气泡形成，将发生严重的分层现象并且获得较低的晶粒剪切强度。结果，对比例1～3的胶粘剂膜不能获得高的可靠性。
从上面的描述中明显看出，示例性的实施方案的用于半导体装配的胶粘剂膜组合物使用了与硅烷偶联剂预反应的酚醛固化树脂，其用于制备半导体装配的胶粘剂膜。在粘附晶粒、引线接合和烘箱固化过程中在胶粘剂膜中没有观察到空隙和气泡。因此，利用胶粘剂膜组合物可以赋予胶粘剂膜高可靠性。
尽管为了说明目的已经公开了示例性的实施方案，但是本领域的普通技术人员知道到在不脱离如所附的权利要求公开的本发明的范围和实质的情况下，可以有多种修改、添加和代替。

Claims (15)

1.一种用于半导体装配的胶粘剂膜组合物，包含具有羟基、羧基或环氧基的弹性体树脂，成膜树脂，与硅烷偶联剂预反应的酚醛固化树脂，环氧树脂，固化促进剂以及填料。
2.如权利要求1所述的胶粘剂膜组合物，其中基于该组合物的总重量，该组合物含有5～60％重量的弹性体树脂，5～60％重量的成膜树脂，3～25％重量的预反应酚醛固化树脂，5～40％重量的环氧树脂，0.01～10％重量的固化促进剂以及3～60％重量的填料。
3.如权利要求2所述的胶粘剂膜组合物，进一步含有酚醛固化树脂，基于该组合物的总重量，其使用量为该另外的酚醛固化树脂和该预反应酚醛固化树脂用量的和为3～30％重量。
4.如权利要求1所述的胶粘剂膜组合物，其中通过将硅烷偶联剂与酚醛固化树脂以1∶5～100的摩尔比反应来制备该预反应酚醛固化树脂。
5.如权利要求3或4所述的胶粘剂膜组合物，其中该酚醛固化树脂由结构式1表示：
Figure FSB00000802505800011
其中每个R1和R2独立地为C1～C4的烷基或氢原子，a和b各自独立地为0～4，以及n为0～7的整数。
6.如权利要求1所述的胶粘剂膜组合物，其中该固化促进剂由结构式2或3表示：
Figure FSB00000802505800021
其中R1～R8每一个独立地为氢原子、卤素原子或烷基；
7.如权利要求1所述的胶粘剂膜组合物，其中该环氧树脂选自由双酚类环氧树脂、苯酚酚醛清漆类环氧树脂、邻甲酚酚醛清漆类环氧树脂、多官能团环氧树脂、胺类环氧树脂、杂环环氧树脂、取代的环氧树脂、萘酚类环氧树脂和它们的混合物组成的组。
8.如权利要求1或2所述的胶粘剂膜组合物，其中该环氧树脂与该预反应酚醛固化树脂以环氧当量与羟基当量的比为0.6～1.4∶1的比例混合。
9.如权利要求3所述的胶粘剂膜组合物，其中该环氧树脂与该预反应酚醛固化树脂和该另外的酚醛固化树脂以环氧当量与羟基当量的比为0.6～1.4∶1的比例混合。
10.如权利要求1所述的胶粘剂膜组合物，其中该成膜树脂的玻璃化转变温度(Tg)在-30℃～200℃的范围内。
11.如权利要求1所述的胶粘剂膜组合物，其中该填料为无机填料，该无机填料以球形或无定型态存在，尺寸为5nm～10μm。
12.如权利要求1所述的胶粘剂膜组合物，进一步含有偶联剂。
13.一种用于半导体装配的胶粘剂膜，其用权利要求1所述的胶粘剂膜组合物制备而成。
14.含有权利要求13所述胶粘剂膜的划片晶粒粘结膜。
15.一种划片晶粒粘结膜，含有依次层压到基膜上的压敏胶粘剂层和胶粘剂膜层，其中该压敏胶粘剂层含有压敏胶粘剂聚合物粘合剂、紫外线可固化丙烯酸酯和光引发剂，该紫外线可固化丙烯酸酯存在的量相对于100重量份该聚合物粘结剂为20～150重量份，该光引发剂的量相对于100重量份该紫外线可固化丙烯酸酯为0.1～5重量份；并且该胶粘剂膜层为权利要求13所述的胶粘剂膜。
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