CN110431003A - 多层制品的工作寿命改善及其制备方法和用途 - Google Patents
多层制品的工作寿命改善及其制备方法和用途 Download PDFInfo
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- CN110431003A CN110431003A CN201880018734.9A CN201880018734A CN110431003A CN 110431003 A CN110431003 A CN 110431003A CN 201880018734 A CN201880018734 A CN 201880018734A CN 110431003 A CN110431003 A CN 110431003A
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Abstract
本发明提供包含至少一个底部填料膜层的多层制品。在某些方面，还提供改善所述制品的工作寿命稳定性的方法。在某些方面，还提供改善所述制品的储存稳定性的方法。在某些方面，还提供制备所述制品的方法。在某些方面，还提供通过本文所述方法制备的稳定制品。
Description
技术领域
本发明涉及包含至少一个底部填料膜(underfill film)层的多层制品。在某些方面，本发明涉及改善所述制品的工作寿命稳定性的方法。在某些方面，本发明涉及改善所述制品的储存稳定性的方法。在某些方面，本发明涉及制备所述制品的方法。在某些方面，本发明涉及得到的稳定制品。
发明内容
根据本发明，提供包含至少一个底部填料膜层的多层制品。在某些方面，还提供改善所述制品的工作寿命稳定性的方法。在某些方面，还提供改善所述制品的储存稳定性的方法。在某些方面，还提供制备所述制品的方法。在某些方面，还提供通过本文所述方法制备的稳定制品。
在一个方面，预期用于本发明的底部填料膜层包含至少以下组分的组合：
(1)成膜粘合剂树脂，
(2)马来酰亚胺、桥亚甲基四氢邻苯二甲酰亚胺(nadimide)或衣康酰胺(itaconamide)，
(3)丙烯酸酯树脂，和
(4)填料。
在某些实施方案中，预期用于本发明的底部填料膜层组合物还任选地含有环氧树脂。
在某些方面，提供通过本文所述方法制备的稳定制品。
在某些方面，提供包含本文所述底部填料膜的制品。
在某些方面，提供包含第一制品的组件，所述第一制品通过本文所述配制物的固化等分试样与第二制品永久粘附。
附图说明
图1示出了根据本发明的示例性制品的结构，其中层1是隔离衬垫(releaseliner)，层2是底部填料膜，层3是覆盖膜的压敏粘合剂，并且层4是覆盖膜的背衬带(backing tape)。在一些实施方案中，层3和层4一起构成(comprise)覆盖膜层(5)。
图2示出了可迁移组分(6)在底部填料膜(2)与覆盖膜层(3)和(4)之间的迁移。一旦底部填料膜(2)与覆盖膜层(3)和(4)层合，可迁移组分(6)开始在整个组件中分布，导致组件不稳定。初始阶段(左侧图)和结束阶段(右侧图)显示，由于可迁移组分(6)的迁移，底部填料膜具有不同的组成。
图3示出了当经受高温老化时，就可迁移组分(6)的迁移而言，根据本发明的制品的稳定性。不希望受任何理论的束缚，目前认为在至少覆盖膜层(3)和(4)中包含可迁移组分(6)，降低可迁移组分(6)在整个制品中不均匀分布的驱动力，并且显著改变制品各层的化学含量。
具体实施方式
根据本发明，提供包含多个层的制品，其中：
所述多个层中的至少一层包含其中具有可迁移组分的底部填料膜，并且
剩余层中的一个或多个，但不是全部，具有包含在其中的可迁移组分。
如本文所用，术语“可迁移组分”包括引发剂、抑制剂、低分子量分子和低聚物等。
在某些实施方案中，预期用于本发明的底部填料膜具有最多约10重量％的可迁移组分；在某些实施方案中，预期用于本发明的底部填料膜具有最多约9重量％的可迁移组分；在某些实施方案中，预期用于本发明的底部填料膜具有最多约8重量％的可迁移组分；在某些实施方案中，预期用于本发明的底部填料膜具有最多约7重量％的可迁移组分；在某些实施方案中，预期用于本发明的底部填料膜具有最多约6重量％的可迁移组分；在某些实施方案中，预期用于本发明的底部填料膜具有最多约5重量％的可迁移组分；在某些实施方案中，预期用于本发明的底部填料膜具有最多约4重量％的可迁移组分；在某些实施方案中，预期用于本发明的底部填料膜具有最多约3重量％的可迁移组分；在某些实施方案中，预期用于本发明的底部填料膜具有最多约2重量％的可迁移组分；在某些实施方案中，预期用于本发明的底部填料膜具有最多约1重量％的可迁移组分。
在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约0.1ppm至最多约100ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约0.1ppm至最多约80ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约0.1ppm至最多约60ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约0.1ppm至最多约40ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约0.1ppm至最多约20ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约0.1ppm至最多约10ppm的范围内。
在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约1ppm至最多约100ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约1ppm至最多约80ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约1ppm至最多约60ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约1ppm至最多约40ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约1ppm至最多约20ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约1ppm至最多约10ppm的范围内。
在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约5ppm至最多约100ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约5ppm至最多约80ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约5ppm至最多约60ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约5ppm至最多约40ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约5ppm至最多约20ppm的范围内；在某些实施方案中，当可迁移组分存在于任何一层中时，所述可迁移组分的量在约5ppm至最多约10ppm的范围内。
根据本发明的另一实施方案，提供制品，其包含：
第一层，
第二层，以及
第三层，
其中：
所述第一层包含隔离衬垫，
所述第二层包含底部填料膜，所述底部填料膜具有最多约10重量％的可迁移组分，并且
所述第三层包含覆盖膜，所述覆盖膜具有0.1-100ppm的可迁移组分。
在某些实施方案中，预期用于本发明的隔离衬垫包含基本上不与底部填料膜层发生化学相互作用的材料，并且用于防止底部填料膜表面粘结。示例性隔离衬垫包括基于纸或塑料的膜片(film sheets)、基于塑料的材料例如PET、聚烯烃和有机硅等。
在某些实施方案中，本发明预期的覆盖膜包含：
压敏粘合剂层，所述压敏粘合剂层具有最多100ppm的可迁移组分，以及
背衬带，所述背衬带具有最多100ppm的可迁移组分。
预期用于本发明的示例性压敏粘合剂层包括基于丙烯酸类(acrylic)聚合物、橡胶、乙烯-乙酸乙烯酯、腈和苯乙烯嵌段共聚物等的弹性体。
在某些实施方案中，预期用于本发明的背衬带选自聚烯烃、聚酰亚胺、聚酯、聚对苯二甲酸乙二醇酯(PET)或含氟聚合物等。
根据本发明的又一实施方案，提供制品，其包含：
第一层，
第二层，以及
第三层，
其中所述层中的一个或多个具有可迁移组分，
其中：
所述第一层包含隔离衬垫，
所述第二层包含底部填料膜，所述底部填料膜具有最多约10重量％的可迁移组分，并且
所述第三层包括覆盖膜，所述覆盖膜包含两层：
压敏粘合剂层，以及
背衬带，
其中当可迁移组分存在于任何一层中时，所述可迁移组分的量在约0.1ppm至最多约100ppm的范围内。
根据本发明的又一实施方案，提供制备本文所述的任何制品的方法，所述方法包括在所述第三层中添加有效量的一种或多种可迁移组分，以在所述第三层中达到约0.1-100ppm的量。
根据本发明的又一实施方案，提供改善本文所述的任何制品的稳定性的方法，所述方法包括在用所述底部填料膜覆盖所述覆盖膜之前，在所述第三层中添加有效量的一种或多种可迁移组分，以在所述第三层中达到约0.1-100ppm的可迁移组分的量。
根据本发明的某些实施方案，所述制品的储存稳定性得到改善。
根据本发明的其它实施方案，所述制品的工作寿命稳定性得到改善。
在一些实施方案中，上述方法还包括将所述制品暴露于高温老化过程约0.1小时至4周，其中所述温度为20℃至100℃。
预期用于本发明的示例性底部填料膜包含组合物，所述组合物包含：
(i)粘合剂树脂，
(ii)马来酰亚胺、桥亚甲基四氢邻苯二甲酰亚胺或衣康酰亚胺(itaconimide)，
(iii)丙烯酸酯树脂，和
(iv)填料，
以及任选存在的环氧树脂；
其中：
所述粘合剂树脂是成膜高分子量聚合物树脂，其可溶解在溶剂中，并在从其除去溶剂后形成薄膜，
所述马来酰亚胺、桥亚甲基四氢邻苯二甲酰亚胺或衣康酰亚胺是单体的或低聚的，并且可经历自由基固化以形成聚合物网状结构；
所述丙烯酸酯树脂是热固性树脂，其可固化成三维聚合物网状结构；
所述填料调节得到的组合物的热膨胀系数(CTE)；并且
所述任选存在的环氧树脂(或环氧官能化树脂)包括基于双酚A的液体型环氧树脂、基于双酚A的固体型环氧树脂、基于双酚F的液体型环氧树脂、基于苯酚-酚醛清漆树脂的多官能环氧树脂、二环戊二烯型环氧树脂、和萘型环氧树脂等，以及它们中任意两种或更多种的混合物，
其中所述组合物在B阶段具有：
100℃-200℃的差示扫描量热法(DSC)起始温度；
100Pa sec-10,000Pa sec的熔融粘度，以及
100℃-200℃的胶凝温度，如由TA DHR2流变仪在10N轴向力分布下所测量。
预期用于本发明的粘合剂树脂包括一种或多种(甲基)丙烯酸酯、一种或多种环氧树脂、乙烯基醚、乙烯基酯、乙烯基酮、乙烯基芳族化合物、乙烯基环烷基化合物(vinylcycloalkyls)、和烯丙基酰胺等。
预期用于本发明的马来酰亚胺、桥亚甲基四氢邻苯二甲酰亚胺或衣康酰亚胺是分别具有以下结构的化合物：
其中：
m是1-15，
p是0-15，
各R2独立地选自氢或低级烷基(例如C1-5)，并且
J是包含有机基团或有机硅氧烷基团的单价或多价基团，以及
它们中两种或更多种的组合。
在本发明的一些实施方案中，J是选自以下基团的单价或多价基团：
-通常具有约6个至最多约500个碳原子的烃基或取代烃基，其中烃基选自烷基、烯基、炔基、环烷基、环烯基、芳基、烷基芳基、芳基烷基、芳基烯基、烯基芳基、芳基炔基或炔基芳基，然而，条件是仅当J包含两种或更多种不同基团的组合时，J才可以是芳基；
-通常具有约6个至最多约500个碳原子的亚烃基或取代亚烃基，其中亚烃基选自亚烷基、亚烯基、亚炔基、亚环烷基、亚环烯基、亚芳基、烷基亚芳基、芳基亚烷基、芳基亚烯基、烯基亚芳基、芳基亚炔基或炔基亚芳基，
-通常具有约6个至最多约500个碳原子的杂环或取代杂环基团，
-聚硅氧烷，或
-聚硅氧烷-聚氨酯嵌段共聚物，以及
上述基团中的一种或多种与选自以下基团的连接基(linker)的组合：共价键、-O-、-S-、-NR-、-NR-C(O)-、-NR-C(O)-O-、-NR-C(O)-NR-、-S-C(O)-、-S-C(O)-O-、-S-C(O)-NR-、-O-S(O)2-、-O-S(O)2-O-、-O-S(O)2-NR-、-O-S(O)-、-O-S(O)-O-、-O-S(O)-NR-、-O-NR-C(O)-、-O-NR-C(O)-O-、-O-NR-C(O)-NR-、-NR-O-C(O)-、-NR-O-C(O)-O-、-NR-O-C(O)-NR-、-O-NR-C(S)-、-O-NR-C(S)-O-、-O-NR-C(S)-NR-、-NR-O-C(S)-、-NR-O-C(S)-O-、-NR-O-C(S)-NR-、-O-C(S)-、-O-C(S)-O-、-O-C(S)-NR-、-NR-C(S)-、-NR-C(S)-O-、-NR-C(S)-NR-、-S-S(O)2-、-S-S(O)2-O-、-S-S(O)2-NR-、-NR-O-S(O)-、-NR-O-S(O)-O-、-NR-O-S(O)-NR-、-NR-O-S(O)2-、-NR-O-S(O)2-O-、-NR-O-S(O)2-NR-、-O-NR-S(O)-、-O-NR-S(O)-O-、-O-NR-S(O)-NR-、-O-NR-S(O)2-O-、-O-NR-S(O)2-NR-、-O-NR-S(O)2-、-O-P(O)R2-、-S-P(O)R2-或-NR-P(O)R2-；其中各R独立地为氢、烷基或取代烷基。
示例性的组合包括其中J是以下基团的那些：氧基烷基、硫代烷基、氨基烷基、羧基烷基、氧基烯基、硫代烯基、氨基烯基、羧基烯基、氧基炔基、硫代炔基、氨基炔基、羧基炔基、氧基环烷基、硫代环烷基、氨基环烷基、羧基环烷基、氧基环烯基、硫代环烯基、氨基环烯基、羧基环烯基、杂环基、氧基杂环基、硫代杂环基、氨基杂环基、羧基杂环基、氧基芳基、硫代芳基、氨基芳基、羧基芳基、杂芳基、氧基杂芳基、硫代杂芳基、氨基杂芳基、羧基杂芳基、氧基烷基芳基、硫代烷基芳基、氨基烷基芳基、羧基烷基芳基、氧基芳基烷基、硫代芳基烷基、氨基芳基烷基、羧基芳基烷基、氧基芳基烯基、硫代芳基烯基、氨基芳基烯基、羧基芳基烯基、氧基烯基芳基、硫代烯基芳基、氨基烯基芳基、羧基烯基芳基、氧基芳基炔基、硫代芳基炔基、氨基芳基炔基、羧基芳基炔基、氧基炔基芳基、硫代炔基芳基、氨基炔基芳基或羧基炔基芳基、氧基亚烷基、硫代亚烷基、氨基亚烷基、羧基亚烷基、氧基亚烯基、硫代亚烯基、氨基亚烯基、羧基亚烯基、氧基亚炔基、硫代亚炔基、氨基亚炔基、羧基亚炔基、氧基亚环烷基、硫代亚环烷基、氨基亚环烷基、羧基亚环烷基、氧基亚环烯基、硫代亚环烯基、氨基亚环烯基、羧基亚环烯基、氧基亚芳基、硫代亚芳基、氨基亚芳基、羧基亚芳基、氧基烷基亚芳基、硫代烷基亚芳基、氨基烷基亚芳基、羧基烷基亚芳基、氧基芳基亚烷基、硫代芳基亚烷基、氨基芳基亚烷基、羧基芳基亚烷基、氧基芳基亚烯基、硫代芳基亚烯基、氨基芳基亚烯基、羧基芳基亚烯基、氧基烯基亚芳基、硫代烯基亚芳基、氨基烯基亚芳基、羧基烯基亚芳基、氧基芳基亚炔基、硫代芳基亚炔基、氨基芳基亚炔基、羧基芳基亚炔基、氧基炔基亚芳基、硫代炔基亚芳基、氨基炔基亚芳基、羧基炔基亚芳基、亚杂芳基、氧基亚杂芳基、硫代亚杂芳基、氨基亚杂芳基、羧基亚杂芳基、含杂原子的二价或多价环状部分、含氧基杂原子的二价或多价环状部分、含硫代杂原子的二价或多价环状部分、含氨基杂原子的二价或多价环状部分、或者含羧基杂原子的二价或多价环状部分。
预期用于本发明的环氧树脂包括其上具有一个或多个环氧基团的聚合物主链。多种环氧官能化树脂预期用于本发明，例如基于双酚A的液体型环氧树脂、基于双酚A的固体型环氧树脂、基于双酚F的液体型环氧树脂(例如Epiclon EXA-835LV)、酚醛清漆环氧树脂、基于苯酚-酚醛清漆树脂的多官能环氧树脂、二环戊二烯型环氧树脂(例如Epiclon HP-7200L)、萘型环氧树脂、硅氧烷改性环氧树脂、脂环族环氧树脂、联苯环氧树脂、和改性环氧树脂等，以及它们中任意两种或更多种的组合。
预期用于本发明的示例性环氧官能化树脂包括脂环族醇的二环氧化物、氢化双酚A(市售为Epalloy 5000)、六氢邻苯二甲酸酐的二官能脂环族缩水甘油酯(市售为Epalloy5200)、Epiclon EXA-835LV、和Epiclon HP-7200L等，以及它们中任意两种或更多种的混合物。
在某些实施方案中，环氧组分可包括两种或更多种不同的基于双酚的环氧树脂的组合。这些基于双酚的环氧树脂可选自双酚A环氧树脂、双酚F环氧树脂或双酚S环氧树脂，或它们的组合。此外，可使用同一类型树脂(例如A、F或S)中的两种或更多种不同的双酚环氧树脂。
预期用于本发明的双酚环氧树脂的市售实例包括双酚F型环氧树脂(例如来自日本Nippon Kayaku的RE-404-S，以及来自Dai Nippon Ink&Chemicals,Inc.的EPICLON 830(RE1801)、830S(RE1815)、830A(RE1826)和830W，以及来自Resolution的RSL 1738和YL-983U)和双酚A型环氧树脂(例如来自Resolution的YL-979和980)。
上面提到的可从Dai Nippon商购的双酚环氧树脂被宣传为液体的未稀释的表氯醇-双酚F环氧树脂，其粘度比基于双酚A环氧树脂的常规环氧树脂低得多，并且具有类似于液体双酚A环氧树脂的物理性质。双酚F环氧树脂比双酚A环氧树脂具有更低的粘度，这两种环氧树脂之间的所有其它方面都相同，这提供了更低的粘度，从而提供了快速流动的底部填料密封剂材料。这四种双酚F环氧树脂的EEW为165-180。25℃的粘度为3,000cps至4,500cps(RE1801除外，其粘度上限为4,000cps)。据报道，RE1815和830W的可水解氯化物含量为200ppm，RE1826的可水解氯化物含量为100ppm。
上面提到的可从Resolution商购的双酚环氧树脂被宣传为低氯化物含量的液体环氧树脂。双酚A环氧树脂的EEW(g/eq)为180-195，25℃的粘度为100cps至250cps。据报道，YL-979的总氯化物含量为500ppm至700ppm，YL-980的总氯化物含量为100ppm至300ppm。双酚F环氧树脂的EEW(g/eq)为165-180，25℃的粘度为30cps至60cps。据报道，RSL-1738的总氯化物含量为500ppm至700ppm，YL-983U的总氯化物含量为150ppm至350ppm。
除了双酚环氧树脂之外，预期其它环氧化合物也可用作本发明配制物的环氧组分。例如，可以使用脂环族环氧树脂，例如3,4-环氧基环己基甲基-3,4-环氧基环己基碳酸酯。单官能、二官能或多官能反应性稀释剂也可用于调节所得树脂材料的粘度和/或降低所得树脂材料的Tg。示例性反应性稀释剂包括丁基缩水甘油醚、甲酚缩水甘油醚、聚乙二醇缩水甘油醚、和聚丙二醇缩水甘油醚等。
适用于本发明的环氧树脂包括酚类化合物的聚缩水甘油基衍生物，例如可以商品名EPON购得的那些，例如来自Resolution的EPON 828、EPON 1001、EPON 1009和EPON 1031；来自Dow Chemical Co.的DER 331、DER 332、DER 334和DER 542，以及来自Nippon Kayaku的BREN-S。其它合适的环氧树脂包括由多元醇等制备的聚环氧化物和酚醛清漆的聚缩水甘油基衍生物，后者例如来自Dow Chemical的DEN 431、DEN 438和DEN 439。甲酚类似物也可以商品名ARALDITE购得，例如来自Ciba Specialty Chemicals Corporation的ARALDITEECN 1235、ARALDITE ECN 1273和ARALDITE ECN 1299。SU-8是可从Resolution购得的双酚A型环氧酚醛清漆。胺、氨基醇和聚羧酸的聚缩水甘油基加合物也可用于本发明，其市售树脂包括来自F.I.C.Corporation的GLYAMINE 135、GLYAMINE 125和GLYAMINE 115；来自CibaSpecialty Chemicals的ARALDITE MY-720、ARALDITE 0500和ARALDITE 0510；以及来自Sherwin-Williams Co.的PGA-X和PGA-C。
本发明任选使用的合适的单官能环氧共反应物稀释剂包括粘度低于环氧组分粘度的稀释剂，所述稀释剂的粘度通常小于约250cps。
单官能环氧共反应物稀释剂应该具有环氧基，所述环氧基带有约6个至约28个碳原子的烷基，其实例包括C6-28烷基缩水甘油醚、C6-28脂肪酸缩水甘油酯、和C6-28烷基酚缩水甘油醚等。
如果包含这种单官能环氧共反应物稀释剂，则基于组合物的总重量，这种共反应物稀释剂的用量应为约0.5重量％至约10重量％；在一些实施方案中，基于组合物的总重量，这种共反应物稀释剂的用量应为约0.25重量％至约5重量％。
环氧组分在组合物中的存在量应在约1重量％至约20重量％的范围内；在一些实施方案中，本发明的配制物包含约2重量％至约18重量％的环氧树脂；在一些实施方案中，本发明的配制物包含约5重量％至约15重量％的环氧树脂。
在一些实施方案中，本文所用的环氧组分是硅烷改性的环氧树脂，例如包括以下物质的组成：
(A)包括在以下结构中的环氧组分：
其中：
Y可以存在也可以不存在，并且当Y存在时，其为直接键、CH2、CH(CH3)2、C＝O、或S，
这里的R1是烷基、烯基、羟基、羧基和卤素，并且
这里的x是1-4；
(B)包括在以下结构中的环氧官能化烷氧基硅烷：
R1-Si(OR2)3
其中
R1是含环氧乙烷的部分，并且
R2是具有1至10个碳原子的烷基或烷氧基取代烷基、芳基或芳烷基；以及
(C)组分(A)与(B)的反应产物。
一种这样的硅烷改性的环氧树脂的实例是作为芳族环氧树脂(例如双酚A、双酚E、双酚F或双酚S环氧树脂或者联苯基环氧树脂)与环氧硅烷的反应产物形成的，其中环氧硅烷包括在以下结构中：
R1-Si(OR2)3
其中
R1是含环氧乙烷的部分，其实例包括2-(乙氧基甲基)环氧乙烷、2-(丙氧基甲基)环氧乙烷、2-(甲氧基甲基)环氧乙烷和2-(3-甲氧基丙基)环氧乙烷，并且
R2是具有1至10个碳原子的烷基或烷氧基取代的烷基、芳基或芳烷基。
在一个实施方案中，R1是2-(乙氧基甲基)环氧乙烷，R2是甲基。
用于制备硅烷改性的环氧树脂的芳族环氧树脂的理想化结构包括
其中
Y可以存在也可以不存在，并且当Y存在时，其为直接键、CH2、CH(CH3)2、C＝O、或S，
R1是烷基、烯基、羟基、羧基或卤素，并且
x是1-4。
当然，当x为2-4时，芳族环氧树脂的扩链形式也被认为包括在该结构中。
例如，芳族环氧树脂的扩链形式可包括在以下结构中：
在一些实施方案中，硅氧烷改性的环氧树脂具有以下结构：
-(O-Si(Me)2-O-Si(Me)(Z)-O-Si(Me)2-O-Si(Me)2)n-
其中：
Z是-O-(CH2)3-O-Ph-CH2-Ph-O-(CH2-CH(OH)-CH2-O-Ph-CH2-Ph-O-)n-CH2-环氧乙烷，并且
n在约1-4的范围内。
在一些实施方案中，硅氧烷改性的环氧树脂通过使以下组分的组合在适合促进其反应的条件下接触来制备：
其中“n”在约1-4的范围内。
硅烷改性的环氧树脂也可以是芳族环氧树脂、环氧硅烷、以及芳族环氧树脂与环氧硅烷的反应产物的组合。反应产物可以由重量比为1:100至100:1，例如重量比为1:10至10:1的芳族环氧树脂和环氧硅烷制备。
预期用于本发明组合物中的一种或多种环氧单体的量是足够的，使得所得配制物包含约1-40重量％的所述环氧树脂。在某些实施方案中，所得配制物包含约2-30重量％的所述环氧树脂。在某些实施方案中，所得配制物包含约5-20重量％的所述环氧树脂。
环氧固化剂(epoxy cure agents)任选地与环氧单体组合使用。示例性环氧固化剂包括脲、脂族和芳族胺、胺硬化剂、聚酰胺、咪唑、双氰胺、酰肼、脲-胺混合固化体系、自由基引发剂(例如过氧化酯、过氧碳酸盐、氢过氧化物、烷基过氧化物、芳基过氧化物、和偶氮化合物等)、有机碱、过渡金属催化剂、酚、酸酐、路易斯酸、和路易斯碱等。
当环氧固化剂存在时，本发明组合物包含约0.1-2重量％的环氧固化剂。在某些实施方案中，本发明组合物包含约0.5-5重量％的环氧固化剂。
任选地，一种或多种额外单体或由其衍生的树脂可以存在于本发明配制物中，例如氰酸酯、有机硅、氧杂环丁烷、聚酯、聚氨酯、聚酰亚胺、三聚氰胺、脲甲醛、酚醛树脂等。当存在时，基于最终配制物的总重量，这种材料可以在约0.1重量％至最多约60重量％的范围内存在。
当存在氰酸酯单体时，预期用于本发明实践的氰酸酯单体含有两个或更多个成环氰酸酯(-O-C≡N)基团，这些氰酸酯基团在加热时环化三聚而形成取代的三嗪环。由于氰酸酯单体固化期间没有形成离去基团或挥发性副产物，因此固化反应被称为加成聚合。可用于本发明实践的合适的聚氰酸酯单体包括例如1,1-双(4-氰酰(cyanato)苯基)甲烷、1,1-双(4-氰酰苯基)乙烷、2,2-双(4-氰酰苯基)丙烷、双(4-氰酰苯基)-2,2-丁烷、1,3-双[2-(4-氰酰苯基)丙基]苯、双(4-氰酰苯基)醚、4,4’-二氰酰二苯基、双(4-氰酰-3,5-二甲基苯基)甲烷、三(4-氰酰苯基)乙烷、氰化酚醛清漆、1,3-双[4-氰酰苯基-1-(1-甲基亚乙基)]苯、和氰化酚二环戊二烯加合物等。根据本发明使用的聚氰酸酯单体可以通过在酸受体存在下使合适的二元或多元酚与卤化氰反应而容易地制备。
根据本发明，可任选地与一种或多种聚氰酸酯单体组合的单体选自那些经历加成聚合的单体。这种单体包括乙烯基醚、二乙烯基醚、二烯丙基醚、二甲基丙烯酸酯、二炔丙基醚、混合炔丙基烯丙基醚、单马来酰亚胺、和双马来酰亚胺等。这种单体的实例包括环己烷二甲醇单乙烯基醚、三烯丙基氰尿酸酯、1,1-双(4-烯丙氧基苯基)乙烷、1,1-双(4-炔丙氧基苯基)乙烷、1,1-双(4-烯丙氧基苯基-4’-炔丙氧基苯基)乙烷、3-(2,2-二甲基三亚甲基缩醛)-1-马来酰亚胺基苯、2,2,4-三甲基六亚甲基-1,6-双马来酰亚胺、和2,2-双[4-(4-马来酰亚胺基苯氧基)苯基]丙烷等。
预期用于本发明实践的其它氰酸酯是本领域众所周知的。参见例如美国专利第5,718,941号，其全部内容通过引用并入本文中。
当存在有机硅时，预期用于本发明实践的有机硅是本领域众所周知的。参见例如美国专利第5,717,034号，其全部内容通过引用并入本文中。
当存在氧杂环丁烷(即1,3-环氧丙烷)时，它是分子式为C3H6O的具有含3个碳原子和1个氧原子的四元环的杂环有机化合物。术语氧杂环丁烷通常也指含有氧杂环丁烷环的任何有机化合物。参见例如Burkhard等人，Angew.Chem.Int.Ed.2010,49,9052-9067，其全部内容通过引用并入本文中。
当存在聚酯时，预期用于本发明实践的聚酯是指通过多元醇(polyol，也称为多元醇(polyhydric alcohol))与饱和或不饱和二元酸反应形成的缩聚物。使用的典型多元醇是二醇，例如乙二醇；常用的酸是邻苯二甲酸和马来酸。水是酯化反应的副产物，不断被除去，推动反应完成。不饱和聚酯和添加剂例如苯乙烯的使用降低树脂的粘度。最初的液体树脂通过交联链转化为固体。这是通过在不饱和键处产生自由基来实现的，所述自由基在链反应中传播到相邻分子中的其它不饱和键，从而在该过程中连接相邻的链。
当存在聚氨酯时，预期用于本发明实践的聚氨酯是指由通过氨基甲酸酯(carbamate，或氨基甲酸乙酯(urethane))键连接的有机单元链组成的聚合物。聚氨酯聚合物通过使异氰酸酯与多元醇反应而形成。用于制备聚氨酯的异氰酸酯和多元醇平均每个分子含有两个或更多个官能团。
当存在聚酰亚胺时，预期用于本发明实践的聚酰亚胺是指由通过酰亚胺键连接的有机单元链组成的聚合物(即-C(O)-N(R)-C(O)-)。聚酰亚胺聚合物可以通过多种反应形成，即通过二酐与二胺的反应、二酐与二异氰酸酯的反应等。
当存在三聚氰胺时，预期用于本发明实践的三聚氰胺是指由三聚氰胺(即1,3,5-三嗪-2,4,6-三胺)与甲醛通过聚合制成的硬质热固性塑料材料。在其丁基化形式中，它可以溶解在正丁醇和/或二甲苯中。它可用于与其它树脂(例如醇酸树脂、环氧树脂、丙烯酸类树脂和聚酯树脂)交联。
当存在脲甲醛时，预期用于本发明实践的脲甲醛是指由脲和甲醛，在弱碱例如氨或吡啶的存在下加热制成的不透明热固性树脂或塑料。
当存在酚醛树脂时，预期用于本发明实践的酚醛树脂是指通过苯酚或取代苯酚与甲醛反应获得的合成聚合物。
预期用于本发明的增韧剂是增强引入它们的配制物的抗冲击性的添加剂。示例性增韧剂包括表氯醇与双酚A的中等至高分子量热塑性聚合物，例如苯氧基树脂，其具有多羟基醚的结构，并且具有末端羟基以及沿其主链的重复羟基。一种这样的增韧剂是具有以下结构的苯氧基树脂：
其中n在约50至最多约150的范围内。
预期用于本发明实践的颗粒填料包括二氧化硅、硅酸钙、氢氧化铝、氢氧化镁、碳酸钙、碳酸镁、氧化铝(Al2O3)、氧化锌(ZnO)、氧化镁(MgO)、氮化铝(AIN)、氮化硼(BN)、碳纳米管、金刚石、粘土、和铝硅酸盐等，以及它们中任意两种或更多种的混合物。在一些实施方案中，颗粒填料是二氧化硅。
通常，本发明配制物中使用的填料的粒径在约0.005μm(即5nm)至最多约20μm的范围内。在某些实施方案中，本文使用的填料的粒径在约0.1μm至最多约5μm的范围内。
根据本发明的组合物包含约30-75重量％的所述颗粒填料。在一些实施方案中，根据本发明的组合物包含约40-60重量％的所述颗粒填料。
本发明组合物可任选地进一步包含约0.2-2重量％的自由基聚合引发剂。在某些实施方案中，本发明组合物可进一步包含约0.2-1重量％的自由基聚合引发剂。
示例性自由基引发剂包括过氧化酯、过氧碳酸盐、氢过氧化物、烷基过氧化物、芳基过氧化物、和偶氮化合物等。
本发明组合物任选地进一步包含一种或多种流动添加剂、粘合促进剂、流变改性剂、助熔剂、膜增韧剂、环氧固化催化剂(例如咪唑)、固化剂(例如自由基引发剂，例如过氧化二异丙苯)、自由基聚合调节剂(例如8-羟基喹啉)和/或自由基稳定剂，以及它们中任意两种或更多种的混合物。
如本文所用，术语“流动添加剂”是指改变引入它们的配制物的粘度的化合物。赋予这种性质的示例性化合物包括含硅聚合物、丙烯酸乙酯/丙烯酸2-乙基己酯共聚物、和酮肟磷酸酯的烷醇铵盐等，以及它们中任意两种或更多种的组合。
如本文所用，术语“粘合促进剂”是指增强引入它们的配制物的粘合性质的化合物。
如本文所用，术语“流变改性剂”是指改变引入它们的配制物的一种或多种物理性质的添加剂。
如本文所用，术语“助熔剂”是指防止熔融金属表面上形成氧化物的还原剂。通常，助熔剂：
-与金属表面上的氧化物反应，促进熔融金属的润湿，以及
-通过涂覆热表面来充当氧气屏障，防止热表面氧化。
示例性助熔剂包括羧酸、醇、多元醇、羟基酸、羟基碱等。
示例性羧酸包括松香胶、十二烷二酸(可作为Corfree M2从Aldrich购得)、己二酸、癸二酸、聚癸二酸酐、马来酸、酒石酸、和柠檬酸等。助熔剂也可以包括醇、羟基酸和羟基碱。示例性助熔材料包括多元醇(例如乙二醇、甘油、3-[双(缩水甘油氧基甲基)甲氧基]-1,2-丙二醇、D-核糖、D-纤维二糖、纤维素、和3-环己烯-1,1-二甲醇等。
在一些实施方案中，预期用于本发明的助熔剂是多元醇。
在一些实施方案中，预期用于本发明的助熔剂是羟基喹啉或羟基喹啉衍生物。通常，本发明配制物的酸性足以起到助熔剂的作用，但不会酸性大到导致过早胶凝或腐蚀。组合物还显示出比不含羟基喹啉或羟基喹啉衍生物的类似组合物更高的Tg值。
如本文所用，术语“自由基稳定剂”是指诸如以下的化合物：氢醌、苯醌、受阻酚、受阻胺(例如基于硫代羰基硫的化合物)、基于苯并三唑的紫外线吸收剂、基于三嗪的紫外线吸收剂、基于二苯甲酮的紫外线吸收剂、基于苯甲酸酯的紫外线吸收剂、基于受阻胺的紫外线吸收剂、和基于氮氧自由基(nitroxide radical)的化合物等，以及它们中任意两种或更多种的组合。
当存在时，本发明组合物包含约0.1-1重量％的所述自由基稳定剂。在一些实施方案中，本发明组合物包含约0.1-0.6重量％的所述自由基稳定剂。
本发明组合物也可以任选地含有一种或多种稀释剂。当存在稀释剂时，相对于总组合物，本发明组合物包含约10-80重量％的稀释剂。在某些实施方案中，本发明组合物包含约20-70重量％的稀释剂。
当存在稀释剂时，预期用于本发明的示例性稀释剂包括芳香烃(例如苯、甲苯、和二甲苯等)、饱和烃(例如己烷、环己烷、庚烷、十四烷)、氯化烃(例如二氯甲烷、氯仿、四氯化碳、二氯乙烷、和三氯乙烯等)、醚(例如乙醚、四氢呋喃、二噁烷、二醇醚、乙二醇单烷基或二烷基醚等)、多元醇(例如聚乙二醇、丙二醇、和聚丙二醇等)、酯(例如乙酸乙酯、乙酸丁酯、和乙酸甲氧基丙酯等)、二元酯、α-松油醇、β-松油醇、煤油、邻苯二甲酸二丁酯、丁基卡必醇、丁基卡必醇乙酸酯、卡必醇乙酸酯、乙基卡必醇乙酸酯、己二醇、高沸点醇及其酯、二醇醚、酮(例如丙酮、和甲基乙基酮等)、酰胺(例如二甲基甲酰胺、和二甲基乙酰胺等)、杂芳族化合物(例如N-甲基吡咯烷酮等)等，以及它们中任意两种或更多种的混合物。
预期用于本发明的含羟基的稀释剂包括水和具有C1至最多约C10主链的含羟基化合物。示例性的含羟基的稀释剂包括水、甲醇、乙醇、丙醇、乙二醇、丙二醇、甘油、和松油醇等，以及它们中任意两种或更多种的混合物。
根据本发明预期使用的含羟基的稀释剂的量可以在宽范围内变化，通常在组合物的约5重量％至最多约80重量％的范围内。在某些实施方案中，含羟基的稀释剂的量在总组合物的约10重量％至最多60重量％的范围内。在一些实施方案中，含羟基的稀释剂的量在总组合物的约20重量％至最多约50重量％的范围内。
任选地，本文所述的组合物可包含流动添加剂等。本文预期任选使用的流动添加剂包括含硅聚合物、丙烯酸乙酯/丙烯酸2-乙基己酯共聚物、和酮肟磷酸酯的烷醇铵盐等，以及它们中任意两种或更多种的组合。
预期用于本发明的示例性底部填料膜层通常包含：
至少5重量％的所述粘合剂树脂，
至少5重量％的所述马来酰亚胺、桥亚甲基四氢邻苯二甲酰亚胺或衣康酰亚胺，
至少1重量％的所述丙烯酸酯树脂，和
至少10重量％的所述填料。
在一些实施方案中，底部填料膜层可以进一步包含：
最多40重量％的环氧树脂，
至少0.1重量％的助熔剂，和/或
至少0.1重量％的粘合促进剂。
在一些实施方案中，底部填料膜层包含：
约5重量％至最多40重量％的所述粘合剂树脂，
约5重量％至最多25重量％的所述马来酰亚胺、桥亚甲基四氢邻苯二甲酰亚胺或衣康酰亚胺，
约1重量％至最多40重量％的所述丙烯酸酯树脂，和
约10重量％至最多80重量％的所述填料。
这种组合物可以进一步包含：
最多40重量％的环氧树脂，
至少0.1重量％至最多约10重量％的助熔剂，和/或
至少0.1重量％至最多约5重量％的粘合促进剂。
根据本发明的另一实施方案，提供包含根据本发明的固化组合物的反应产物的底部填料膜。
当暴露于85℃和85％相对湿度下约2天时，根据本发明的底部填料膜通常吸收小于2重量％的水分；在一些实施方案中，当暴露于85℃和85％相对湿度下约2天时，根据本发明的底部填料膜通常吸收小于1.5重量％的水分；在一些实施方案中，当暴露于85℃和85％相对湿度下约2天时，根据本发明的底部填料膜通常吸收小于1.2重量％的水分；在一些实施方案中，当暴露于85℃和85％相对湿度下约2天时，根据本发明的底部填料膜通常吸收小于1.0重量％的水分。
根据本发明的底部填料膜，在固化后当在B阶段时，通过力学热分析(TMA)测定的Tg高于约80℃。
根据本发明的底部填料膜的特征还在于在260℃具有至少2.5N/mm2的芯片剪切(die shear，如用SiN芯片/PI芯片/SiO2(尺寸：3×3×700mm3)所测试)，其中将芯片以120℃/1kg力/5秒贴附在BT基材上，然后通过在30分钟内将温度从室温升高到175℃而固化，然后在175℃保持6小时。
根据本发明的另一实施方案，提供制备底部填料膜的方法，所述方法包括在将如本文所述的组合物施加到合适的基材之后使所述组合物固化。
根据本发明的又一实施方案，提供包含如本文所述的底部填料膜的制品，所述底部填料膜粘合至合适的基材。
预期用于本发明的合适基材包括聚对苯二甲酸乙二醇酯、聚甲基丙烯酸甲酯、聚乙烯、聚丙烯、聚碳酸酯、环氧树脂、聚酰亚胺、聚酰胺、聚酯、玻璃、具有氮化硅钝化的Si芯片、具有聚酰亚胺钝化的Si芯片、BT基材、裸Si、SR4基材、和SR5基材等。
在本发明制品中，所述底部填料膜与所述基材的粘附力通常至少为2.5N/mm2，如用SiN芯片/PI芯片/SiO2(尺寸：3×3×700mm3)所测试，其中将芯片以120℃/1kg力/5秒贴附在BT基材上，然后通过在30分钟内将温度从室温升高到175℃而固化，然后在175℃保持6小时。
可以使用本发明的材料制备多种制品，包括例如倒装芯片(flip chip)封装、层叠芯片、混合存储立方体(hybrid memory cubes)、TSV器件等。
本发明的各个方面通过以下非限制性实施例来说明。这些实施例是为了说明的目的，而不是对本发明的任何实践的限制。应当理解，在不脱离本发明的精神和范围的情况下，可以进行变化和修改。本领域普通技术人员知道如何合成或商业获得本文所述的试剂和组分。
实施例
如表1中所总结的，制备了几种根据本发明的制品，表1给出了代表性的底部填料膜材料配制物，其中所述配制物中具有可迁移的小分子，例如引发剂和抑制剂。
表1
对上述每种制品进行性能测试，测试结果列于表2中。
表2给出了实施例#1中所述的底部填料膜的结果，并且显示除了表现出相对稳定的熔融粘度之外，还基于诸如DSC起始温度、峰值温度、起始温度与峰值温度之间的ΔT、和反应热的测量，本发明制品获得了稳定的材料性质。
表2
除了本文示出和描述的修改之外，本发明的各种修改对于以上描述的领域的技术人员来说是显而易见的。这种修改也意欲包括在所附权利要求的范围内。
说明书中提到的专利和出版物表明了本发明所属领域技术人员的水平。这些专利和出版物通过引用并入本文中，其程度如同每个单独的申请或出版物具体和单独地通过引用并入本文中。
前面的描述是对本发明具体实施方案的说明，而不意味着对本发明实践的限制。后面的权利要求，包括其所有等同物，旨在限定本发明的范围。
Claims (18)
1.制品，其包含多个层，其中：
所述多个层中的至少一层包含其中具有可迁移组分的底部填料膜，并且
剩余层中的一个或多个，但不是全部，具有包含在其中的可迁移组分。
2.根据权利要求1所述的制品，其中所述可迁移组分选自引发剂或抑制剂。
3.根据权利要求1所述的制品，其中所述底部填料膜具有最多约10重量％的可迁移组分。
4.根据权利要求1所述的制品，其中当所述可迁移组分存在于任何一层中时，所述可迁移组分的量在约0.1ppm至最多约100ppm的范围内。
5.制品，其包含：
第一层，
第二层，以及
第三层，
其中：
所述第一层包含隔离衬垫，
所述第二层包含底部填料膜，所述底部填料膜具有最多约10重量％的可迁移组分，并且
所述第三层包含覆盖膜，所述覆盖膜具有0.1-100ppm的可迁移组分。
6.根据权利要求5所述的制品，其中所述覆盖膜包含：
压敏粘合剂层，所述压敏粘合剂层具有最多100ppm的可迁移组分，以及
背衬带，所述背衬带具有最多100ppm的可迁移组分。
7.根据权利要求6所述的制品，其中所述背衬带选自聚烯烃、聚酰亚胺、聚酯、聚对苯二甲酸乙二醇酯(PET)或含氟聚合物。
8.制品，其包含：
第一层，
第二层，以及
第三层，
其中所述层中的一个或多个具有可迁移组分，
其中：
所述第一层包含隔离衬垫，
所述第二层包含底部填料膜，所述底部填料膜具有最多约10重量％的可迁移组分，并且
所述第三层包含覆盖膜，所述覆盖膜包含两层：
压敏粘合剂层，以及
背衬带，
其中当可迁移组分存在于任何一层中时，所述可迁移组分的量在约0.1ppm至最多约100ppm的范围内。
9.制备根据权利要求1所述的制品的方法，所述方法包括在所述第三层中添加有效量的一种或多种可迁移组分，以在所述第三层中达到约0.1-100ppm的量。
10.根据权利要求9所述的方法，其还包括将所述制品暴露于高温老化过程约0.1小时至4周，其中所述温度为20℃至100℃。
11.制备根据权利要求5所述的制品的方法，所述方法包括在所述第三层中添加有效量的一种或多种可迁移组分，以在所述第三层中达到约0.1-100ppm的量。
12.制备根据权利要求8所述的制品的方法，所述方法包括在所述第三层中添加有效量的一种或多种可迁移组分，以在所述第三层中达到约0.1-100ppm的量。
13.改善根据权利要求1所述的制品的稳定性的方法，所述方法包括在用所述底部填料膜覆盖所述覆盖膜之前，在所述第三层中添加有效量的一种或多种可迁移组分，以在所述第三层中达到约0.1-100ppm的可迁移组分的量。
14.根据权利要求13所述的方法，其中所述制品的储存稳定性得到改善。
15.根据权利要求13所述的方法，其中所述制品的工作寿命稳定性得到改善。
16.根据权利要求13所述的方法，其进一步包括将所述制品暴露于高温老化过程约0.1小时至4周，其中所述温度为20℃至100℃。
17.改善根据权利要求5所述的制品的稳定性的方法，所述方法包括在用所述底部填料膜覆盖所述覆盖膜之前，在所述第三层中添加有效量的一种或多种可迁移组分，以在所述第三层中达到约0.1-100ppm的可迁移组分的量。
18.改善根据权利要求8所述的制品的稳定性的方法，所述方法包括在用所述底部填料膜覆盖所述覆盖膜之前，在所述第三层中添加有效量的一种或多种可迁移组分，以在所述第三层中达到约0.1-100ppm的可迁移组分的量。
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