CN102066487A - 流动可控的可b阶化组合物 - Google Patents

流动可控的可b阶化组合物 Download PDF

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CN102066487A
CN102066487A CN2009801225423A CN200980122542A CN102066487A CN 102066487 A CN102066487 A CN 102066487A CN 2009801225423 A CN2009801225423 A CN 2009801225423A CN 200980122542 A CN200980122542 A CN 200980122542A CN 102066487 A CN102066487 A CN 102066487A
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J·沙阿
J·范
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Henkel Corp
National Starch and Chemical Investment Holding Corp
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Abstract

描述的是用于在电子封装件组装期间进行流动控制的可B阶化介电组合物。该可B阶化组合物包括树脂基体和流动控制剂。所述可B阶化组合物对用于电子器件和电子元件的层压基底是特别有用的，其中所述组合物的流动性能在组装期间必须被严格控制。

Description

流动可控的可B阶化组合物
技术领域
本发明涉及可B阶化组合物，其中在电子封装件组装期间B阶化组合物的流动特征可被控制。
背景技术
导电的和绝缘的可B阶化材料常用于电子组装，这是由于它们提供数种处理优势并且容易在粘贴材料上应用。可B阶化材料可被用于基底并干燥(B阶化)成为B阶化膜。可选地，可B阶化材料可被用于膜载体并且可在膜载体上B阶化。然后这种膜可以被切成特定的尺寸并用于印刷电路板和柔性印刷电路基底。随后B阶化膜可以被活化，随之材料流动并变粘以将电子元件粘附至基底。
组装电子封装件经常需要B阶化材料以进行后续处理步骤。后续的组装一般包括用导电材料填充导孔(vias)，细节距的金线键合和焊接。由于一些后续步骤需要热，B阶化材料可能流出到封装件的其它区域上。
随着更小更精密的电子元件的出现，组装封装件的总体尺寸得到下降。在后续组装步骤期间，B阶化材料必须保持在适当的位置而不流到封装件的其它区域上。B阶化材料的过量流动可能污染封装件的其它部分，导致封装件较差的功能性和产量。
控制流动的一种方法是使用高分子量树脂作为可B阶化材料。但是，使用这种高分子量树脂需要更高的活化条件以使粘性(tack)和粘合最优化。高活化条件(如高温和/或高压)是不期望的，这是因为高活化条件将造成更高的成本和更多的封装故障。但是，在低活化条件，高分子量树脂基B阶化材料不能显现粘性，这导致元件与基底间差的粘合性。
控制流动特征的另一方法是在可B阶化材料中添加触变剂(如硅石、粘土、云母、滑石、氧化铝等填料)。尽管触变性在室温下增强了，但在后续的组装步骤中流动并不能得到良好控制，特别是在更高温度下。而且，使用触变剂可造成分离或不一致的粘合层，特别是在窄的粘合层中。
引入间隔珠(spacer beads)是控制可B阶化材料的流动的另一常用方法。这样的方法需要间隔珠保持悬浮；但是间隔珠倾向于下沉，这造成不均匀的分布和不一致的粘合层。
在本领域内仍然需要在组装期间提供强的粘合性和流动控制的可B阶化组合物。本发明致力于该需要。
发明内容
本发明是可B阶化介电组合物，其中加入流动控制剂允许在电子封装件组装期间进行流动控制。该可B阶化组合物可以形成为层压材料，并且其在层压电子基底中特别有用。一些电子基底需要层压材料以仅保持在基底的特定区域中，因为同一基底的其它区域必须保持无污染物。如果层压材料侵入基底的无污染物区域，其可能造成电子器件故障。
可B阶化组合物作为层压材料可被B阶化。活化后，或在层压条件下，层压材料显示出粘性，这允许层压材料粘附至基底，但基本上不流动并保持在其位置。即使在需要高热的后续组装步骤中，层压材料也基本上不流动并保持在其位置。因此，使用所述可B阶化组合物，产生了高产量和良好功能性的电子封装件。
一个实施方式涉及包括树脂基体和流动控制剂的可B阶化组合物。
在另一实施方式中，可B阶化组合物包括树脂基体、流动控制剂以及任选的催化剂、填料、消泡剂和促粘剂。
在进一步的实施方式中，在封装件组装步骤期间，由可B阶化组合物形成的B阶化膜显现粘性，但基本上不流动。
在仍有另一实施方式中，可B阶化组合物的树脂基体包含树脂、固化剂和溶剂。
在进一步的实施方式中，可B阶化组合物的流动控制剂包含核壳聚合物、嵌段共聚物及其混合物。
组合物的另一实施方式涉及沉积在基底上的B阶化膜，其中在封装件组装步骤期间，该B阶化膜显示出粘性但基本上不流动。
在进一步的实施方式中，基底包括具有穿孔、导孔、洞、掩膜、I/O输入和类似物的区域/部件，其需要在组装步骤期间基本上不与可B阶化组合物接触。
仍有另一实施方式涉及使用可B阶化组合物粘结和/或层压电子器件、电子元件和/或电子基底的方法。所述方法包括将可B阶化组合物施加在第一基底上，使所述可B阶化组合物B阶化为非粘性层压材料，使第二基底接触在非粘性的层压材料上以及活化所述非粘性层压材料，从而所述第一基底层压/粘结至所述第二基底。
另一实施方式提供使用本发明的可B阶化组合物制造的电子器件。包括薄膜太阳能电池模块。
附图说明
图1是用本发明的可B阶化组合物使层压的第一基底(带导孔)粘附到第二基底(不带任何导孔)的Olympus显微镜SZX-12 DP-70放大5倍图像。
图2是用对比样品使层压的第一基底(带导孔)粘附到第二基底(不带任何导孔)的Olympus显微镜SZX-12 DP-70放大5倍图像。
具体实施方式
本发明涉及可B阶化组合物，特别地该可B阶化组合物在活化后或后续组装步骤中显现粘性但基本上不流动。本发明对层压电子基底特别有用，其中层压材料的流动性能在封装件组装期间必须被严格控制。
术语“B阶化(B-stage)”在本文定义为，糊状组合物通过热和/或空气在室温下被干燥和/或半固化为非粘性膜，然后其在活化后可被再熔化。
术语“B阶化的(B-staged)”在本文定义为室温下由B阶化方法形成非粘性膜。
术语“活化”在本文定义为将B阶化膜粘附/层压在基底上的压力、热和/或辐射。
术语“低活化条件”在本文定义为低压和低温，如低于大约35psi和低于大约120℃，以将B阶化膜粘附/层压在基底上。
上位术语“基底”在本文定义为半导体板、半导体芯片、柔性基底、金属箔、表面安装元件、电阻器、电容器以及类似物。
术语“基本上”在本文定义为低于约10％。
本文所述的发明为本领域提供可B阶化组合物，其可被用于粘附基底与电子元件，同时在活化和后续的组装期间严格地控制B阶化材料的流动。
在一个实施方式中，可B阶化组合物包含树脂基体和流动控制剂。可B阶化组合物可以被沉积在第一基底上，进行B阶化以在第一基底上形成膜，并且在低活化条件下，所述膜显现粘性以粘附到第二基底但基本上不流动以避免污染不期望的区域。甚至在后续的组装条件下，所述膜保持在适当的位置并且基本上不流动。
可B阶化组合物可被施加在金属和非金属基底上。一些基底包含穿孔、导孔、洞、掩膜、I/O和元件；并且这些区域一定要保持没有污染物。这对进行后续的组装很重要；另外的处理步骤，如金线键合、通孔元件粘合、焊膏沉积等，可在基底的穿孔、导孔、洞、掩膜、I/O和元件上进行以形成可行的电子封装件。基底上B阶化材料的过分流动将干扰后面的组装，导致较差功能性和产量的封装件。
树脂基体由成膜树脂、固化剂和溶剂组成。
合适的树脂包括可以形成膜的任何热固性或热塑性树脂。具有约1000到约50000分子量范围的树脂对树脂基体来说是优选的。在各种实施方式中，这些树脂选自环氧树脂、苯氧基化合物、聚丁二烯[包括环氧化聚(丁二烯)、马来酸化聚(丁二烯)、丙烯酸化聚(丁二烯)、丁二烯-苯乙烯共聚物和丁二烯-丙烯腈共聚物]、马来酰亚胺[包括双马来酰亚胺]、聚酰亚胺、丙烯酸酯和甲基丙烯酸酯、以及氰酸酯、乙烯基醚、硫醇烯(thiol-enes)、含连接在芳香环并且与芳香环中不饱和部分共轭的碳碳双键的树脂(如由肉桂基和苯乙烯起始化合物衍生的化合物)、延胡索酸酯和马来酸酯。在各种其他实施方式中，这些树脂包括聚酰胺、苯并
Figure BPA00001277467400051
嗪、聚苯并
Figure BPA00001277467400052
嗪、聚醚砜、硅化烯烃(硅氧烷化烯烃，siliconized olefins)、聚烯烃、聚酯、聚苯乙烯、聚碳酸酯、聚丙烯、聚氯乙烯、聚异丁烯、聚丙烯腈、聚乙烯乙酸酯、聚(2-乙烯基吡啶)、顺式-1，4-聚异戊二烯、3，4-聚氯丁二烯、乙烯共聚物、聚环氧乙烷、聚乙二醇、聚甲醛、聚乙醛、聚(β-丙内酯)(poly(b-propiolacetone)s)、聚(10-癸酸酯)、聚对苯二甲酸乙二酯、聚己内酰胺、聚(11-十一酰胺)、聚对苯二甲酰间苯二胺、聚(四亚甲基-间-苯磺酰胺)(poly(tetramethlyene-m-benzenesulfonamide))、聚酯多芳基化合物、聚苯醚、聚苯硫、聚砜、聚醚酮、聚醚酰亚胺、氟化聚酰亚胺、聚酰亚胺硅氧烷、聚-异吲哚并-喹唑啉二酮(poly-isoindolo-quinazolinediones)、聚硫醚酰亚胺聚-苯基-喹喔啉、聚喹喔酮(polyquinixalones)、酰亚胺-芳基醚苯基喹喔啉共聚物、聚喹喔啉(polyquinoxalines)、聚苯并咪唑、聚苯并
Figure BPA00001277467400053
唑、聚降冰片烯、聚芳撑醚、聚硅烷、聚对亚苯基二甲基、苯并环丁烯、羟基-(苯并
Figure BPA00001277467400054
唑)共聚物和聚(硅亚芳基硅氧烷)(poly(silarylene siloxanes))。一种树脂或树脂组合可以被用于树脂基体中。基于干燥组合物(不包括溶剂)，树脂的使用范围在约40至约99重量百分比，优选为从约50至约99重量百分比。
固化剂可以是用于热固性树脂的任何传统固化剂或潜在固化剂。固化剂的实例包括脂肪族和芳香族聚胺、酸酐、衍生自聚羧酸的酰肼、咪唑衍生物(包括咪唑加合物、封端咪唑)、咪唑-酐加合物、双氰胺(dicyanodiamides)、胍衍生物、双胍衍生物(biguamide derivatives)、叔胺、胺盐、有机金属盐和无机金属盐以及酚。优选的固化剂是双氰胺、二氨基二环甲烷、二(4-氨基-3-甲基环己基)甲烷、二氨基二苯基甲烷、二氨基二苯基砜、4，4′-二氨基-3，3′-二氯二苯基甲烷(4，4’diamino-3，3’-dichlorodiphexylmethane)、己二酸二酰肼、癸二酸二酰肼(sabecic dihydrazide)、间苯二甲酸二酰肼、邻苯二甲酸酐、氯茵酸酐、2-甲基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑、2-乙基-4-甲基咪唑、2-十一烷基咪唑、1-苄基-2-甲基咪唑、1-氰基乙基-2-甲基咪唑、1-氰基乙基-2-乙基-4-甲基咪唑等。基于活性树脂，固化剂以大约0.1至大约30份的量存在。
合适的溶剂包括酯、醇、醚、乙酸酯、酮和溶解组合物中的树脂并在B阶化过程期间蒸发的其它常用溶剂。溶剂以有效溶解组合物中的树脂并使组合物具有良好的可操作性以形成膜的量存在。优选的溶剂包括丙二醇甲醚乙酸酯、γ-丁内酯、丙二醇甲醚、丙二醇正丙醚、二丙二醇二甲醚、乙二醇丙烯醚及其混合物。本领域技术人员可以根据树脂基体的需要调节溶剂的量，而不需要大量的试验。本领域技术人员也可以根据溶剂的量通过改变温度和时间来调节B阶化条件，而不需要大量的试验。
树脂基体可以进一步任选地包括添加剂如催化剂或加速剂、填料、消泡剂和促粘剂。在一些系统中，除了固化剂之外，催化剂或加速剂也可以被用于最优化固化速率。催化剂包括但不限于脲、衍生物(包括咪唑加合物、封端咪唑)、咪唑-酐加合物、环烷酸金属盐(metal napthenates)、乙酰丙酮金属盐(螯合物)、辛酸金属盐、乙酸金属盐、金属卤化物、金属咪唑络合物、金属胺络合物、三苯基膦、烷基取代的咪唑、咪唑盐和硼酸
Figure BPA00001277467400062
盐。优选的填料包括硅石、粘土、滑石、氧化铝、一氮化硼、氮化铝和碳酸钙。示例性的消泡剂包括消除泡沫的聚硅氧烷、聚丙烯酸酯和聚醚改性的甲基烷基聚硅氧烷共聚物。示例性的促粘剂为硅烷和聚乙烯醇缩丁醛(polyvinyl butyrol)。基于干燥组合物(不包括溶剂)，任选的添加剂可被添加多至约80重量百分比。
适合的流动控制剂包括核壳聚合物和嵌段共聚物。示例性的核壳聚合物包括丙烯腈-丁二烯-苯乙烯、甲基丙烯酸酯-丁二烯-苯乙烯、聚丁二烯、苯乙烯-丁二烯、硅氧烷等，其从Kaneka以Kane Ace MX series可得。其他示例性的核壳聚合物包括以商品名BLENDEX-415(General Electric Company)销售的丙烯腈-丁二烯-苯乙烯，和以商品名BTA-753(Rohm & Haas Company)和商品名E-950(Arkema)销售的甲基丙烯酸酯-丁二烯-苯乙烯。
示例性的嵌段共聚物包括三嵌段共聚物，其被设计为在侧嵌段和中间嵌段之间产生强的排斥。特别优选的是聚苯乙烯、1，4-聚丁二烯和间同聚(甲基丙烯酸甲酯)的共聚物；以及两个聚(甲基丙烯酸甲酯)嵌段围绕中心嵌段聚(丙烯酸丁酯)的共聚物(两者皆可以以Nanostrength从Arkema可得)。基于干燥组合物(不包括溶剂)，流动控制剂的使用范围在约0.1至约30重量百分比，优选为从约1至约20重量百分比。
流动控制剂应该被均匀地分散在树脂基体中。可以使用多种方法以完成该分散，例如，原位生成、高剪切分散、空化等。
在一个实施方式中，可B阶化组合物可以作为层压材料被B阶化，所述层压材料可以被活化以将第一基底粘附至第二基底。所述基底可以进一步包括带穿孔、导孔、洞、掩膜、I/O输入、电子元件等的区域，不期望这些区域被层压材料污染。
在下文中，将详细描述在层压过程中使用所述可B阶化组合物的方法。所述可B阶化组合物被施加在第一基底上，其中所述基底包括导孔。所述基底被B阶化同时向导孔中吹入空气以保持所述可B阶化组合物不流入导孔。然后非粘性(室温下)层压材料形成在所述第一基底上，并且所述导孔不含层压材料。不带任何导孔的第二基底被施加在所述层压材料上，并且整个封装件经受低活化条件。虽然所述层压材料变粘，但其基本上不流动，并且导孔基本上保持不含层压材料。然后，所述封装件经过后续的组装步骤，通常以大于120℃加热，而层压材料仍保持在适当的位置并且基本上不流入导孔。
以下实施例仅为说明的目的而非意欲以任何方式限制本发明的范围。
实施例
表1中的样品通过以下方法制成：(1)首先用SpeedMixer(FlackTek)在高速下混合树脂；(2)然后，流动控制剂、触变剂、间隔珠、固化剂和催化剂被加入并在高速下继续混合；和(3)加入溶剂直至总粘度范围在约1,000至约20,000cP。
表1.制剂和对比样品
Figure BPA00001277467400071
  触变剂f   11.53   11.53
  间隔珠g   0.30   0.89
  固化剂h   1.22   0.81   1.52   1.52
  催化剂i   0.56   0.41   0.70   0.70
  溶剂j   33.49   8.78   16.86   16.86
a98-411(CTBN-环氧加合物分散体(75％固体))；Reichhold corporation
bCTBN-环氧加合物分散体(55％固体)；National Starch & Chemical Company
c高分子量苯氧基树脂分散体(30％固体)；InChem Corporation
dKaneAce MX 136(在环氧树脂中的25％苯乙烯-丁二烯核壳分散体)；Kaneka
eKaneAce MX 965(在环氧树脂中的25％硅氧烷核壳分散体)；Kaneka
fCabosil M5(在环氧中分散的9％热解法二氧化硅分散)；Cabot Corporation
g间隔珠(2.5密耳的直径)；Potters Industries
h双氰胺；Degussa
i取代脲加速剂；CVC Specialty Chemical
j丙二醇甲醚乙酸酯(Propylene glycol methyl ethyl acetate)；Dow Chemical and Eastern Chemical
根据表1制备的样品被测试并评估以确定其流动特征。每个样品被施加在金属箔基底上，所述金属箔基底包括在整个基底卷(roll)以1cm均匀分布的1mm直径导孔。从导孔底部吹入空气以保持所述样品在涂布过程中不流入导孔。然后将所述样品在对流炉中110℃下B阶化6分钟。冷却至室温后，所述样品在第一基底上形成非粘性、平滑的层压材料。没有任何导孔的第二基底被施加在所述层压材料上，并在85℃和30psi下活化。然后对层压的基底在150℃下应用最后固化10分钟。检测导孔，并且导孔填充有层压粘合剂的百分比被报告在表2中。使用制剂1和2使得0％的导孔被层压材料填充。使用触变剂和/或间隔珠使得40％的导孔填充有层压材料。使用高分子量树脂作为层压材料不发生流动并且不能将基底粘附在一起。
表2.流动特征评估
  的％
*基底不能粘附在一起，因为层压材料不能流动并且在上述处理条件下不能显现粘性。
参考图1，用制剂1层压的基底，导孔基本上是空的。无论是在层压期间还是在后续的固化步骤期间，所述B阶化层压材料基本上不流入导孔。另一方面，使用对比B样品则在层压期间和后续的固化步骤期间填充了导孔(图2)。
进一步测试样品，检查基底的粘合性。根据ASTM-D标准方法，剥离强度值用Instron测试，结果列于表3中。如表3所示，在B阶化和完全固化后，制剂1和2具有高的剥离强度值。同样，如表3所示，对比C和D产生差的粘合性，因为其在85℃和30psi的活化条件下不能显现足够的粘性。
表3.粘合性
*基底不能粘附在一起，因为层压材料不能流动并且在上述处理条件下不能显现粘性。
在不偏离其精神和范围的情况下，可以对本发明进行许多改进和变化，这对本领域技术人员来说是显而易见的。本文描述的具体实施方式仅以举例的方式提供，本发明仅由所附权利要求的术语，以及这些权利要求所授权的等同物的全部范围所限定。

Claims (20)

1.层压材料组合物，其中所述组合物包括树脂基体和流动控制剂的B阶化产物，其中所述B阶化产物在活化后显现粘性但基本上不流动。
2.根据权利要求1所述的层压材料组合物，其中所述树脂基体包括树脂、固化剂和溶剂。
3.根据权利要求2所述的层压材料组合物，其中所述树脂选自环氧树脂、苯氧基化合物、聚丁二烯环氧树脂、苯氧基化合物、聚丁二烯、马来酰亚胺、聚酰亚胺、丙烯酸酯、甲基丙烯酸酯、氰酸酯、乙烯基醚、硫醇烯、延胡索酸酯、马来酸酯及其混合物。
4.根据权利要求2所述的层压材料组合物，其中所述固化剂选自双氰胺、二氨基二环甲烷、二(4-氨基-3-甲基环己基)甲烷、二氨基二苯基甲烷、二氨基二苯基砜、4，4′-二氨基-3，3′-二氯二苯基甲烷、己二酸二酰肼、癸二酸二酰肼、间苯二甲酸二酰肼、邻苯二甲酸酐、氯茵酸酐、2-甲基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑、2-乙基-4-甲基咪唑、2-十一烷基咪唑、1-苄基-2-甲基咪唑、1-氰基乙基-2-甲基咪唑、1-氰基乙基-2-乙基-4-甲基咪唑及其混合物。
5.根据权利要求2所述的层压材料组合物，其中所述树脂基体进一步包括催化剂。
6.根据权利要求2所述的层压材料组合物，其中所述树脂基体进一步包括填料、消泡剂和促粘剂。
7.根据权利要求1所述的层压材料组合物，其中所述流动控制剂选自苯乙烯-丁二烯核壳聚合物、硅氧烷核壳聚合物、丙烯腈-丁二烯-苯乙烯核壳聚合物、甲基丙烯酸酯-丁二烯-苯乙烯核壳聚合物、聚苯乙烯-1，4-聚丁二烯-间同聚(甲基丙烯酸甲酯)三嵌段共聚物、聚(甲基丙烯酸甲酯)-聚(丙烯酸丁酯)-聚(甲基丙烯酸甲酯)三嵌段共聚物及其混合物。
8.根据权利要求1所述的层压材料组合物，其中所述活化选自辐射、热、压力及其混合。
9.根据权利要求8所述的层压材料组合物，其中所述活化低于约120℃和低于约50psi。
10.沉积在基底上的B阶化膜，其中所述膜在活化后显示出粘性但基本上不流动，其中所述B阶化膜是树脂基体和流动控制剂的B阶化产物。
11.根据权利要求10所述的沉积在基底上的B阶化膜，其中所述基底包括穿孔、导孔、洞、掩膜、I/O输入、电子元件或其混合物。
12.根据权利要求11所述的沉积在基底上的B阶化膜，其中所述基底包括导孔。
13.根据权利要求10所述的沉积在基底上的B阶化膜，其中所述流动控制剂选自苯乙烯-丁二烯核壳聚合物、硅氧烷核壳聚合物、丙烯腈-丁二烯-苯乙烯核壳聚合物、甲基丙烯酸酯-丁二烯-苯乙烯核壳聚合物、聚苯乙烯-1，4-聚丁二烯-间同聚(甲基丙烯酸甲酯)三嵌段共聚物、聚(甲基丙烯酸甲酯)-聚(丙烯酸丁酯)-聚(甲基丙烯酸甲酯)三嵌段共聚物及其混合物。
14.根据权利要求10所述的沉积在基底上的B阶化膜，其中所述活化选自辐射、热、压力及其混合。
15.根据权利要求14所述的沉积在基底上的B阶化膜，其中所述活化低于约120℃和低于约50psi。
16.层压方法，其用包含树脂基体和流动控制剂的组合物将第一基底层压至第二基底，其中所述方法包括：
(a)将所述组合物施加在第一基底上；
(b)将所述组合物B阶化成B阶化膜；
(c)使第二基底接触在所述B阶化膜上；和
(d)活化所述B阶化膜；
藉此，所述第一基底粘附至所述第二基底。
17.根据权利要求16所述的层压方法，其中所述流动控制剂选自苯乙烯-丁二烯核壳聚合物、硅氧烷核壳聚合物、丙烯腈-丁二烯-苯乙烯核壳聚合物、甲基丙烯酸酯-丁二烯-苯乙烯核壳聚合物、聚苯乙烯-1，4-聚丁二烯-间同聚(甲基丙烯酸甲酯)三嵌段共聚物、聚(甲基丙烯酸甲酯)-聚(丙烯酸丁酯)-聚(甲基丙烯酸甲酯)三嵌段共聚物及其混合物。
18.根据权利要求16所述的方法，其中所述基底的至少一个包括穿孔、导孔、洞、掩膜、I/O输入、电子元件或其混合物。
19.一种制品，其包括用权利要求1所述的层压材料组合物至少粘附到第二基底的第一基底，其中所述基底的至少一个包括穿孔、导孔、洞、掩膜、I/O输入、电子元件或其混合物。
20.权利要求19所述的制品，其是薄膜太阳能电池模块。
CN2009801225423A 2008-04-16 2009-04-10 流动可控的可b阶化组合物 Pending CN102066487A (zh)

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