CN1894785A - 硅氧烷粘接剂 - Google Patents

硅氧烷粘接剂 Download PDF

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Publication number
CN1894785A
CN1894785A CNA2004800370662A CN200480037066A CN1894785A CN 1894785 A CN1894785 A CN 1894785A CN A2004800370662 A CNA2004800370662 A CN A2004800370662A CN 200480037066 A CN200480037066 A CN 200480037066A CN 1894785 A CN1894785 A CN 1894785A
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composition
silicon atom
adhesive agent
glass plate
silicone rubber
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CN100431121C (zh
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田村长
平井信男
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Momentive Performance Materials Japan LLC
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GE Toshiba Silicones Co Ltd
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Abstract

本发明提供一种硅氧烷粘接剂，其不降低金属丝接合性，而且半导体片表面和引线框及密封树脂的密合性不降低。更详细地说，本发明是一种用于接合半导体片和该片的安装构件的硅氧烷粘接剂，其含有加热固化时对玻璃板的沾染使得在玻璃板上的接触角为70°或以下的加成反应固化型硅氧橡胶组合物。

Description

硅氧烷粘接剂
技术领域
本发明涉及用于将半导体片和引板(タブ)等半导体片的安装构件接合的硅氧烷粘接剂(模粘合剂)。
背景技术
半导体装置是这样一种结构体：例如，使用环氧树脂、聚酰亚胺树脂等粘接剂(模粘合剂)等将含硅的半导体片与作为其支撑体的引板等半导体片的安装构件接合，然后将半导体片与金属制引线框电连接，并将它们的一体化物用环氧树脂等密封树脂密封而成的。鉴于使用以往的模粘合剂所引起的开裂等问题，提出了使用硅氧烷粘接剂粘接半导体片和引板的半导体装置(特开昭61-55300号公报)。这是使用硅氧橡胶弹性体缓和由半导体片和引板的热膨胀率差异引起的内部变形的装置。
但是，在上述特开昭61-55300号公报的技术中存在如下问题：用硅氧橡胶将半导体片与引板粘接之后，将半导体片和引线框用金属丝等接合金属丝连接时，半导体片与接合金属丝或引线框与接合金属丝的接合性(金属丝接合性)降低，从而使半导体装置的可靠性降低。
为解决此类问题，特开昭61-55300号公报中提出，使用在200℃下具有100mmHg或以上蒸汽压的、低分子硅氧烷含量在500ppm或以下的加成反应固化型硅氧橡胶组合物；特开2002-60719号公报中提出，使用硅原子数为11-50的环状和直链状低分子无官能硅氧烷的含量在3重量％或以下的粘接性硅氧橡胶。
发明内容
但是，本发明人的研究表明，即使按照上述特开昭61-55300号公报、特开2002-60719号公报的方法，接合性的可靠性仍存在改良的余地。
本发明的目的在于提供一种硅氧烷粘接剂，其克服了现有技术的缺点，不降低金属丝接合性，而且半导体片表面和引线框及密封树脂的密合性不降低。
为达到上述目的，本发明人进行了深入研究，结果发现，将含有特定加成反应固化型硅氧橡胶组合物的硅氧烷粘接剂作为用于接合半导体片和该片的安装构件的粘合剂非常有效，从而完成了本发明。
即本发明是用于接合半导体片和该片的安装构件的硅氧烷粘接剂，其特征在于，含有加热固化时对玻璃板的沾染使得在玻璃板上的接触角为70°或以下的加成反应固化型硅氧橡胶组合物。
本发明是用含有加热固化时对玻璃板的沾染使得在玻璃板上的接触角为70°或以下的加成反应固化型硅氧橡胶组合物的硅氧烷粘接剂将半导体片和该片的安装构件接合的方法。
本发明是加成反应固化型硅氧橡胶组合物在用于接合半导体片和该片的安装构件的硅氧烷粘接剂中的应用，所述加成反应固化型硅氧橡胶组合物加热固化时对玻璃板的沾染使得在玻璃板上的接触角为70°或以下。
具体实施方式
以下，对本发明进行详细说明。本发明是用于接合半导体片和该片的安装构件的硅氧烷粘接剂，其特征在于，含有加热固化时对玻璃板的沾染使得在玻璃板上的接触角为70°或以下的加成反应固化型硅氧橡胶组合物，作为这种加成反应固化型硅氧橡胶组合物，可列举：
加成反应固化型硅氧橡胶组合物(以下，称为本发明组合物1)，其含有：
(A)1分子中具有2个或以上硅原子键合的链烯基的聚有机硅氧烷，100重量份；
(B)100℃×1小时的加热减量在5重量％或以下、1分子中具有2个或以上硅原子键合的氢原子的聚有机硅氧烷，对于1个(A)成分的链烯基可足够提供0.5～3个本成分的硅原子键合的氢原子的量；
(C)具有硅原子键合的烷氧基、且不含硅原子键合的氢原子的粘接性赋予剂，0.1～10重量份；
(D)铂类催化剂，催化剂量；以及
加成反应固化型硅氧橡胶组合物(以下，称为本发明组合物2)，其含有：
(A)1分子中具有2个或以上硅原子键合的链烯基的聚有机硅氧烷，100重量份；
(B)100℃×1小时的加热减量在5重量％或以下、1分子中具有2个或以上硅原子键合的氢原子的聚有机硅氧烷，对于1个(A)成分的链烯基可足够提供0.5～3个本成分的硅原子键合的氢原子的量；
(D)铂类催化剂，催化剂量；
(E)粘接性赋予剂，0.1～10重量份；
(F)Al或Ti化合物，0.05～10重量份。
首先，说明本发明组合物1。作为本发明的(A)成分的1分子中含有2个或以上硅原子键合的链烯基的聚有机硅氧烷是本发明组合物的主剂(原料聚合物)，用下述平均组成式(1)表示，
R1 aSiO(4-a)/2        (1)
(式中，R1可以相同也可以不同，为碳原子数1～10的未取代或取代的一价烃基，a为1～3的正数)。
作为上述R1表示的与硅原子键合的未取代或取代的一价烃基，可列举：甲基、乙基、丙基、异丙基、丁基、异丁基、叔丁基、戊基、新戊基、己基、环己基、辛基、壬基、癸基等烷基；苯基、甲苯基、二甲苯基、萘基等芳基；苄基、苯乙基、苯丙基等芳烷基；乙烯基、烯丙基、丙烯基、异丙烯基、丁烯基、己烯基、环己烯基、辛烯基等链烯基；上述基团氢原子的一部分或全部被氟、溴、氯等卤原子、氰基等取代的基团，如氯甲基、氯丙基、溴乙基、3，3，3-三氟丙基、2-氰基乙基等。
这种情况下，R1中的至少2个必须是链烯基(尤其是优选碳原子数2～8的，更优选2～6的)。另外，链烯基的含量，优选在与硅原子键合的所有有机基团中(即，前述平均组成式(1)中作为R1的未取代或取代的一价烷基中)占0.01～20摩尔％，特别优选占0.1～10摩尔％。这些链烯基可以与分子链末端的硅原子键合，也可以与分子链中的硅原子键合，也可与二者键合，但从组合物的固化速度、固化物的物性等方面考虑，本发明使用的聚有机硅氧烷优选至少含有与分子链末端的硅原子键合的链烯基。另外，作为链烯基以外的R1，优选甲基、苯基、3，3，3-三氟丙基。
上述聚有机硅氧烷的结构通常是主链包括二有机基硅氧烷的重复单元，分子链两末端用三甲基甲硅烷氧基、二甲基苯基甲硅烷氧基、二甲基羟基甲硅烷氧基、二甲基乙烯基甲硅烷氧基、三乙烯基甲硅烷氧基等三有机基甲硅烷氧基封端的基本上具有直链结构的二有机基聚硅氧烷，部分是支链状结构、环状结构等也可以。平均聚合度(重量平均聚合度)优选为100～100,000，特别优选为200～10,000，另外25℃时粘度优选为100～100,000,000cSt(厘沲)，特别优选为1,000～1,000,000cSt。
(B)成分的聚有机硅氧烷是在例如10mmHg或以下的减压下、100～140℃的加热条件下进行反萃取等，100℃×1小时的加热减量在5重量％或以下的聚有机硅氧烷。而且它作为(A)成分交联剂起作用，1分子中含有2个或以上硅原子键合的氢原子，其分子结构可以是直链状、支链状或环状结构的任何一种。
对于1个(A)成分的链烯基，这种聚有机硅氧烷的配合量为可以足够提供0.5～3个本成分的硅原子键合的氢原子的量，优选可足够提供1～2个的量。
作为(B)成分，可列举甲基氢聚环硅氧烷、甲基氢硅氧烷-二甲基硅氧烷环状共聚物、两末端用三甲基甲硅烷氧基封端的甲基氢聚硅氧烷、两末端用三甲基甲硅烷氧基封端的二甲基硅氧烷-甲基氢硅氧烷共聚物、两末端用二甲基氢甲硅烷氧基封端的二甲基聚硅氧烷、两末端用二甲基氢甲硅烷氧基封端的二甲基硅氧烷-甲基氢硅氧烷共聚物、两末端用三甲基甲硅烷氧基封端的甲基氢硅氧烷-二苯基硅氧烷共聚物、两末端用三甲基甲硅烷氧基封端的甲基氢硅氧烷-二苯基硅氧烷-二甲基硅氧烷共聚物、两末端用二甲基氢甲硅烷氧基封端的甲基氢硅氧烷-二甲基硅氧烷-二苯基硅氧烷共聚物、含有(CH3)2HSiO1/2单元和(CH3)3SiO1/2单元及SiO4/2单元的共聚物、含有(CH3)2HSiO1/2单元和SiO4/2单元的共聚物、含有(CH3)2HSiO1/2单元和SiO4/2单元及(C6H5)3SiO1/2单元的共聚物等。
本发明的(C)成分是含有与硅原子键合的烷氧基，且不含有与硅原子键合的氢原子的粘接性赋予剂。
第3成分的粘接性赋予剂优选使用分子中分别含有1个或以上与硅原子键合的烷氧基、和选自链烯基、丙烯酰基、甲基丙烯酰基和环氧基的至少1个反应性官能基团的有机硅烷或硅原子数为2～50、优选4～20个左右的有机硅氧烷低聚物等有机硅化合物。这些有机硅化合物是用于赋予硅氧橡胶组合物与半导体片、安装部、引线框等的粘合性的物质，可以使用公知的有机硅化合物，只要不防碍硅氧橡胶组合物的加成硫化即可。
作为这种有机硅化合物，可列举例如γ-环氧丙氧基丙基三甲氧基硅烷、β-(3，4-环氧环己基)乙基三甲氧基硅烷等含有环氧基官能团的烷氧基硅烷；乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三(甲氧乙氧基)硅烷等含有链烯基的烷氧基硅烷；γ-甲基丙烯酰氧基丙基三甲氧基硅烷、γ-丙烯酰氧基丙基三甲氧基硅烷等含有丙烯酰基或甲基丙烯酰基的烷氧基硅烷等烷氧基硅烷。
(C)成分相对于(A)成分100重量份使用0.1～10重量份。
(D)成分的铂类催化剂是用于使本发明的粘接剂固化的催化剂，一般可使用公知的加成反应用催化剂，作为这种催化剂可列举铂黑、将固体铂担载于氧化铝、二氧化硅等担体而成的催化剂、氯铂酸、醇改性氯铂酸、氯铂酸与烯烃的配位化合物或铂与乙烯基硅氧烷的配位化合物等。使用这些催化剂时，如果是固体催化剂，为了使分散性好，优选将其粉碎，制成粒径小、比表面积大的，对于氯铂酸或其与烯烃的配位化合物，优选将其溶解于醇、酮、醚或烃类等溶剂中使用。另外，这种催化剂的添加量可以根据所期望的固化速度适当地调整，为得到良好的固化物，对于氯铂酸等这样的与硅氧烷相溶的物质，以铂量计，相对于上述(A)成分和(B)成分的总量，优选在1～100ppm的范围。
其次，对本发明组合物2的方案进行说明。
本发明组合物2中，(A)、(B)、(D)成分与本发明组合物1的情况相同。
本发明组合物2使用(E)粘接性赋予剂和(F)Al或Ti化合物代替本发明组合物1的(C)成分。
(E)成分的粘接性赋予剂没有(C)成分那样的含有与硅原子键合的烷氧基、且不含有与硅原子键合的氢原子的限定，可以使用包含(C)成分的各种公知的粘接性赋予剂。
但是，在使用(C)成分以外的粘接性赋予剂时，必须并用(F)Al或Ti化合物。
作为(F)成分的Al化合物，(MeO)3Al、(EtO)3Al、(a-PrO)3Al等醇铝，环烷酸、硬脂酸、辛酸或苯甲酸等的铝盐，醇铝与乙酰乙酸酯或二烷基丙二酸盐反应得到的。
等铝螯合物、氧化铝的有机酸盐及乙酰丙酮铝等可列举，但从水解性方面考虑，优选铝螯合物或醇铝。而且由于为液态，处理方便考虑，优选双乙酰乙酸乙酯单乙酰丙酮铝或乙酰烷氧基二异丙醇铝。
作为(F)成分的Ti化合物可列举四(正丁氧基)钛、四(异丙氧基)钛、四(2-乙基己氧基)钛、四(硬脂氧基)钛等四烷氧基钛化合物；二异丙氧基双(乙酰丙酮)钛、异丙氧基(2-乙基己二醇)钛、二异丙氧基二乙酰乙酸乙酯钛，羟基双(乳酸)钛等钛螯合物，另外，还有异丙基三异硬脂酰钛酸酯、异丙基三(二辛基磷酸酯)钛酸酯、四异丙基)双(二辛基亚磷酸酯)钛酸酯、四辛基双(二(十三烷基)亚磷酸酯)钛酸酯、四(2，2-二烯丙氧基甲基-1-丁基)双(二(十三烷基))亚磷酸酯钛酸酯、双(二辛基焦磷酸酯)羟基乙酸钛酸酯、双(二辛基焦磷酸酯)亚乙基钛酸酯、异丙基三辛酰基钛酸酯、异丙基二甲基丙烯酰基异硬脂酰钛酸酯，从所得到的固化性聚有机硅氧烷组合物的保存稳定性优良考虑，优选四(正丁氧基)钛。
相对于(A)成分重量份100，(F)成分的配合量为0.05～10重量份，优选为0.1～5重量份。
本发明中可以进一步配合填充材料。填充材料除了增强硅氧橡胶组合物以赋予必要的橡胶强度以外，还能保证粘接作业时必要的粘度，作为填充材料，优选增强性二氧化硅类填充材料。增强性二氧化硅类填充材料可列举热解法二氧化硅、疏水处理二氧化硅、烧结二氧化硅、沉淀二氧化硅等。
另外，在本发明的组合物中，只要不损害其目的，可以适当配合炔属醇其他的加成硫化调节剂、二氧化钛、氧化铝、碳黑等。
附图说明
图1是实施例中用于评价金属丝接合性的评价用半导体装置的概略截面图。
实施例
以下为本发明的实施例。以下实施例和比较例中份均表示重量份。
实施例1～5，比较例1～3
·(A)成分
将760份三甲基氯硅烷、141份甲基乙烯基二氯硅烷、146份原硅酸乙酯在甲苯中进行共水解，按常法进行脱酸、中和、水洗之后用苛性钾水溶液处理，用醋酸中和、水洗、脱水，得到基本上不具有与硅原子键合的羟基，而具有与硅原子键合的乙烯基的树脂。使用配合这种含乙烯基树脂10份与23℃时粘度为3,000cP的α，ω-二乙烯基聚二甲基硅氧烷90份的有机硅氧烷作为(A)成分。
·(B)成分
将MM表示的二硅氧烷、D4表示的环状硅氧烷、D’4表示的环状硅氧烷在硫酸催化剂存在下聚合，然后中和，得到平均组成式MD’23D16M表示的具有与硅原子键合的氢原子的有机硅氧烷。将该硅氧烷在2mmHg的减压下、温度120℃的加热条件下，进行2～4小时的反萃取处理，得到在100℃、1小时的加热减量如下所述的有机硅氧烷。
4小时处理    (B)-1(加热减量1.3重量％)
3小时处理    (B)-2(加热减量3.8重量％)
2小时处理    (B)-3(加热减量6.5重量％)
未处理       (B)-4(加热减量10重量％)。
另外，简写为M，D，D’的物质分别代表如下结构。
Figure A20048003706600101
·(C)成分(在本实施例中也代表(E)成分)
(C)-1
下式表示的硅烷化合物
Figure A20048003706600102
(C)-2
下式表示的硅烷化合物
Figure A20048003706600103
(C)-3
下式表示硅烷化合物
Figure A20048003706600111
的反应生成物。
·(D)成分
含有3.8％铂的Lamorrow’s催化剂
·(F)成分
(F)-1
下式表示的铝螯合物
Figure A20048003706600112
将如上所示的有机硅氧烷和添加剂按表1所示的量均匀混合得到组合物1～8。另外，组合物6～8为比较例组合物。
实施例中，按照如下记载的方法进行玻璃板上接触角的测定和粘合剂特性。
(玻璃板上接触角的测定)
在50×50×1mm的玻璃板上涂布0.0100～0.0130g组合物，其上载置18×18×0.16mm的盖玻片，组合物夹在其间并使组合物扩展至整个盖玻片。将其放入玻璃培养皿(内径70mm，深19mm)，加盖，在150℃下、1小时加热使其固化。降至室温后，在盖玻片4个角和中心部位5处，测定对于水的接触角，算出它们的平均值。
(粘接性评价)
将80×25×2mm的两片铜板平行放置，长边只重合10mm，在两片铜板之间形成1mm厚的上述组合物层，使其重合部分相对的2面接合，在150℃加热1小时，放冷之后制成试样。另外，用陶瓷(氧化铝)板以同样的方法制成试样。将这样得到的试样装在拉伸试验机上，以10mm/min的拉伸速度进行粘合性试验，确认断裂面是内聚破坏还是界面剥离。
(金属丝接合性评价)
在图1所示的评价用半导体中，使粘接剂8介于半导体片2和引板1之间，在150℃加热1小时。用金属丝5接合(金属丝接合)铝垫3和铜制引线框4从而制成一体化物。金属丝4的接合是通过超声波热压接合法进行接合的。接着，对于该一体化物，观察金属丝5和铝垫3或金属丝5和引线框4的连接点，同时拉伸该金属丝5，金属丝脱离者为接合不良产品。每1检品包括64个引线框，制成10个检品，在共计640管脚中统计不良数。6为环氧树脂，7为铜制外部引线框。
它们的结果如表1所示。
表1
  组合物No.   1   2   3   4   5   6   7   8
  实施例1   实施例2   实施例3   实施例4   实施例5   比较例1   比较例2   比较例3
 (A)   100   100   100   100   100   100   100   100
 (B)-1   5.4   5.4   5.4   5.4   5.4
 (B)-2   5.4
 (B)-3   5.4
 (B)-4   5.4
 (D)   0.05   0.05   0.05   0.05   0.05   0.05   0.05   0.05
 (C)-1   2   2   2   2   2
 (C)-2   2
 (C)-3   2   2
 (F)   0.2   0.2
 接触角(150℃×1h)°   66   65   68   66   64   72   74   76
 粘接性
 铜板   内聚破坏   内聚破坏   内聚破坏   内聚破坏   内聚破坏   内聚破坏   内聚破坏   内聚破坏
 陶瓷(氧化铝)板   内聚破坏   内聚破坏   内聚破坏   内聚破坏   内聚破坏   内聚破坏   内聚破坏   内聚破坏
 金属丝接合性不良数   0   0   0   0   0   28   43   51

Claims (5)

1.硅氧烷粘接剂，其用于接合半导体片和该片的安装构件，其特征在于，含有在加热固化时对玻璃板的沾染使得在玻璃板上的接触角为70°或以下的加成反应固化型硅氧橡胶组合物。
2.权利要求1所述的硅氧烷粘接剂，其中加成反应固化型硅氧橡胶组合物包括：
(A)1分子中含有2个或以上硅原子键合的链烯基的聚有机硅氧烷，100重量份；
(B)100℃×1小时的加热减量在5重量％或以下、1分子中含有2个或以上硅原子键合的氢原子的聚有机硅氧烷，对于1个(A)成分的链烯基可足够提供0.5～3个本成分的硅原子键合的氢原子的量；
(C)具有硅原子键合的烷氧基、且不含有硅原子键合的氢原子的粘接性赋予剂，0.1～10重量份；
(D)铂类催化剂，催化剂量。
3.权利要求1所述的硅氧烷粘接剂，其中加成反应固化型硅氧橡胶组合物包括：
(A)1分子中含有2个或以上硅原子键合的链烯基的聚有机硅氧烷，100重量份；
(B)100℃×1小时的加热减量在5重量％或以下、1分子中含有2个或以上硅原子键合的氢原子的聚有机硅氧烷，对于1个(A)成分的链烯基可提供0.5～3个本成分的硅原子键合的氢原子的量；
(D)铂类催化剂，催化剂量；
(E)粘接性赋予剂，0.1～10重量份；
(F)Al或Ti化合物，0.05～10重量份。
4.接合半导体片和该片的安装构件的方法，其利用硅氧烷粘接剂进行接合，所述硅氧烷粘接剂含有加热固化时对玻璃板的沾染使得在玻璃板上的接触角为70°或以下的加成反应固化型硅氧橡胶组合物。
5.加成反应固化型硅氧橡胶组合物在用于接合半导体片和该片的安装构件的硅氧烷粘接剂中的应用，所述加成反应固化型硅氧橡胶组合物加热固化时对玻璃板的沾染使得在玻璃板上的接触角为70°或以下。
CNB2004800370662A 2003-12-10 2004-12-09 硅氧烷粘接剂及其应用以及将半导体片和安装构件接合的方法 Expired - Fee Related CN100431121C (zh)

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