CN1288668C - 柔顺且可交联的热界面材料 - Google Patents

柔顺且可交联的热界面材料 Download PDF

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CN1288668C
CN1288668C CNB028042662A CN02804266A CN1288668C CN 1288668 C CN1288668 C CN 1288668C CN B028042662 A CNB028042662 A CN B028042662A CN 02804266 A CN02804266 A CN 02804266A CN 1288668 C CN1288668 C CN 1288668C
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M·阮
J·格伦迪
C·爱德华兹
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Honeywell International Inc
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Abstract

描述了一种由至少一种硅氧烷树脂混合物，至少一种润湿促进剂和至少一种导热填料形成的柔顺的且可交联的热界面材料，制备和使用该材料的方法；以及提高聚合物和树脂体系导热率的方法。

Description

柔顺且可交联的热界面材料
本申请要求美国实用新型申请No.09/774466的权利，在此将其全文引入作为参考。
背景
随着电子器件变得更小并更高速地运行，以热量形式放射出的能量剧增。在本行业中普遍的做法是在这些器件中单独或借助于载体使用热脂或油脂状材料，来转移经过物理界面散逸的多余热量。最常用的热界面材料的类型是热脂、相变材料和弹性体带。热脂或相变材料比弹性体带的阻热更低，这是因为其能够被分布成为极薄层并能在相邻表面之间提供紧密接触。典型的热阻抗值为0.6-1.6℃cm2/W。
热脂的严重缺陷是当其用于VLSI芯片中时，在热循环，如-65℃至150℃之后，或在做功循环之后，其导热性能会显著变差。还发现，当表面平面度的大偏差在电子器件中的接触面之间形成缝隙或由于其它原因如制造公差等在接触面之间出现大的缝隙时，这些材料的性能会变差。当这些材料的热传递能力失效时，使用了这些材料的电子器件的性能会受到负面影响。本发明提供了一种热界面材料，该材料特别适合用作电子器件的界面材料。
发明概述
本发明提供了一种柔顺且可交联的材料，所述材料包含硅氧烷树脂混合物，如乙烯基硅氧烷、乙烯基Q树脂、含氢功能团的硅氧烷和铂-乙烯基硅氧烷的混合物，润湿促进剂和至少一种导热填料。所述柔顺的导热材料能够促进高功率半导体器件中的热量散选并保持稳定的热性能。在使用该材料的电子器件的热-力学应力或波动的功率循环中，不会发生界面层离或相分离。
所述柔顺且可交联的热界面材料可以这样进行配制：将各组分混合在一起以得到一种糊状物，可用各种分配方法将其施涂在任何特定的表面上并在室温或高温下固化。也可以配制为高度柔顺、固化的、粘性弹性体薄膜或片材以用在其它的界面用途中，在这些用途中该材料可以预先施用在例如受热器上或用在任何其它的界面情况下。
最好在将要掺入的填料中包含至少一种导热填料，如银、铜、铝及其合金；氮化硼、氮化铝、镀银的铜、镀银的铝和碳纤维。另外，向其中加入抗氧化剂以降低树脂氧化作用，加入润湿促进剂以促进表面的润湿作用，加入固化加速剂如可令其在室温下固化，加入降粘剂来提高分散性和加入交联助剂，这样做可能也是有用的。还经常需要包含基本为球形颗粒的填料以限制所述用于界面用途中的柔顺材料的可压缩性，即限制或控制其厚度。
还发现，树脂体系如上述的填料和混有硅氧烷树脂混合物的组合的导热率可通过向体系中掺入碳微纤维和其它填料而得到特别地改进。
发明详述
柔顺且可交联的热界面材料可以如下配制：将硅氧烷树脂混合物如乙烯基硅氧烷、乙烯基Q树脂、含氢功能团的硅氧烷和铂-乙烯基硅氧烷的混合物，有机钛酸酯润湿促进剂和至少一种导热填料混合在一起。可以混入不止一种的硅氧烷树脂混合物来制造柔顺且可交联的界面材料。含硅氧烷树脂的界面材料，结合以适当的导热填料，表现出的热容低于0.5cm2℃/W。与热脂不同，所述材料的热性能在IC器件的热循环或流动循环(flow cycling)之后不会变差，这是因为液态的硅氧烷树脂在热活化作用下会交联形成软凝胶。而且，当用作界面材料时，其不会像热脂那样被“挤出来”并且不会在热循环中发生界面层离。该新材料可以以可分配的液体糊状物的形式提供，用分配方法施用，然后按需要固化。其也可以以高度柔顺、固化的弹性体薄膜或片材的形式提供以预先施用在界面如受热器上。使用导热率大于约0.2，优选至少为约0.4w/m℃的填料是有利的。柔顺的导热材料促进了高功率半导体器件的热量散逸。所述糊状物可以配制成功能硅氧烷树脂和导热填料的混合物。
如本文中所使用的，术语“柔顺”涵盖的材料性能是：该材料在室温下是屈服且可成型的，与室温下是固体且不屈服的材料相反。如本文中所使用的，术语“可交联”指尚未交联的那些材料或化合物。
乙烯基Q树脂是一种活性硫化的特种硅氧烷橡胶，其具有如下的基体聚合物结构：
Figure C0280426600061
乙烯基Q树脂还是用于加成固化弹性体的透明的增强添加剂。含有至少20％Q-树脂的乙烯基Q树脂分散体的例子有VQM-135(DMS-V41Base)，VQM-146(DMS-V46Base)和VQX-221(在二甲苯Base中含50％)。
例如，一种可考虑使用的硅氧烷树脂混合物可如下形成：
  组分   重量百分数   备注/功能
  乙烯基硅氧烷乙烯基Q树脂含氢功能团的硅氧烷铂-乙烯基硅氧烷   75(在70-97范围内)20(在0-25范围内)5(在3-10范围内)20-200ppm   乙烯基封端的硅氧烷增强添加剂交联剂催化剂
该树脂混合物既可在室温下也可在高温下固化以形成柔顺的弹性体。该反应通过含氢功能团的硅氧烷在催化剂，如铂络合物或镍络合物存在下与含乙烯基功能团的硅氧烷的氢化硅烷化作用(加成固化)来实现。优选的铂催化剂为SIP6830.0，SIP6832.0和铂-乙烯基硅氧烷。
可考虑的乙烯基硅氧烷的实例包括分子量为约10000-50000的乙烯基封端的聚二甲基硅氧烷。含氢功能团的硅氧烷的实例包括甲基氢化硅氧烷-二甲基硅氧烷共聚物，其分子量为约500-5000。物理性质可从非常低交联密度下的非常柔软的凝胶到较高交联密度的韧性弹性体网络之间变化。
分散在树脂混合物中的导热填料颗粒最好具有高导热率。适合的填料材料包括银、铜、铝及其合金；氮化硼，铝球体，氮化铝，镀银的铜，镀银的铝和碳纤维。氮化硼和银或氮化硼和银/铜的组合也能提供高导热率。至少为20wt％用量的氮化硼，至少为70wt％用量的铝球体和至少为约60wt％用量的银特别有用。
一种包含称作“蒸汽生成碳纤维”(VGCF)的特殊形式的碳纤维的填料具有特殊效能，其可从Applied Sciences，Inc.，Cedarville，.Ohio获得。VGCF，或“碳微纤维”，是一种经过热处理的高度石墨化的形式(导热率＝1900w/m℃)。加入约0.5wt％的碳微纤维能显著提高导热率。可以购得各种长度和直径的此类纤维；如，1mm至几十厘米长和小于0.1至超过100μm的直径。一种有用的形式为直径不大于约1μm且长度为约50-100μm，其具有的导热率比直径大于5μm的其它普通碳纤维大约2或3倍。
向树脂体系如上述的硅氧烷树脂混合物中加入大量的VGCF是困难的。当向所述树脂中加入碳微纤维，例如(约1μm或更小)时，它们不能良好地混合，因为相对于树脂的量需要加入大量的纤维以有益地提高导热率。然而，我们发现可以向含有相对大量的其它纤维的树脂体系中加入较大量的碳微纤维。当树脂中加入了其它纤维时可以比单独向聚合物中添加时加入更大量的碳微纤维，由此可以在改善热界面材料的导热率方面提供更大益处。碳微纤维与聚合物的重量比优选为0.05-0.50。
掺入基本为球形的填料颗粒使填充密度最大化也是有利的。另外，基本为球体或相似的形状还可以在压实过程中提供对厚度的某种控制。加入功能化有机金属偶联剂或润湿剂，如有机硅烷，有机钛酸酯，有机锆等可以使填料颗粒易于分散。在树脂材料中使用的填料的一般颗粒度可以是约1-20μm，最大为约100μm。可以加入抗氧化剂以抑制树脂混合物凝胶的氧化作用和热降解。一般使用的抗氧化剂包括Irganoz1076，酚类的Irganox 565，胺类，(用量为0.01％-约1wt％)，购自Ciba Giegy of Hawthorne，New York。
为说明本发明，通过将描述于以下实施例A-F中的各组分混合制备了一些实例。所列的实施例包含一种或多种任选的添加物，例如抗氧化剂或润湿性促进剂。这些添加物的量可以变化，但是通常它们以大约以下的量存在是有用的(以重量百分数计)：填料为最高至总量(填料加树脂)的95％；润湿性促进剂为(总量的)0.1-5％；增粘剂为(总量)的0.01-1％以及抗氧化剂为(总量的)0.01-1％。应当注意的是加入至少约0.5％的碳纤维显著提高了导热率。实施例还显示了对所考虑使用的混合物的各种物理-化学性能的测试。
导热糊状物实施例
  组分    A    B    C    D    E    F
  硅氧烷树脂混合物环氧硅烷硅烷醇封端的乙烯基硅氧烷有机钛酸酯铝球体   2575   2080   24.80.10.175   19.80.10.180   160.10.13.880   120.10.13.884
  粘度(Pa.s)粘合强度(psi)25℃的模量(Mpa)热阻抗(cm2C/w)导热率(w/mC)   80100200.441.8   27545350.551.5   78250220.401.8   280180300.501.5   85160140.283.0   180250280.253.2
环氧硅烷和硅烷醇封端的乙烯基硅氧烷是增粘添加剂。有机钛酸酯作为润湿促进剂降低了糊状物粘度并增加填料负载。所用的有机钛酸酯为异丙基三异硬脂酰基钛酸酯。有机钛酸酯的一般结构为RO-Ti(OXRY)，其中RO为可水解基团，X和Y是粘合剂官能团。铝球体的颗粒尺寸为1-20μm。
这样，柔顺且可交联的热界面材料的特定实施方案和用途得到了公开。然而，对于本领域技术人员而言，除已经描述过的那些，在不背离本发明的概念的情况下是可能有更多的改进方案，这一点是显而易见的。因此，本发明的主旨除了受所附权利要求的精神限制以外将不受其它限制。而且，在理解说明书和权利要求时，所有术语都应以与上下文一致的最广义的可能方式去理解。特别是术语“包含”应被理解为其是非排除地引用元素、组分或步骤，表明其所指的元素、组分或步骤可与其它未特别指明的元素、组分或步骤一起存在或使用或相互结合。

Claims (22)

1.一种柔顺的且可交联的材料，其用作电子器件的界面材料，包含至少一种硅氧烷树脂混合物，至少一种润湿促进剂和至少一种导热填料。
2.权利要求1的柔顺的且可交联的材料，其中的至少一种硅氧烷树脂混合物包含乙烯基封端的硅氧烷，增强添加剂，交联剂和催化剂。
3.权利要求2的柔顺的且可交联的材料，其中的乙烯基封端的硅氧烷是乙烯基硅氧烷。
4.权利要求2的柔顺的且可交联的材料，其中的增强添加剂是乙烯基Q树脂。
5.权利要求2的柔顺的且可交联的材料，其中的交联剂包含一种含氢功能团的硅氧烷。
6.权利要求2的柔顺的且可交联的材料，其中的催化剂包含一种铂络合物。
7.权利要求6的柔顺的且可交联的材料，其中的铂络合物是铂-乙烯基硅氧烷化合物。
8.权利要求1的柔顺的且可交联的材料，其中的润湿促进剂包含一种有机钛酸酯化合物。
9.权利要求1的柔顺的且可交联的材料，其中所述填料包含如下的至少一种：银、铜、铝及其合金；氮化硼，氮化铝，铝球体，镀银的铜，镀银的铝和碳纤维；以及它们的混合物。
10.权利要求9的柔顺的且可交联的材料，除了至少含有至少一种填料以外还包含碳微纤维。
11.权利要求1的柔顺的且可交联的材料，其中所述填料包含碳微纤维和至少一种其它填料，其包含银、铜、铝及其合金；氮化硼，氮化铝，镀银的铜，镀银的铝和碳纤维；以及它们的混合物。
12.权利要求1的柔顺的且可交联的材料，其中至少一部分所述填料包含球形的颗粒。
13.权利要求1的柔顺的且可交联的材料，还包含一种抗氧化剂。
14.权利要求13的柔顺的且可交联的材料，其中所述抗氧化剂存在的量为0.01-1wt％。
15.用作电子器件界面材料的柔顺的且可交联的材料的可分配的糊状物，其包含至少一种硅氧烷树脂混合物，至少一种润湿促进剂和至少一种导热填料。
16.用作电子器件界面材料的柔顺的且可交联材料的片材或薄膜，其包含至少一种硅氧烷树脂混合物，至少一种润湿促进剂和至少一种导热填料。
17.一种制备柔顺且可交联材料的方法，包含将至少一种硅氧烷树脂混合物与至少一种润湿促进剂和至少一种导热填料相混合。
18.权利要求17的方法，其进一步包括配制所述材料的可分配糊状物。
19.权利要求17的方法，其进一步包含将所述材料模制成片材或薄膜，所述片材或薄膜能够按尺寸切割并用作电子器件中各部分间的界面。
20.一种提高聚合物导热率的方法，包含向其中掺入碳微纤维和至少一种导热填料。
21.权利要求20的方法，其中所述碳微纤维存在的量为至少0.5wt％，或碳微纤维与聚合物之比至少为0.05。
22.权利要求21的方法，其还包含另外掺入一种填料，该填料包括如下的至少一种：银、铜、铝及其合金；氮化硼、氮化铝、镀银的铜、镀银的铝和碳纤维；以及它们的混合物。
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US20020007035A1 (en) 2002-01-17
EP1356477B1 (en) 2008-10-15
CA2433567A1 (en) 2002-08-08
KR20040030491A (ko) 2004-04-09

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