CN110382565A - 用作底部填充材料的热固性组合物和半导体装置 - Google Patents
用作底部填充材料的热固性组合物和半导体装置 Download PDFInfo
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- CN110382565A CN110382565A CN201880015827.6A CN201880015827A CN110382565A CN 110382565 A CN110382565 A CN 110382565A CN 201880015827 A CN201880015827 A CN 201880015827A CN 110382565 A CN110382565 A CN 110382565A
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Classifications
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
- H01L21/56—Encapsulations, e.g. encapsulation layers, coatings
- H01L21/563—Encapsulation of active face of flip-chip device, e.g. underfilling or underencapsulation of flip-chip, encapsulation preform on chip or mounting substrate
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
- H01L23/296—Organo-silicon compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F20/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F20/02—Monocarboxylic acids having less than ten carbon atoms, Derivatives thereof
- C08F20/10—Esters
- C08F20/20—Esters of polyhydric alcohols or polyhydric phenols, e.g. 2-hydroxyethyl (meth)acrylate or glycerol mono-(meth)acrylate
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
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- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/31—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/02—Bonding areas ; Manufacturing methods related thereto
- H01L24/07—Structure, shape, material or disposition of the bonding areas after the connecting process
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/02—Bonding areas; Manufacturing methods related thereto
- H01L2224/04—Structure, shape, material or disposition of the bonding areas prior to the connecting process
- H01L2224/05—Structure, shape, material or disposition of the bonding areas prior to the connecting process of an individual bonding area
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- H—ELECTRICITY
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- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
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- H01L2224/12—Structure, shape, material or disposition of the bump connectors prior to the connecting process
- H01L2224/13—Structure, shape, material or disposition of the bump connectors prior to the connecting process of an individual bump connector
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- H01L2224/13082—Two-layer arrangements
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- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
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- H01L2224/12—Structure, shape, material or disposition of the bump connectors prior to the connecting process
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- H01L2224/13101—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of less than 400°C
- H01L2224/13111—Tin [Sn] as principal constituent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/10—Bump connectors; Manufacturing methods related thereto
- H01L2224/12—Structure, shape, material or disposition of the bump connectors prior to the connecting process
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- H01L2224/13138—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
- H01L2224/13147—Copper [Cu] as principal constituent
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- H01—ELECTRIC ELEMENTS
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Abstract
本发明的目的是提供一种热固性组合物,其用作底部填充材料以密封在基材和面朝下接合到该基材上的半导体芯片之间的间隙,并具有改善半导体装置的RF特性的能力。用作底部填充材料的热固性组合物含有:单官能或双官能丙烯酸类化合物;热自由基聚合引发剂;二氧化硅;和包含1,2‑乙烯基基团的弹性体。所述热固性组合物是液体,并且具有在热固化时转变成固化产物的性质,所述固化产物具有在25℃为3.2以下的相对介电常数和在25℃为0.013以下的介电损耗角正切。
Description
技术领域
本发明涉及用作底部填充材料的热固性组合物,以及包括由所述用作底部填充材料的热固性组合物制成的密封剂(sealant)的半导体装置。
背景技术
底部填充技术广泛用于通过将半导体芯片面朝下倒装芯片接合到基材(board)上来制造半导体装置。具体地,根据底部填充技术,在将半导体芯片接合到基材上之后,基材和半导体芯片之间的间隙用树脂组合物填充并由此进行密封(参见,例如,专利文献1)。
最近,对作为射频(RF)装置运行的半导体装置的需求不断增加。换句话说,越来越需要半导体装置来发送、接收和处理RF信号。例如,需要用作机载雷达的组成元件的半导体装置来发送、接收和处理毫米波。需要满足相同的需求以建立下一代无线高速通信系统或将现有的有线设施改造成无线设施。
引用列表
专利文献
专利文献1:JP 2015-108155 A
发明概述
本发明的发明人特别注意密封剂对半导体装置的RF特性的影响。
本发明的一个目的是提供一种用作底部填充材料的热固性组合物,其用于密封在基材和面朝下接合到基材上的半导体芯片之间的间隙并且具有改善半导体装置的RF特性的能力,并且还提供包括由这样的用作底部填充材料的热固性组合物制成的密封剂的半导体装置。
根据本发明一个方面的用作底部填充材料的热固性组合物含有:单官能或双官能丙烯酸类化合物;热自由基聚合引发剂;二氧化硅;和包含1,2-乙烯基基团的弹性体。所述热固性组合物是液体并且具有当热固化时转变为固化产物的性质,所述固化产物具有在25℃为3.2以下的相对介电常数和在25℃为0.013以下的介电损耗角正切。
根据本发明另一个方面的半导体装置包括:基材;面朝下接合到基材上的半导体芯片;和配置成密封在所述基材和所述半导体芯片之间的间隙的密封剂。所述密封剂是所述用作底部填充材料的热固性组合物的固化产物。
附图简述
图1是举例说明根据本发明一个实施方案的半导体装置的示意性截面图。
实施方案描述
现在将描述本发明的实施方案。
根据此实施方案的用作底部填充材料的热固性组合物(下文称为组合物(X))用来制备用于半导体装置1的密封剂5。
首先,将描述半导体装置1。图1示出了半导体装置1的一个实例。此半导体装置1包括基材2、面朝下接合到基材2上的半导体芯片3以及用于密封在基材2和半导体芯片3之间的间隙的密封剂5。密封剂5是组合物(X)的固化产物。半导体芯片3包括在其面对基材2的表面上的多个凸起电极31,而基材2包括在其面对半导体芯片3的表面上的导体布线21。凸起电极31和导体布线21相对于彼此进行定位,并且经由焊料凸起4连接在一起。这些凸起电极31和导体布线21嵌入密封剂5中。
下面将描述用于制造此半导体装置1的方法。
首先,提供组合物(X)、基材2和半导体芯片3。
基材2可以例如是母板、插件板或转接板。基材2包括玻璃环氧树脂、聚酰亚胺、聚酯、陶瓷或任何其他合适材料的绝缘衬底以及由电导体如铜制成并且在绝缘衬底的表面上形成的导体布线21。
半导体芯片3可以是裸芯片或半导体封装,同时没有限制。半导体芯片3可以由GaAs、SiGe或任何其他合适的化合物半导体制成。半导体芯片3可以作为互补金属氧化物半导体(CMOS)芯片实现。凸起电极31设置在半导体芯片3的一个表面上。凸起电极31中的每一个均包括焊料凸起4。备选地,基材2上的导体布线21(而不是凸起电极31)可以包括焊料凸起4。仍然备选地,凸起电极31和导体布线21都可以包括焊料凸起4。也就是说,半导体芯片3的基材2上的凸起电极31和/或导体布线21可以包括焊料凸起4。焊料凸起4可以由熔点等于或高于210℃的无铅焊料如Sn-3.5Ag(熔点为221℃)、Sn-2.5Ag-0.5Cu-1Bi(熔点为214℃)、Sn-0.7Cu(熔点为227℃)或Sn-3Ag-0.5Cu(熔点为217℃)制成。
接下来,将半导体芯片3面朝下接合到基材2上。为此目的,将半导体芯片3相对于基材2定位并且布置在基材2上方的适当位置,使得半导体芯片3的凸起电极31精确地堆叠在基材2上的导体布线21上。在这种状态下,加热半导体芯片3和基材2以将焊料凸起4的温度升高到预定温度,该温度根据焊料凸起4的组成和密封用丙烯酸类组合物的化学组成而适当地设定,并且该温度可以落在例如180℃至300℃的范围内。加热焊料凸起4导致焊料凸起4熔化,从而将凸起电极31和导体布线21电连接在一起。
接下来,将组合物(X)注入到在基材2和半导体芯片3之间的间隙中。在此过程步骤中,根据需要,组合物(X)可以在被加热以使其粘度降低之后注入。在此时,组合物(X)可以加热至落在例如40℃至100℃范围内的温度。这使得组合物(X)可以流过在基材2和半导体芯片3之间的间隙以用该组合物(X)填充该间隙。
随后,将组合物(X)加热。这导致组合物(X)热固化并且转变为密封剂5。用于加热组合物(X)的条件根据组合物(X)的化学组成确定,并且可以包括例如80至150℃的加热温度和5至120分钟的加热持续时间。
以这种方式,制得包括基材2、半导体芯片3和密封剂5的半导体装置1。
在以上描述的实例中,在已将半导体芯片3接合到基材2上之后,在半导体芯片3和基材2之间的间隙用组合物(X)填充,然后使该组合物(X)固化以形成密封剂5。
然而,这不是制备密封剂5的唯一方法,而仅仅是一个示例。根据制备密封剂5的一种备选方法,在将半导体芯片3接合到基材2上之前,将组合物(X)涂布到半导体芯片3或基材2上。此后,将半导体芯片3布置在基材2上方的适当位置,使得组合物(X)插入在半导体芯片3和基材2之间。之后,将半导体芯片3电连接至基材2并且使组合物(X)固化以形成密封剂5。当密封剂5通过这样的方法制成时,组合物(X)称为例如预先提供的底部填充剂或非导电膏(NCP)。也就是说,组合物(X)可以例如是预先提供的底部填充剂或NCP。
接下来,将描述组合物(X)。组合物(X)含有热固性组分。组合物(X)是液体。当热固化时,组合物(X)转变为这样的固化产物,其具有在25℃为3.2以下的相对介电常数和在25℃为0.013以下的介电损耗角正切。
根据此实施方案,当热固化时,组合物(X)转变为具有低相对介电常数和低介电损耗角正切的密封剂5。在半导体装置1中的基材2和半导体芯片3之间插入这样的密封剂5使得该密封剂5可以改善半导体装置1的RF特性。
组合物(X)合适地含有:单官能或双官能丙烯酸类化合物;热自由基聚合引发剂;二氧化硅;和包含1,2-乙烯基基团的弹性体。组合物(X)合适地是液体并且合适地具有当热固化时转变为这样的固化产物的性质:该固化产物具有在25℃为3.2以下的相对介电常数和在25℃为0.013以下的介电损耗角正切。在这种情况下,将组合物(X)热固化使得可以获得具有特别低的相对介电常数、特别低的介电损耗角正切、高耐热性和高弹性的密封剂5。
固化产物的相对介电常数合适地至多等于2.8,并且更合适地为2.5以下。固化产物可以具有例如至少1.5的相对介电常数。然而,这仅仅是一个示例,而不应解释为限制性的。同时,固化产物的介电损耗角正切合适地至多等于0.01并且更合适地为0.08以下。固化产物可以具有例如至少0.002的介电损耗角正切。然而,这仅仅是一个示例,而不应解释为限制性的。
要注意的是,用于测量介电损耗角正切和相对介电常数的方法将在下文对于本发明的工作实施例描述评价试验时进行描述。
组合物(X)合适地具有在25℃为100Pa·s以下的粘度。这有利于利用在形成密封剂5中的组合物(X)来填充在半导体芯片3和基材2之间的间隙。
组合物(X)特别合适地在25℃为50Pa·s以下的粘度。在该情况下,组合物(X)可以具有良好的流动性。这特别是在已经将半导体芯片3接合到基材2上之后才将组合物(X)注入到在半导体芯片3和基材2之间的间隙中时,减少了组合物(X)不能充分填充该间隙的机会。要注意的是,用于测量粘度的方法将在下文对于本发明的工作实施例描述评价试验时进行描述。
组合物(X)合适地具有在25℃为2以下的触变指数。在该情况下,组合物(X)也可以具有良好的流动性。这特别是在已经将半导体芯片3接合到基材2上之后才将组合物(X)注入到在半导体芯片3和基材2之间的间隙中时,减少了组合物(X)不能充分填充该间隙的机会。触变指数更合适地至多等于1.5并且甚至更合适地为1.2以下。组合物(X)可以具有例如至少0.5的触变指数。然而,这仅仅是一个示例,而不应解释为限制性的。要注意的是,用于测量触变指数的方法将在下文对于本发明的工作实施例描述评价试验时进行描述。
特别地,组合物(X)合适地具有为10mm以上的侵入性试验评价值。在该情况下,组合物(X)即使在狭窄空间中也能够表现出优异的流动性。这特别是在已经将半导体芯片3接合到基材2上之后才将组合物(X)注入到在半导体芯片3和基材2之间的间隙中时,显著地减少了组合物(X)不能充分填充该间隙的机会。近来,随着半导体芯片3和基材2之间的间隙以及凸起电极31之间的间隔都变窄,对于增加半导体器件1中的半导体芯片3的尺寸的需求不断增加。即使在需要满足这样的需求时,仍然使组合物(X)可以在半导体芯片3和基材2之间足够平稳地流动,以减少不能充分填充间隙的机会。侵入性试验评价值更合适地至少等于20mm,并且甚至更合适地为50mm以上。要注意的是,用于进行侵入性试验的方法将在下文对于本发明的工作实施例描述评价试验时进行描述。
此外,组合物(X)的固化产物合适地具有等于或高于100℃的玻璃化转变温度。这使得半导体装置1可以具有优异的耐热性。玻璃化转变温度更合适地为至少高达125℃,并且甚至更合适地为150℃以上。要注意的是,用于测量玻璃化转变温度的方法将在下文对于本发明的工作实施例描述评价试验时进行描述。
固化产物合适地具有在等于或低于玻璃化转变温度的温度下为50ppm/℃以下的线性热膨胀系数。也就是说,当固化产物的温度等于或低于其玻璃化转变温度时,该固化产物的线性热膨胀系数(下文称为“CTE1”)合适地等于或小于50ppm/℃。
固化产物合适地具有在等于或高于玻璃化转变温度的温度下为120ppm/℃以下的线性热膨胀系数。也就是说,当固化产物的温度等于或高于其玻璃化转变温度时,该固化产物的线性热膨胀系数(下文称为“CTE2”)合适地等于或小于120ppm/℃。
要注意的是,用于测量CTE1和CTE2的方法将在下文对于本发明的工作实施例描述评价试验时进行描述。
具有这样的低线性热膨胀系数的固化产物减少了半导体装置1由于在密封剂5和半导体芯片3之间的线性膨胀系数方面的差异导致的翘曲和损坏。其中,最近已将应用扩展至RF装置的SiGe的半导体芯片和CMOS芯片,具有比GaAs的半导体芯片更低的线性热膨胀系数和更大的尺寸。因此,前一类型的半导体芯片比后一类型的半导体芯片更容易引起半导体器件1的翘曲和损坏。然而,即使在SiGe的半导体芯片中,此实施方案仍然能够减少半导体器件1的翘曲和损坏。
CTE1更合适地至多等于40ppm/℃,并且甚至更合适地为30ppm/℃以下。在实践中,CTE1至少等于10ppm/℃。然而,这仅仅是一个示例,而不应解释为限制性的。CTE2更合适地至多等于100ppm/℃,并且甚至更合适地为80ppm/℃以下。在实践中,CTE2至少等于30ppm/℃。然而,这仅仅是一个示例,而不应解释为限制性的。
组合物(X)合适地具有在150℃为至多100秒,更合适地为15秒以下的凝胶时间。这使得组合物具有优异的可固化性。凝胶时间可以通过以下方法测量。为了测量凝胶时间,一旦将1g的组合物(X)放在加热至150℃±2℃范围内的温度的热板上,立即用由聚四氟乙烯制成的搅拌夹具在每秒1转的条件下搅拌组合物(X)。凝胶时间是从组合物(X)搅拌开始至由于其粘度增加而不再能够搅拌之前所经过的时间量。
组合物(X)的反应开始温度合适地落在80℃至180℃的范围内,更合适地落在100℃至150℃的范围内,并且甚至更合适地落在100℃至130℃的范围内。反应开始温度可以通过以下方式测量:在大气中以10℃/min的升温速率和在30℃至300℃的温度范围内,使用例如DSC 7020(由Seiko Instruments Inc.制造)作为测量仪器,对放在铝盘上的组合物(X)进行差示扫描量热测定。在如此获得的热分析图中,将其基线与通过外推由反应产生的发热峰的上升梯度绘制的线之间的交叉点视为反应开始温度。
组合物(X)和固化产物这样的性质通过以下要描述的组合物(X)的化学组成实现。
如上所述,组合物(X)具有热固性组分。
热固性组分中所含的化合物合适地具有低极性。这降低固化产物的相对介电常数。为此目的,热固性组分中所含的化合物合适地不含或含有很少的N、O或S。
通过聚合热固性组分获得的结构合适地是刚性的。这降低固化产物的介电损耗角正切和线性热膨胀系数并且增加固化产物的玻璃化转变温度。为了实现此目的,热固性组分中所含的化合物合适地具有这样的大体积(bulky)结构,该结构具有许多烃骨架如叔丁基基团。
还推荐的是,通过聚合热固性组分获得的结构具有高的交联密度。这增大固化产物的玻璃化转变温度。
热固性组分含有环氧化合物或丙烯酸类化合物中的至少一种。
如果热固性组分含有环氧化合物,则该环氧化合物可以是每分子具有两个以上环氧基的化合物。环氧化合物可以含有至少一种选自由以下各项组成的组中的组分:双酚A型环氧化合物;双酚F型环氧化合物;联苯型环氧化合物;邻甲酚酚醛清漆型环氧化合物;二环戊二烯型环氧化合物;含萘环的环氧化合物;脂环族环氧化合物;含溴的环氧化合物;及其氢化的化合物。
其中,环氧化合物合适地具有萘骨架。这进一步增大玻璃化转变温度。还推荐的是,环氧化合物是具有低粘度的液体。在该情况下,即使当增大组合物(X)中的填料的含量时,组合物(X)仍然能够保持低粘度。因此,这不仅保持组合物(X)的粘度低,而且降低固化产物的线性热膨胀系数和介电损耗角正切。
如果热固性组分含有环氧化合物,则热固性组分合适地还含有固化剂。固化剂可以是任何化合物,只要该固化剂与环氧化合物反应并且使环氧化合物固化。固化剂含有至少一种选自由以下各项组成的组中的组分:酸酐,胺,咪唑,酚醛树脂,聚硫醇和氰酸酯。
相对于一当量的环氧化合物,固化剂的当量数可以落在0.6至1.4eq的范围内。
特别地,固化剂合适地含有酸酐。酸酐有助于降低组合物(X)的粘度。此外,在没有向其中添加固化剂的情况下,咪唑合适地以催化量添加至组合物(X),以在组合物(X)热固化时使环氧化合物自身发生聚合。这通过减小固化产物的极性来降低固化产物的相对介电常数。
如果热固性组分含有环氧化合物,则组合物合适地含有固化促进剂。固化促进剂可以含有至少一种选自由以下各项组成的组中的组分:胺系固化促进剂,聚酰胺系固化促进剂,咪唑系固化促进剂和路易斯酸系固化促进剂。固化促进剂合适地是所谓的“潜在性固化促进剂”,其在等于或高于特定温度的温度下发挥固化促进作用。这通过抑制组合物(X)的热固化而使组合物(X)保持良好流动性,同时使注入到在基材2和半导体芯片3之间的间隙中的组合物(X)在被加热以形成密封剂5之后可以流动。之后,将组合物(X)的温度升高以使固化促进剂发挥其促进组合物(X)的热固化的意图作用。这使组合物(X)可以充分均匀地在基材2和半导体芯片3之间的间隙上分布,由此减少不能用密封剂5充分填充间隙的机会。为此目的,固化促进剂合适地包封在微胶囊中。
相对于组合物(X)的固含量,固化促进剂的质量百分比可以落在例如0.1至60%的范围内。如本文使用的,“固含量”是指组合物(X)中要成为固化产物的组分并且不包括挥发性组分如溶剂。
特别地,固化促进剂合适地含有大体积的、咪唑系固化促进剂。这特别显著地减小固化产物的介电损耗角正切。还推荐的是,固化促进剂含有具有低熔点的高反应性的咪唑系固化促进剂。这减少固化催化剂的量,同时保持组合物(X)的良好的可固化性,由此减小固化产物的相对介电常数和介电损耗角正切。
此外,丙烯酸类化合物在本文是指包括(甲基)丙酰基的化合物。也就是说,丙烯酸类化合物是包含丙烯酰基或甲基丙烯酰基中的至少一种的化合物。丙烯酸类化合物可以含有具有(甲基)丙烯酰基的单体或具有(甲基)丙烯酰基的低聚物中的至少一种。
当组合物(X)含有丙烯酸类化合物时,在由组合物(X)制成的密封剂5中不太可能产生空隙。这应该是因为该组合物(X)在通过自由基聚合反应固化丙烯酸类化合物的初始阶段期间增大其粘度。
特别地,丙烯酸类化合物是单官能或双官能丙烯酸类化合物。也就是说,丙烯酸类化合物包括每个分子具有一个(甲基)丙烯酰基的单官能丙烯酸类化合物或每个分子具有两个(甲基)丙烯酰基的双官能丙烯酸类化合物中的至少一种。
为了确保密封剂5的耐热性,丙烯酸类化合物合适地包括每个分子具有两个(甲基)丙烯酰基的化合物(即,双官能丙烯酸类化合物)。
这样的各自每个分子具有两个(甲基)丙烯酰基的化合物的实例包括乙二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、1,9-壬二醇二(甲基)丙烯酸酯、1,3-丁二醇二(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯、二聚体二醇二(甲基)丙烯酸酯、二羟甲基三环癸烷二(甲基)丙烯酸酯、二乙二醇二(甲基)丙烯酸酯、三乙二醇二(甲基)丙烯酸酯、四乙二醇二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、三丙二醇二(甲基)丙烯酸酯、聚丙二醇二(甲基)丙烯酸酯、甘油二(甲基)丙烯酸酯、三羟甲基丙烷二(甲基)丙烯酸酯、季戊四醇二(甲基)丙烯酸酯、二(甲基)丙烯酸锌、环己烷二醇二(甲基)丙烯酸酯、环己烷二甲醇二(甲基)丙烯酸酯、环己烷二乙醇二(甲基)丙烯酸酯、环己烷二烷基醇二(甲基)丙烯酸酯和二甲醇三环癸烷二(甲基)丙烯酸酯。
这样的每个分子具有两个(甲基)丙烯酰基的化合物的实例包括在1摩尔的双酚A、双酚F或双酚AD和2摩尔的丙烯酸甘油醚酯之间的反应物以及在1摩尔的双酚A、双酚F或双酚AD和2摩尔的甲基丙烯酸甘油醚酯之间的反应物。
这样的每个分子具有两个(甲基)丙烯酰基的化合物的实例还包括具有交联的多环结构的(甲基)丙烯酸酯。这样的每个分子具有两个(甲基)丙烯酰基的化合物的具体实例包括由下式(I)表示的化合物和由下式(II)表示的化合物。含有由下式(I)表示的化合物或由下式(II)表示的化合物中的至少一种的组合物(X)特别显著地改善密封剂5的耐热性。
[化学式1]
在式(I)中,R1和R2各自彼此独立地表示氢原子或甲基,a是1或2,并且b是0或1。
[化学式2]
在式(II)中,R3和R4各自彼此独立地表示氢原子或甲基,X表示氢原子、甲基、羟甲基、氨基或(甲基)丙烯酰基氧基甲基,并且c是0或1。
具有交联多环结构的(甲基)丙烯酸酯的更具体实例包括:具有由式(I)表示的二环戊二烯骨架的(甲基)丙烯酸酯,其中a是1并且b是0;具有由式(II)表示的全氢-1,4:5,8-二羟甲基(dimethano)萘骨架的(甲基)丙烯酸酯,其中c是1;具有由式(II)表示的降莰烷骨架的(甲基)丙烯酸酯,其中c是0;由式(I)表示的二丙烯酸二环戊二烯基酯(三环癸烷二甲醇二丙烯酸酯),其中R1和R2各自表示氢原子、a=1并且b=0;由式(I)表示的二甲基丙烯酸二环戊二烯基酯(三环癸烷二甲醇二甲基丙烯酸酯),其中R1和R2各自表示甲基、a=1并且b=0;由式(II)表示的全氢-1,4:5,8-二羟甲基萘-2,3,7-三羟甲基三丙烯酸酯,其中X表示丙烯酰基氧基甲基,R3和R4各自表示氢原子,并且c是1;由式(II)表示的降莰烷二羟甲基二丙烯酸酯,其中X、R3和R4各自表示氢原子,并且c是0;和由式(II)表示的全氢-1,4:5,8-二羟甲基萘-2,3-二羟基二丙烯酸酯,其中X、R3和R4各自表示氢原子,并且c是1。
尤其是,具有交联多环结构的(甲基)丙烯酸酯合适地包括二丙烯酸二环戊二烯基酯(三环癸烷二羟甲基二丙烯酸酯)、二甲基丙烯酸二环戊二烯基酯(三环癸烷二羟甲基二甲基丙烯酸酯)或降莰烷二羟甲基二丙烯酸酯中的至少一种。也就是说,组合物(X)合适地包括二丙烯酸二环戊二烯基酯(三环癸烷二羟甲基二丙烯酸酯)、二甲基丙烯酸二环戊二烯基酯(三环癸烷二羟甲基二甲基丙烯酸酯)或降莰烷二羟甲基二丙烯酸酯中的至少一种。这些化合物有助于增大固化产物的玻璃化转变温度和降低组合物(X)的粘度。
这样的每个分子具有两个(甲基)丙烯酰基的化合物的实例还包括具有其中烯化氧加入到双酚骨架中的结构的二(甲基)丙烯酸酯。这样的每个分子具有两个(甲基)丙烯酰基的化合物的实例包括由下式(III)表示的化合物和由下式(IV)表示的化合物。含有由下式(III)表示的化合物或由下式(IV)表示的化合物中的至少一种的丙烯酸类化合物提高密封剂5、半导体芯片3和基材2之间的紧密接触的程度:
[化学式3]
在式(III)中,R5表示氢、甲基或乙基,R6表示二价有机基团,并且m和n各自表示落入1至20范围内的整数。
[化学式4]
在式(VI)中,R5表示氢、甲基或乙基,R6表示二价有机基团,并且m和n各自表示落入1至20范围内的整数。
具有这样的其中烯化氧加入到双酚骨架中的结构的二(甲基)丙烯酸酯的具体实例包括:EO改性的双酚A型二(甲基)丙烯酸酯(其中n=2至20)如ARONIX M-210和M-211B(由Toagosei Co.,Ltd.制造),以及NK酯ABE-300、A-BPE-4、A-BPE-6、A-BPE-10、A-BPE-20、A-BPE-30、BPE-100、BPE-200、BPE-500、BPE-900和BPE-1300N(由Shin-Nakamura ChemicalCo.,Ltd.制造);EO改性的双酚F型二(甲基)丙烯酸酯(其中n=2至20)如ARONIX M-208(由Toagosei Co.,Ltd.制造);PO改性的双酚A型二(甲基)丙烯酸酯(其中n=2至20)如DENACOLACRYLATE DA-250(由Nagase ChemteX Corporation制造)和VISCOAT 540(由OsakaOrganic Chemical Industry Ltd.制造);和PO改性的邻苯二甲酸二丙烯酸酯如DENACOLACRYLATE DA-721(由Nagase ChemteX Corporation制造)。
每个分子具有两个(甲基)丙烯酰基的化合物合适地包含环氧(甲基)丙烯酸酯。也就是说,丙烯酸类化合物合适地包含环氧(甲基)丙烯酸酯。在该情况下,含有环氧化合物的组合物(X)特别地不仅提高组合物(X)的反应性,而且也提高密封剂5的耐热性和紧密接触的程度。
环氧(甲基)丙烯酸酯例如是作为环氧化合物和不饱和一元酸如甲基丙烯酸之间的额外反应物的低聚物。
作为用于环氧(甲基)丙烯酸酯的材料的环氧化合物包括通过双酚如双酚A或双酚F和环氧卤丙烷之间的缩合反应获得的缩水甘油化合物(双酚型环氧化合物)。环氧化合物可以包括具有酚骨架的环氧化合物。具有酚骨架的环氧化合物的实例包括通过苯酚酚醛树脂(其是苯酚或甲酚和醛如福尔马林的缩合物)和环氧卤丙烷之间的缩合反应获得的聚缩水甘油醚(如苯酚-酚醛型环氧化合物和甲酚-酚醛型环氧化合物)。任选地,环氧化合物可以包括具有环己基环的环氧化合物。
环氧(甲基)丙烯酸酯合适地包括双酚A型环氧丙烯酸酯,其是在25℃为固体或粘度为10Pa·s以上的液体。双酚A型环氧丙烯酸酯可以例如由下式(V)表示:
[化学式5]
在式(V)中,n表示正整数。
商购可得的双酚A型环氧丙烯酸酯的实例包括DENACOL ACRYLATE DA-250(由Nagase ChemteX Corporation生产并且在25℃具有的粘度为60Pa·s)、DENACOL ACRYLATEDA-721(由Nagase ChemteX Corporation生产并且在25℃具有的粘度为100Pa·s),RIPOXYVR-60(由Showa High Polymers Co.,Ltd.生产;在常温下为固体)和RIPOXY VR-77(由Showa High Polymers Co.,Ltd.生产并且在25℃具有的粘度为100Pa·s)。
丙烯酸类化合物可以例如含有具有交联多环结构并且占整个丙烯酸类化合物的10-50质量%的(甲基)丙烯酸酯、具有其中烯化氧加入至双酚骨架中的结构并且占整个丙烯酸类化合物的3-20质量%的二(甲基)丙烯酸酯和占整个丙烯酸类化合物的5-30质量%的环氧(甲基)丙烯酸酯。
任选地,除了上述组分之外,丙烯酸类化合物还可以含有多种乙烯基单体中的任一种,如单官能乙烯基单体。
特别地,丙烯酸类化合物合适地含有具有二环戊二烯骨架的化合物。这样的具有二环戊二烯骨架的化合物有助于降低组合物(X)的粘度并且增大固化产物的玻璃化转变温度和减小固化产物的介电损耗角正切。
如果热固性组分含有丙烯酸类化合物,则该热固性组分还可以含有在末端带有具有可自由基聚合性的取代基的聚苯醚。聚苯醚可以包括聚苯醚链和键合至该聚苯醚链的末端的取代基。
取代基可以具有任何结构而没有限制,只要该取代基具有可自由基聚合性。取代基的实例包括具有碳碳双键的基团。
取代基合适地是具有碳碳双键的基团。在该情况下,取代基与丙烯酸类化合物的反应将聚苯醚结合到大分子的骨架中。这使得组合物(X)的固化产物表现出优异的耐热性和耐湿性。
例如,取代基可以具有由下式(1)表示的结构或由下式(2)表示的结构:
[化学式6]
在式(1)中,R表示氢或烷基。如果R是烷基,则该烷基合适地是甲基。
[化学式7]
在式(2)中,n是落入在0至10范围内的整数(例如,n=1),Z表示亚芳基,并且R1至R3各自彼此独立地表示氢或烷基。如果在式(2)中n=0,则Z直接键合至聚苯醚(C)的聚苯醚环(c1)的一端。
尤其是,取代基合适地具有由式(1)表示的结构。
聚苯醚可以具有由下式(3)表示的结构的化合物:
[化学式8]
在式(3)中,Y表示碳数为1至3的亚烷基或直接键。例如,Y可以是二甲基亚甲基。在式(3)中,X表示取代基,例如其可以具有由式(1)表示的结构的基团或由式(2)表示的结构的基团。尤其是,X合适地是具有由式(1)表示的结构的基团。此外,在式(3)中,s是等于或大于0的数,t也是等于或大于0的数,并且s和t的和是等于或大于1的数。具体地,s合适地是落入在0至20范围内的数,t合适地是落入在0至20范围内的数,并且s和t的和合适地是落入1至30范围内的数。
如果热固性组分含有聚苯醚,则聚苯醚与丙烯酸类化合物和聚苯醚的总质量的比率合适地落入在45质量%至70质量%范围内。当此比率等于或大于45质量%时,固化产物可以具有更高程度的耐热性。此外,当此比率等于或小于70质量%时,固化产物可以具有更高程度的柔韧性。该比率更合适地落入在50质量%至65质量%范围内。
如果热固性组分含有丙烯酸类化合物,则该热固性组分还可以含有引起与丙烯酸类化合物的热固化反应的另一种非聚苯醚化合物。这样的化合物的实例包括双马来酰亚胺树脂。
此外,如果热固性组分含有丙烯酸类化合物,则该热固性组分可以含有每分子具有三个以上的可自由基聚合官能团的交联助剂(下文简称为“交联助剂”)。也就是说,组合物(X)还可以含有交联助剂。可自由基聚合官能团例如可以是乙烯式不饱和键。
交联助剂中含有的化合物的实例包括各自每分子具有三个以上(甲基)丙烯酰基的化合物。具体地,这样的各自每分子具有三个以上(甲基)丙烯酰基的化合物的实例包括季戊四醇三丙烯酸酯、季戊四醇四丙烯酸酯、季戊四醇五丙烯酸酯、乙氧基化(3)三羟甲基丙烷三丙烯酸酯、乙氧基化(6)三羟甲基丙烷三丙烯酸酯、乙氧基化(9)三羟甲基丙烷三丙烯酸酯、丙氧基化(6)三羟甲基丙烷三丙烯酸酯、丙氧基化(3)甘油三丙烯酸酯、高度丙氧基化(55)甘油三丙烯酸酯、乙氧基化(15)三羟甲基丙烷三丙烯酸酯、三羟甲基丙烷三甲基丙烯酸酯、四乙二醇二丙烯酸酯、二羟甲基丙烷四丙烯酸酯、三丙二醇二丙烯酸酯、五丙烯酸酯、1,3-金刚烷-二醇二甲基丙烯酸酯、1,3-金刚烷-二醇二丙烯酸酯、1,3-金刚烷二羟甲基二甲基丙烯酸酯、1,3-金刚烷二羟甲基二丙烯酸酯和乙氧基化异氰尿酸三丙烯酸酯。交联助剂中含有的化合物的实例还包括异氰尿酸三烯丙烯基酯。交联助剂可以含有选自由这些化合物组成的组中的至少一种化合物。
交联助剂合适地含有具有三嗪骨架的化合物。也就是说,组合物(X)合适地含有具有三嗪骨架的交联助剂。尤其是,具有三嗪骨架的交联助剂有助于增大固化产物的玻璃化转变温度。这使得半导体装置1具有特别高程度的耐热性。这样的具有三嗪骨架的交联助剂含有乙氧基化异氰尿酸三丙烯酸酯或异氰尿酸三烯丙基酯中的至少一种。特别地,含有异氰尿酸三烯丙基酯的组合物(X)使得异氰尿酸三烯丙基酯有助于降低组合物(X)的粘度。
相对于组合物(X)中的丙烯酸类化合物的整个质量,组合物(X)中交联助剂的含量合适地落入在2质量%至50质量%范围内。在该情况下,交联助剂特别显著地有助于增大固化产物的玻璃化转变温度。添加的交联助剂的含量更合适地至少等于4.8质量%并且甚至更合适地为5质量%以上。添加的交联助剂的含量更合适地至多等于30质量%并且甚至更合适地为20.5质量%以下。
如果热固性组分含有丙烯酸类化合物,则组合物(X)合适地含有热自由基聚合引发剂。
热自由基聚合引发剂合适地具有在等于或高于一定温度的温度下引发热自由基聚合反应的能力。也就是说,热自由基聚合引发剂合适地具有潜伏期。这使得组合物(X)通过抑制组合物(X)的热固化而维持良好的可流动性,同时使得注入到基材2和半导体芯片3之间的间隙中的组合物(X)在被加热而形成密封剂5之后流动。之后,将组合物(X)的温度增加以使热自由基聚合引发剂发挥其加速组合物(X)的热固化的预期作用。这使得组合物(X)在基材2和半导体芯片3之间的间隙上充分均匀地分布,由此减少不能用密封剂5充分地填充间隙的机会。
热自由基聚合引发剂可以例如含有有机过氧化物。为了使有机过氧化物具有潜伏期,有机过氧化物合适地具有落入在100℃至200℃范围内的一分钟半衰期温度。
有机过氧化物的具体实例包括单碳酸叔丁基过氧-2-乙基己基酯(具有的一分钟半衰期温度为161.4℃)、过氧苯甲酸叔丁酯(具有的一分钟半衰期温度为166.8℃)、过氧化叔丁基枯基(具有的一分钟半衰期温度为173.3℃)、过氧化二枯基(具有的一分钟半衰期温度为175.2℃)、α-α′-二(叔丁基过氧化)二异丙基苯(具有的一分钟半衰期温度为175.4℃)、2,5-二甲基-2,5-二(叔丁基过氧化)己烷(具有的一分钟半衰期温度为179.8℃)、过氧化二-叔丁基(具有的一分钟半衰期温度为185.9℃)和2,5-二甲基-2,5-二(叔丁基过氧化)己炔(具有的一分钟半衰期温度为194.3℃)。
相对于100质量份的丙烯酸类化合物和引起与所述丙烯酸类化合物的热固化反应的组分,热自由基聚合引发剂的含量合适地落入0.25至2.0质量份的范围内。这使得固化产物具有良好的物理性能。热自由基聚合引发剂的含量更合适地落入在0.5至1.5质量份的范围内。
组合物(X)可以含有弹性体。弹性体有助于降低固化产物的弹性模量并且减少半导体装置1的翘曲和损伤。另外,弹性体还减少对于已重复加热的半导体装置1产生的损伤。此外,弹性体也进一步有助于降低固化产物的相对介电常数。
弹性体合适地含有具有1,2-乙烯基基团的化合物。也就是说,组合物(X)合适地还含有具有1,2-乙烯基基团的弹性体。这样的具有1,2-乙烯基基团的弹性体能够与组合物(X)中的丙烯酸类化合物反应,并且因此,不太可能降低固化产物的玻璃化转变温度。因此,具有1,2-乙烯基基团的弹性体使得半导体装置1维持良好的耐热性。
弹性体合适地含有液体丁二烯橡胶。尤其是,液体丁二烯橡胶有助于缓解固化产物中的应力。液体丁二烯橡胶还有助于降低固化产物的介电损耗角正切。液体丁二烯橡胶合适地包括氢化的液体丁二烯橡胶。氢化的液体丁二烯橡胶尤其有助于降低固化产物的介电损耗角正切。特别地,弹性体合适地含有具有1,2-乙烯基基团的液体聚丁二烯。
弹性体可以含有不同于液体丁二烯橡胶的另外的组分。例如,弹性体还可以含有具有马来酸酐作为加成物的异戊二烯聚合物,如马来酸酐改性的聚丁二烯。含有具有马来酸酐作为加成物的异戊二烯聚合物的组合物(X)使得具有马来酸酐作为加成物的异戊二烯聚合物进一步增大在半导体装置1中的密封剂5、半导体芯片3和基材2之间的密切接触程度。具有马来酸酐作为加成物的异戊二烯聚合物合适地具有1,2-乙烯基基团。
弹性体可以含有丁二烯-苯乙烯共聚物。含有丁二烯-苯乙烯共聚物的组合物(X)使得丁二烯-苯乙烯共聚物缓解固化产物中的应力,由此尤其有助于降低固化产物的介电损耗角正切。丁二烯-苯乙烯共聚物合适地包括1,2-乙烯基基团。
如果组合物(X)含有弹性体,则弹性体相对于整个组合物(X)的百分比合适地落入在5质量%至20质量%的范围内。当此百分比等于或大于5质量%时,固化产物的介电损耗角正切可特别显著地减小。当此百分比等于或小于20质量%时,不仅可减小组合物(X)的粘度的增加,而且也可减小固化产物的玻璃化转变温度的下降和线性热膨胀系数的增大。弹性体的百分比更合适地落入在6.4质量%至10.4质量%的范围内并且甚至更合适地落入在6.4质量%至8.2质量%的范围内。
任选地,组合物(X)还可以含有填料,只要合适,其可以是无机填料或有机填料。
含有无机填料的组合物(X)使得该无机填料有助于降低固化产物的线性热膨胀系数,并且由此减少半导体装置1的翘曲和损伤。另外,有机填料还有助于改善密封剂5的导热性,因此通过密封剂5有效地消散由半导体芯片3产生的热。
无机填料可以含有选自由以下各项组成的组中的至少一种材料:二氧化硅如熔融二氧化硅、合成二氧化硅、结晶二氧化硅或中空二氧化硅;金属氧化物如氧化铝和氧化钛;硅酸盐如滑石、煅烧粘土、未煅烧的粘土、云母和玻璃;碳酸盐如碳酸钙、碳酸镁和水滑石;氢氧化物如氢氧化铝、氢氧化镁和氢氧化钙;硫酸盐或亚硫酸盐如硫酸钡、硫酸钙和亚硫酸钙;硼酸盐如硼酸锌、偏硼酸钡、硼酸铝、硼酸钙和硼酸钠;和氮化物如氮化铝、氮化硼和氮化硅。只要合适,熔融二氧化硅可以是熔融球形二氧化硅或熔融粉碎二氧化硅。
无机填料合适地含有二氧化硅等。也就是说,组合物(X)合适地含有如上所述的二氧化硅。在这种情况下,二氧化硅尤其有助于增加固化产物的弹性并且降低其线性热膨胀系数和介电损耗因数。特别地,二氧化硅合适地含有中空二氧化硅。在这种情况下,中空二氧化硅有助于特别显着地降低固化产物的相对介电常数。中空二氧化硅合适地具有40至70%的孔隙率。
如果组合物(X)含有二氧化硅,则二氧化硅相对于整个组合物(X)的质量比合适地为至少20%,更合适地为30%以上,并且甚至更合适地为49%以上。二氧化硅的质量比合适地为70%以下,更合适地为73.9%以下,并且甚至更合适地为65%以下。
如果组合物(X)含有二氧化硅,则组合物(X)可以进一步含有有机填料或除二氧化硅之外的另一种无机填料中的至少一种。有机填料和其它非二氧化硅无机填料有助于特别显着地降低固化产物的相对介电常数。为了降低固化产物的相对介电常数,组合物(X)可以含有有机填料,并且有机填料可以含有四氟乙烯粒子。也就是说,组合物(X)合适地含有四氟乙烯粒子。
无机填料可以具有任何合适的形状而没有限制,其实例包括压碎、针状、片状和球形形状。为了改善无机填料在组合物(X)中的分散性以及控制组合物(X)的粘度,无机填料尤其合适地具有球形形状。
有机填料合适地含有氟碳聚合物粒子。氟碳聚合物的粒子有助于降低固化产物的相对介电常数。有机填料更合适地含有聚四氟乙烯粒子,其尤其有助于降低固化产物的相对介电常数。
填料合适地具有这样的平均粒度,其小于在基材2和粘合至基材2的半导体芯片3之间的间隙的尺寸。为了增加组合物(X)和密封剂5中的填料的填充密度并且为了调整组合物(X)的粘度,填料合适地具有的平均粒度为至多等于10μm,更合适地为5μm以下,并且甚至更合适地为3μm以下。例如,填料可以具有等于或大于0.1μm的平均粒度。然而,这仅仅是一个示例,而不应解释为限制性的。
组合物(X)的触变指数可以通过调整多种因素如填料的粒度分布、表面处理方法和比表面积来调控。
如本文使用的,“平均粒度”是指基于通过激光束衍射的粒度分布测量的结果计算的基于体积的中值直径。
为了调节组合物(X)的粘度或控制密封剂5的物理性能,填料可以含有具有不同平均粒度的两种以上组分。
相对于组合物(X)的固含量,填料的含量可以落入在10质量%至90质量%的范围内。
根据需要,组合物(X)还可以包括热塑性树脂、分散稳定剂、阻燃剂、弹性减低剂(elasticity reducer)、粘着赋予剂(增粘剂,adhesion imparting agent)、触变剂、着色剂、稀释剂、消泡剂、偶联剂、离子诱捕剂和/或自由基清除剂。特别地,含有偶联剂的组合物(X)使得该偶联剂提高在密封剂5、半导体芯片3和基材2之间的密切接触的程度。
组合物(X)可以含有溶剂。溶剂可以包括选自由以下各项组成的组中的至少一种:甲醇,乙醇,乙二醇单甲醚,乙二醇单乙醚,乙二醇单丁醚,甲乙酮,丙酮,异丙基酮,甲苯和二甲苯。溶剂的含量适当地设置以使组合物(X)具有合适的粘度。
实施例
接下来,将描述本发明的具体实施例。要注意的是,这些仅是本发明的示例并且不应解释为限制性的。
(1)组合物的制备
通过将表1的组成栏中所示的相应组分混合在一起来制备组合物。具体地,混合在一起的组分为:
-环氧化合物1:三官能缩水甘油胺型环氧树脂,其中环氧当量为95g/eq.;
-环氧化合物2:1,6-萘二醇二缩水甘油醚;
-固化剂1:3-甲基-六氢邻苯二甲酸酐;
-固化剂2:三烷基四氢邻苯二甲酸酐;
-固化促进剂:2-苯基-4-甲基咪唑;
-丙烯酸类化合物1:乙氧基化双酚A二甲基丙烯酸酯;
-丙烯酸类化合物2:双酚A型环氧丙烯酸酯,产品编号:VR-77(由Showa HighPolymers Co.,Ltd.生产);
-丙烯酸类化合物3:三环癸烷二羟甲基二甲基丙烯酸酯,产品编号DCP(由Shin-Nakamura Chemical Co.,Ltd.生产);
-交联助剂1:乙氧基化异氰尿酸三丙烯酸酯,产品编号A-9300(由Shin-NakamuraChemical Co.,Ltd.生产);
-交联助剂2:异氰尿酸三烯丙基酯;
-热自由基聚合引发剂:过氧化二枯基,产品名称Percumyl D(由NOF Corporation生产);
-弹性体1:具有1,2-乙烯基基团的马来酸酐改性的聚丁二烯,产品编号Ricobond1756(由Cray Valley Ltd.生产);
-弹性体2:不具有1,2-乙烯基基团的液体丁二烯橡胶,产品编号LBR 307(由Kuraray Co.,Ltd.生产生产);
-弹性体3:不具有1,2-乙烯基基团的液体聚丁二烯,产品编号Polyvest 110(由Evonik Japan生产);
-弹性体4:具有1,2-乙烯基基团的丁二烯-苯乙烯共聚物,产品编号Ricon 100(由Cray Valley Ltd.生产);
-偶联剂:3-丙烯酰氧基丙基三甲氧基硅烷,产品编号KBM-5103(由Shin-EtsuChemical Co.,Ltd.生产);
-无机填料1:平均粒度为1.0μm的球形二氧化硅;
-无机填料2:平均粒度为15μm、孔隙率为70%并且比重为0.6的中空二氧化硅;和
-无机填料3:平均粒度为1.5μm的球形二氧化硅。
(2)评价试验
使组合物经过以下评价试验。结果示于表1的“评价”栏。
(2-1)粘度测量
组合物的粘度在包括转子直径为8.74mm、温度为25℃并且转数为50rpm的条件下通过B型粘度计(产品编号DV-II,由Brookfield Asset Management Inc.制造)进行测量。
(2.2)触变指数的测量
组合物的粘度在包括转子直径为8.74mm、温度为25℃并且转数为5rpm和50rpm的条件下通过B型粘度计(产品编号DV-II,由Brookfield Asset Management Inc.制造)进行测量。获得在转数为5rpm测得的粘度μ5与在转数为50rpm测得的粘度μ50的比率μ5/μ50作为触变指数。
(2.3)玻璃化转变温度的测量
将组合物倒入到有机硅模具中并在150℃加热一小时以制备尺寸为20mm×40mm×3mm的固化产物。
在包括压缩力为9.8mN、升温速率为5℃/min和30至300℃的温度范围的条件下,使固化产物经过利用热力学分析仪(产品编号SS 7100,由Seiko Instruments Inc.制造)的热力学分析。其玻璃化转变温度基于分析的结果获得。
(2-4)在等于或低于玻璃化转变温度的温度下测量线性热膨胀系数(CTE1)
固化产物的热力学分析在与测量玻璃化转变温度的相同条件下进行。固化产物的线性热膨胀系数基于在从30℃至比玻璃化转变温度低15℃的温度的温度范围内所获得的结果进行计算。
(2-5)在等于或高于玻璃化转变温度的温度下测量线性热膨胀系数(CTE2)
固化产物的热力学分析在与测量玻璃化转变温度的相同条件下进行。固化产物的线性热膨胀系数基于在从比玻璃化转变温度高15℃的温度至300℃的温度范围内获得的结果进行计算。
(2-6)相对介电常数和介电损耗角正切的测量
将组合物倒入到有机硅制成的模具中,在30分钟内从室温加热至100℃,在100℃保持60分钟,在15分钟内再次加热至150℃,在150℃保持60分钟,然后在30分钟内冷却至室温,由此获得尺寸为2mm×2mm×50mm的具有四边形棱镜形状的固化产物。
将该固化产物在30分钟内加热至120℃,然后在25℃在30%RH气氛中留置一天。
此固化产物在25℃的相对介电常数和介电损耗角正切通过腔微扰法(cavityresonator perturbation method)测量。此测量利用网络分析仪(产品编号N5230A,由Keysight Technologies Inc.制造)做额外测量仪器在20GHz的测量频率进行,其中测量期间电场的方向与固化产物的长度一致。
(2-7)热循环试验
半导体装置利用此组合物以以下方式制作。
作为基材,提供尺寸为10mm×10mm×300μm的Walts TEG IP80(由WALTS Co.,Ltd.制造)。
作为半导体晶片,提供尺寸为7.3mm×7.3mm×100μm的Walts TEG CC80(由WALTSCo.,Ltd.制造)。该半导体晶片包括1048个凸起电极,其每一个包括高度为30μm的Cu柱和堆叠在其上且高度为15μm的焊料凸起,并且每对相邻焊料凸起之间的间距为80μm。将此半导体晶片利用砂轮划片机进行切割以获得各自尺寸为7.3mm×7.3mm的半导体芯片。
然后,将半导体芯片的每一个布置在基材上,以使得凸起电极安装在基材上的导体布线上,然后加热以熔化凸起电极的焊料凸起。之后,使熔化的焊料凸起固化,由此将凸起电极电连接至导体布线。
随后,倒入组合物以填充基材和半导体芯片之间的间隙,然后加热至150℃持续一小时,并由此固化以形成密封剂。以这种方式,获得半导体装置。
使此半导体装置经过温度循环试验,其一个循环包括将半导体装置在-55℃的环境暴露30分钟,然后将该半导体装置在125℃的环境暴露30分钟。将在位于还要进行测试的半导体装置的外周周围的凸起电极和导体布线之间的电阻值与经过该测试的半导体装置的电阻值进行比较。将甚至在经过此测试的1000个循环之后仍保持不变的半导体装置评价为A级。将在经过此测试的500个循环之后仍保持不变的半导体装置评价为B级。在经过此测试的500个循环之后显著变化的半导体装置评价为C级。
权利要求书(按照条约第19条的修改)
1.一种用作底部填充材料的热固性组合物,所述热固性组合物包含:
单官能或双官能丙烯酸类化合物;
热自由基聚合引发剂;
二氧化硅;和
包含1,2-乙烯基基团的弹性体,
所述热固性组合物是液体并且具有当热固化时转变为固化产物的性质,所述固化产物具有在25℃为3.2以下的相对介电常数和在25℃为0.013以下的介电损耗角正切。
2.(当前修改)根据权利要求1所述的用作底部填充材料的热固性组合物,所述热固性组合物还包含每个分子具有三个以上的可自由基聚合官能团的交联助剂。
3.根据权利要求1或2所述的用作底部填充材料的热固性组合物,其中
所述热固性组合物具有在25℃为100Pa·s以下的粘度。
4.根据权利要求1至3中任一项所述的用作底部填充材料的热固性组合物,其中
所述固化产物具有等于或高于100℃的玻璃化转变温度。
5.根据权利要求1至4中任一项所述的用作底部填充材料的热固性组合物,其中
所述固化产物具有在等于或低于玻璃化转变温度的温度下为50ppm/℃以下的线性热膨胀系数。
6.根据权利要求1至5中任一项所述的用作底部填充材料的热固性组合物,其中
所述固化产物具有在等于或高于玻璃化转变温度的温度下为120ppm/℃以下的线性热膨胀系数。
7.一种半导体装置,所述半导体装置包括:
基材;
面朝下接合到所述基材上的半导体芯片;和
配置成密封在所述基材和所述半导体芯片之间的间隙的密封剂,
所述密封剂是根据权利要求1至6中任一项所述的用作底部填充材料的热固性组合物的固化产物。
Claims (7)
1.一种用作底部填充材料的热固性组合物,所述热固性组合物包含:
单官能或双官能丙烯酸类化合物;
热自由基聚合引发剂;
二氧化硅;和
包含1,2-乙烯基基团的弹性体,
所述热固性组合物是液体并且具有当热固化时转变为固化产物的性质,所述固化产物具有在25℃为3.2以下的相对介电常数和在25℃为0.013以下的介电损耗角正切。
2.根据权利要求1或2所述的用作底部填充材料的热固性组合物,所述热固性组合物还包含每个分子具有三个以上的可自由基聚合官能团的交联助剂。
3.根据权利要求1或2所述的用作底部填充材料的热固性组合物,其中
所述热固性组合物具有在25℃为100Pa·s以下的粘度。
4.根据权利要求1至3中任一项所述的用作底部填充材料的热固性组合物,其中
所述固化产物具有等于或高于100℃的玻璃化转变温度。
5.根据权利要求1至4中任一项所述的用作底部填充材料的热固性组合物,其中
所述固化产物具有在等于或低于玻璃化转变温度的温度下为50ppm/℃以下的线性热膨胀系数。
6.根据权利要求1至5中任一项所述的用作底部填充材料的热固性组合物,其中
所述固化产物具有在等于或高于玻璃化转变温度的温度下为120ppm/℃以下的线性热膨胀系数。
7.一种半导体装置,所述半导体装置包括:
基材;
面朝下接合到所述基材上的半导体芯片;和
配置成密封在所述基材和所述半导体芯片之间的间隙的密封剂,
所述密封剂是根据权利要求1至6中任一项所述的用作底部填充材料的热固性组合物的固化产物。
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KR20230152659A (ko) * | 2021-02-22 | 2023-11-03 | 가부시끼가이샤 레조낙 | 수지 조성물, 경화물, 적층체, 투명 안테나 및 그 제조방법, 및, 화상 표시 장치 |
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