JP2012224799A - Liquid sealing resin composition and semiconductor device using the same - Google Patents

Liquid sealing resin composition and semiconductor device using the same Download PDF

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JP2012224799A
JP2012224799A JP2011095645A JP2011095645A JP2012224799A JP 2012224799 A JP2012224799 A JP 2012224799A JP 2011095645 A JP2011095645 A JP 2011095645A JP 2011095645 A JP2011095645 A JP 2011095645A JP 2012224799 A JP2012224799 A JP 2012224799A
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resin composition
sealing resin
liquid sealing
semiconductor device
liquid
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Hiroshi Ito
浩志 伊藤
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Sumitomo Bakelite Co Ltd
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Sumitomo Bakelite Co Ltd
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Priority to JP2011095645A priority Critical patent/JP2012224799A/en
Priority to PCT/JP2012/059545 priority patent/WO2012144355A1/en
Priority to TW101113649A priority patent/TW201311790A/en
Publication of JP2012224799A publication Critical patent/JP2012224799A/en
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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
    • H01L23/295—Organic, e.g. plastic containing a filler
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
    • C08G59/686—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used containing nitrogen
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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    • 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
    • H01L24/10—Bump connectors ; Manufacturing methods related thereto
    • H01L24/11—Manufacturing methods
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
    • H01L24/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
    • H01L24/81—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a bump connector
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • 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
    • 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
    • H01L2224/10—Bump connectors; Manufacturing methods related thereto
    • H01L2224/15—Structure, shape, material or disposition of the bump connectors after the connecting process
    • H01L2224/16—Structure, shape, material or disposition of the bump connectors after the connecting process of an individual bump connector
    • H01L2224/161—Disposition
    • H01L2224/16151—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
    • H01L2224/16221—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
    • H01L2224/16225—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being non-metallic, e.g. insulating substrate with or without metallisation
    • 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
    • H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L2224/31—Structure, shape, material or disposition of the layer connectors after the connecting process
    • H01L2224/32—Structure, shape, material or disposition of the layer connectors after the connecting process of an individual layer connector
    • H01L2224/321—Disposition
    • H01L2224/32151—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
    • H01L2224/32221—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
    • H01L2224/32225—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being non-metallic, e.g. insulating substrate with or without metallisation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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    • H01L2224/73—Means for bonding being of different types provided for in two or more of groups H01L2224/10, H01L2224/18, H01L2224/26, H01L2224/34, H01L2224/42, H01L2224/50, H01L2224/63, H01L2224/71
    • H01L2224/732—Location after the connecting process
    • H01L2224/73201—Location after the connecting process on the same surface
    • H01L2224/73203—Bump and layer connectors
    • H01L2224/73204—Bump and layer connectors the bump connector being embedded into the layer connector
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • 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
    • H01L2224/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
    • H01L2224/81—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a bump connector
    • H01L2224/8119—Arrangement of the bump connectors prior to mounting
    • H01L2224/81191—Arrangement of the bump connectors prior to mounting wherein the bump connectors are disposed only on the semiconductor or solid-state body
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    • H01L2224/91—Methods for connecting semiconductor or solid state bodies including different methods provided for in two or more of groups H01L2224/80 - H01L2224/90
    • H01L2224/92—Specific sequence of method steps
    • H01L2224/921—Connecting a surface with connectors of different types
    • H01L2224/9212—Sequential connecting processes
    • H01L2224/92122—Sequential connecting processes the first connecting process involving a bump connector
    • H01L2224/92125—Sequential connecting processes the first connecting process involving a bump connector the second connecting process involving a layer connector
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    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
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    • H01L2924/35—Mechanical effects
    • H01L2924/351—Thermal stress

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  • Condensed Matter Physics & Semiconductors (AREA)
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  • Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
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Abstract

PROBLEM TO BE SOLVED: To provide a liquid sealing resin composition having high thermal conductivity and high gap inflow properties in combination.SOLUTION: There is provided the liquid sealing resin composition used in sealing a gap between a semiconductor element and a substrate after the semiconductor element and the substrate are bump-connected. The liquid sealing resin composition contains (A) an epoxy resin, (B) a curing agent, and (C) an inorganic filler. where (C) the inorganic filler contains a mixture of (1) spherical alumina with an average diameter of ≥0.5 μm and <1.0 μm and (2) spherical alumina with an average diameter of ≥1.0 μm and <3.0 μm. The liquid sealing resin composition further contains (D) a basic compound, and preferably has a pH of >7.

Description

本発明は高熱伝導率と高隙間流入性とを兼備した液状封止樹脂組成物、及びその液状封止樹脂組成物を用いたバンプ接続方式の半導体装置に関する。 The present invention relates to a liquid sealing resin composition having both high thermal conductivity and high gap inflow property, and a bump connection type semiconductor device using the liquid sealing resin composition.

近年様々な電子情報処理機器には、狭い面積に高密度実装することが可能なバンプ接続方式の半導体装置が広く用いられるようになってきている。そのようなバンプ接続方式の半導体装置では、半導体素子をバンプによって電気的に接続した後、接続信頼性を向上するために、アンダーフィル材と呼ばれる液状封止樹脂をバンプ接続部へ充填して硬化させ、接続バンプ周辺を補強するのが一般的である。   In recent years, bump connection type semiconductor devices capable of high-density mounting in a small area have been widely used in various electronic information processing devices. In such a bump connection type semiconductor device, after electrically connecting semiconductor elements by bumps, in order to improve connection reliability, a liquid sealing resin called an underfill material is filled into the bump connection portion and cured. In general, the periphery of the connection bump is reinforced.

また一方で高度情報化社会進展の一端として、あらゆる情報が電子データ化され、それを瞬時に処理して伝達する必要にも迫られてきており、さらに低炭素社会の実現など環境問題への対応も必須とされていることから、大容量の電子データを高速且つ低消費電力で処理できる安価な電子情報処理機器が求められてきている。それに伴って機器に組み入れられる半導体装置にも、より低消費電力で安定した高速動作の可能なことが求められており、そのため半導体装置の発熱対策も重要になってきたことから、バンプ接続方式の半導体装置に用いられる液状封止樹脂に対しても高い熱伝導性が必要になってきている。
さらに、電子情報処理機器の低価格化を実現するために、半導体装置は小型・薄型化が進んできており、近年ではバンプ接続方式の半導体装置における接続部の隙間やバンプ間隔は１００μｍに満たないものがほとんどで、今後もますます微細化が進むとみられるため、用いられる液状封止樹脂にはいっそう高い隙間流入性が求められてきている。このように、高い熱伝導性と高い隙間流入性とを兼備した液状封止樹脂が求められてきた。 At the same time, as part of the advancement of an advanced information society, there is an urgent need for all information to be converted into electronic data, processed and transmitted instantly, and to address environmental issues such as the realization of a low-carbon society. Therefore, an inexpensive electronic information processing device capable of processing a large amount of electronic data with high speed and low power consumption has been demanded. Along with this, semiconductor devices incorporated in equipment are also required to be capable of stable high-speed operation with lower power consumption. For this reason, countermeasures against heat generation of semiconductor devices have become important. High thermal conductivity is also required for liquid sealing resins used in semiconductor devices.
Furthermore, in order to realize a reduction in the price of electronic information processing equipment, semiconductor devices are becoming smaller and thinner. In recent years, the gaps and bump spacings of connection portions in bump connection type semiconductor devices are less than 100 μm. Since most of them are expected to become increasingly finer in the future, the liquid sealing resin used is required to have higher gap inflow properties. Thus, a liquid sealing resin having both high thermal conductivity and high gap inflow has been demanded.

従来、半導体装置用液状封止樹脂には熱時寸法の安定性や強度保持のためシリカフィラーを含有するのが一般的であったが、熱伝導性を改善するためには比較的熱伝導性の低いシリカフィラーに替えて、より高い熱伝導性のフィラーをできるだけ多く含有するのが一般的であり、窒化ケイ素や窒化アルミニウム、アルミナ、酸化マグネシウムなどの高熱伝導性フィラーを使用できることは広く知られている。
それらの中で、例えば球状アルミナを用いたものとして、平均粒径２〜３０μｍであり、且つ粒径２４μｍ以上の粒子を１５％以上、１μｍ以下の粒子を３％以上含有する球状アルミナを含有したものが提案されている（特許文献１参照）。しかし、この技術では２４μｍ以上の粒子を１５％以上含有していることを必要とすることから、バンプ接続部の隙間やバンプとバンプの間へフィラーが詰まる可能性が高くなるため、ますます微細化する傾向にある半導体装置への適用には限界があった。一方、前述に比べてより小さい径の球状アルミナを用いることで、そのような問題に対応するものとして、平均粒子径が１〜５μｍ、最大粒子径が２０μｍ以下で、１０μｍを超える粒子の構成割合が１０質量％未満の球状アルミナを組成物全体の６０〜９０質量％含有するものも提案されている（特許文献２参照）。しかしこの技術では流動性に問題が生じるとの理由から、平均径１μｍ未満のアルミナを用いることはできなかった。その結果、平均径１μｍ以下のアルミナを用いることでアルミナの充填度をアップし、高熱伝導化を図ることは困難であった。さらに、平均径１μｍ未満のフィラーを用いるものとして、平均粒径１〜３０μｍのアルミナと平均粒径０．１〜３０μｍのシリカの混合物に、さらに平均粒径０．１μｍ未満の超微粉無機充填材を全樹脂組成物中に４４〜７５体積％含むものなども提案されている（特許文献３）。しかし、アルミナと比べて熱伝導性の低いシリカを併用する必要があることから、アルミナだけを含有したものに比べ熱伝導性が低下することは避ける事が出来ないという問題があった。 Conventionally, a liquid sealing resin for semiconductor devices generally contains a silica filler in order to maintain the thermal dimension stability and strength, but in order to improve thermal conductivity, it is relatively thermal conductive. It is common to contain as much heat-conductive filler as possible instead of low-silica filler, and it is widely known that high heat-conductive fillers such as silicon nitride, aluminum nitride, alumina, and magnesium oxide can be used. ing.
Among them, for example, using spherical alumina, it contains spherical alumina having an average particle diameter of 2 to 30 μm and containing particles having a particle diameter of 24 μm or more of 15% or more and 1 μm or less of 3% or more. The thing is proposed (refer patent document 1). However, this technology requires 15% or more particles of 24μm or more, so the possibility of clogging filler between gaps between bumps and between bumps increases. There has been a limit to application to semiconductor devices that tend to be integrated. On the other hand, by using spherical alumina having a smaller diameter than that described above, the composition ratio of particles having an average particle diameter of 1 to 5 μm, a maximum particle diameter of 20 μm or less, and exceeding 10 μm as a countermeasure to such a problem. Has also been proposed that contains spherical alumina of less than 10% by mass of 60 to 90% by mass of the total composition (see Patent Document 2). However, alumina with an average diameter of less than 1 μm could not be used because this technique causes problems in fluidity. As a result, it was difficult to increase the filling degree of alumina by using alumina having an average diameter of 1 μm or less and to achieve high thermal conductivity. Further, as a filler using an average particle diameter of less than 1 μm, an ultrafine inorganic filler having an average particle diameter of less than 0.1 μm is added to a mixture of alumina having an average particle diameter of 1 to 30 μm and silica having an average particle diameter of 0.1 to 30 μm. Have been proposed in which the total resin composition contains 44 to 75% by volume (Patent Document 3). However, since it is necessary to use silica having a low thermal conductivity as compared with alumina, there is a problem that it is unavoidable that the thermal conductivity is lowered as compared with those containing only alumina.

特許第２６４３７１４号公報Japanese Patent No. 2644314 特開２００８−２７４０８３号公報JP 2008-274083 A 特開２０１０−１１８６４９号公報JP 2010-118649 A

本発明の目的は、従来は実現が困難であった高い熱伝導率と高い隙間流入性とを兼備した液状封止樹脂組成物を提供することである。   An object of the present invention is to provide a liquid encapsulating resin composition having both high thermal conductivity and high gap inflow properties that have been difficult to realize in the past.

本発明は以下の通りである。
［１］半導体装置の組立に用いる液状封止樹脂組成物であって、（Ａ）液状エポキシ樹脂、（Ｂ）アミン系硬化剤、（Ｃ）無機充填材を含有し、（Ｃ）無機充填材が平均径０．５μｍ以上１．０μｍ未満の球状アルミナ（１）と平均径１．０μｍ以上３．０μｍ未満の球状アルミナ（２）との混合物を含有し、且つ（Ｄ）塩基性化合物を含有することを特徴とする液状封止樹脂組成物。
［２］ｐＨ値が７を超えるものである［１］記載の液状封止樹脂組成物。
［３］（Ｄ）塩基性化合物が、１，８−ジアザビシクロ（５．４．０）ウンデセン−７、１，５−ジアザビシクロ（４．３．０）ノネン−５、およびそれらの塩のうち少なくとも１種類である［１］又は［２］記載の液状封止樹脂組成物。
［４］（Ｃ）無機充填材の含有量が８０質量％以上であって、そのうち（Ｃ）無機充填剤に占める０．５μｍ以上１．０μｍ未満の球状アルミナ（１）の割合が５質量％以上５０質量％未満である［１］〜［３］いずれかに記載の液状封止樹脂組成物。
［５］［１］〜［４］いずれかに記載の液状封止樹脂組成物の硬化物で封止されていることを特徴とする半導体装置。
［６］［１］〜［４］いずれかに記載の液状封止樹脂組成物を充填する充填工程を有することを特徴とする半導体装置の製造方法。 The present invention is as follows.
[1] A liquid sealing resin composition used for assembling a semiconductor device, which contains (A) a liquid epoxy resin, (B) an amine-based curing agent, (C) an inorganic filler, and (C) an inorganic filler. Contains a mixture of spherical alumina (1) having an average diameter of 0.5 μm or more and less than 1.0 μm and spherical alumina (2) having an average diameter of 1.0 μm or more and less than 3.0 μm, and (D) containing a basic compound A liquid sealing resin composition characterized by comprising:
[2] The liquid sealing resin composition according to [1], wherein the pH value exceeds 7.
[3] (D) the basic compound is at least one of 1,8-diazabicyclo (5.4.0) undecene-7, 1,5-diazabicyclo (4.3.0) nonene-5, and salts thereof The liquid sealing resin composition according to [1] or [2], which is one kind.
[4] The content of (C) inorganic filler is 80% by mass or more, and the proportion of spherical alumina (1) of 0.5 μm or more and less than 1.0 μm in (C) inorganic filler is 5% by mass. The liquid sealing resin composition according to any one of [1] to [3], which is less than 50% by mass.
[5] A semiconductor device which is sealed with a cured product of the liquid sealing resin composition according to any one of [1] to [4].
[6] A method for manufacturing a semiconductor device comprising a filling step of filling the liquid sealing resin composition according to any one of [1] to [4].

本発明によれば、高い熱伝導率と高い隙間流入性とを兼備した液状封止樹脂組成物の提供を可能にし、それを用いて組み立てられたバンプ接続方式の半導体装置の発熱対策や小型・薄型化を可能にすることで、低消費電力で安定した高速動作が可能な半導体装置を得ることができる   According to the present invention, it is possible to provide a liquid sealing resin composition having both high thermal conductivity and high gap inflow property, and it is possible to prevent heat generation and to reduce the size and size of a bump connection type semiconductor device assembled using the liquid sealing resin composition. By enabling thinning, a semiconductor device capable of stable high-speed operation with low power consumption can be obtained.

以下、本発明の液状封止樹脂組成物および半導体装置について説明する。
本発明は、半導体素子をバンプ接続した後、接続部の隙間を封止する際に用いる液状封止樹脂組成物であって、（Ａ）エポキシ樹脂、（Ｂ）硬化剤、（Ｃ）無機充填材を含有し、（Ｃ）無機充填材が平均径０．５μｍ以上１．０μｍ未満の球状アルミナ（１）と平均径１．０μｍ以上３．０μｍ未満の球状アルミナ（２）との混合物を含有し、且つ（Ｄ）塩基性化合物を含有することを特徴とする液状封止樹脂組成物、及び該液状封止樹脂組成物の硬化物で封止された半導体装置である。 Hereinafter, the liquid sealing resin composition and the semiconductor device of the present invention will be described.
The present invention relates to a liquid sealing resin composition used for sealing a gap of a connecting portion after bump connection of a semiconductor element, and includes (A) an epoxy resin, (B) a curing agent, and (C) an inorganic filling. And (C) a mixture of spherical alumina (1) having an average diameter of 0.5 μm or more and less than 1.0 μm and spherical alumina (2) having an average diameter of 1.0 μm or more and less than 3.0 μm. And (D) a liquid encapsulating resin composition containing a basic compound, and a semiconductor device encapsulated with a cured product of the liquid encapsulating resin composition.

まず、液状封止樹脂組成物について説明する。
本発明の液状封止樹脂組成物は、エポキシ樹脂（Ａ）を含む。これにより、硬化後の封止樹脂脂組成物が耐熱性、耐湿性、機械的強度に優れ、且つバンプ接続部を強固に接着することができる。そのため、信頼性に優れた半導体装置を得ることができる。
エポキシ樹脂（Ａ）としては、一分子中にエポキシ基を２個以上有するものであれば特に分子量や構造は限定されるものではないが、例えば、フェノールノボラック型エポキシ樹脂、クレゾールノボラック型エポキシ樹脂などのノボラック型エポキシ樹脂、ビスフェノールＡ型エポキシ樹脂、ビスフェノールＦ型エポキシ樹脂などのビスフェノール型エポキシ樹脂、Ｎ，Ｎ−ジグリシジルアニリン、Ｎ，Ｎ−ジグリシジルトルイジン、ジアミノジフェニルメタン型グリシジルアミン、アミノフェノール型グリシジルアミンなどの芳香族グリシジルアミン型エポキシ樹脂、ハイドロキノン型エポキシ樹脂、ビフェニル型エポキシ樹脂、スチルベン型エポキシ樹脂、トリフェノールメタン型エポキシ樹脂、トリフェノールプロパン型エポキシ樹脂、アルキル変性トリフェノールメタン型エポキシ樹脂、トリアジン核含有エポキシ樹脂、ジシクロペンタジエン変性フェノール型エポキシ樹脂、ナフトール型エポキシ樹脂、ナフタレン型エポキシ樹脂、フェニレンおよび／またはビフェニレン骨格を有するフェノールアラルキル型エポキシ樹脂、フェニレンおよび／またはビフェニレン骨格を有するナフトールアラルキル型エポキシ樹脂などのアラルキル型エポキシ樹脂などのエポキシ樹脂、ビニルシクロヘキセンジオキシド、ジシクロペンタジエンオキシド、アリサイクリックジエポキシ−アジペイドなどの脂環式エポキシなどの脂肪族エポキシ樹脂が挙げられる。 First, the liquid sealing resin composition will be described.
The liquid sealing resin composition of the present invention contains an epoxy resin (A). Thereby, the cured resin resin composition after curing is excellent in heat resistance, moisture resistance and mechanical strength, and the bump connecting portion can be firmly bonded. Therefore, a semiconductor device with excellent reliability can be obtained.
The epoxy resin (A) is not particularly limited in molecular weight and structure as long as it has two or more epoxy groups in one molecule. For example, a phenol novolac type epoxy resin, a cresol novolak type epoxy resin, etc. Bisphenol epoxy resins such as novolak epoxy resin, bisphenol A epoxy resin, bisphenol F epoxy resin, N, N-diglycidylaniline, N, N-diglycidyltoluidine, diaminodiphenylmethane type glycidylamine, aminophenol type glycidyl Aromatic glycidylamine type epoxy resin such as amine, hydroquinone type epoxy resin, biphenyl type epoxy resin, stilbene type epoxy resin, triphenolmethane type epoxy resin, triphenolpropane type epoxy resin Alkyl-modified triphenolmethane type epoxy resin, triazine nucleus-containing epoxy resin, dicyclopentadiene-modified phenol type epoxy resin, naphthol type epoxy resin, naphthalene type epoxy resin, phenol aralkyl type epoxy resin having phenylene and / or biphenylene skeleton, phenylene and / Or epoxy resins such as aralkyl epoxy resins such as naphthol aralkyl type epoxy resins having a biphenylene skeleton, and aliphatic epoxies such as alicyclic epoxies such as vinylcyclohexene dioxide, dicyclopentadiene oxide, alicyclic diepoxy-adipade Resin.

さらに本発明の場合、芳香族環にグリシジル構造またはグリシジルアミン構造が結合した構造を含むものが耐熱性、機械特性、耐湿性という観点からより好ましく、脂肪族または脂環式エポキシ樹脂は信頼性、特に接着性という観点から使用する量を制限するほうがさらに好ましい。これらは単独でも２種以上混合して使用してもよい。また本発明では液状封止樹脂組成物の態様のため、エポキシ樹脂（Ａ）として最終的に常温（２５℃）で液状であることが好ましいが、常温で固体のエポキシ樹脂であっても常温で液状のエポキシ樹脂に溶解させ、結果的に液状の状態であればよい。
本発明において、常温とは２５℃を指し、また、液状とは樹脂又は樹脂組成物が流動性を有していることを指す。
本発明において、上記液状樹脂組成物は、常温（２５℃）において流動性を有している。 Further, in the case of the present invention, those containing a structure in which a glycidyl structure or a glycidylamine structure is bonded to an aromatic ring are more preferable from the viewpoint of heat resistance, mechanical properties, and moisture resistance, and aliphatic or alicyclic epoxy resins are reliable, In particular, it is more preferable to limit the amount used from the viewpoint of adhesion. These may be used alone or in combination of two or more. In the present invention, the epoxy resin (A) is finally liquid at room temperature (25 ° C.) because of the liquid encapsulating resin composition. What is necessary is just to dissolve in a liquid epoxy resin and to be in a liquid state as a result.
In the present invention, normal temperature refers to 25 ° C., and liquid refers to that the resin or resin composition has fluidity.
In the present invention, the liquid resin composition has fluidity at room temperature (25 ° C.).

本発明の液状封止樹脂組成物は、アミン系硬化剤（Ｂ）を含む。そのようなものとしては、例えばジエチレントリアミン、トリエチレンテトラアミン、テトラエチレンペンタミン、ｍ−キシレンジアミン、トリメチルヘキサメチレンジアミン、２−メチルペンタメチレンジアミン脂肪族ポリアミン、イソフォロンジアミン、１，３−ビスアミノメチルシクロヘキサン、ビス（４−アミノシクロヘキシル）メタン、ノルボルネンジアミン、１，２−ジアミノシクロヘキサンなどの脂環式ポリアミン、Ｎ−アミノエチルピペラジン、１，４−ビス（２−アミノ−２−メチルプロピル）ピペラジンなどのピペラジン型のポリアミン、ジアミノジフェニルメタン、ｍ−フェニレンジアミン、ジアミノジフェニルスルホン、ジエチルトルエンジアミン、トリメチレンビス（４−アミノベンゾエート）、ポリテトラメチレンオキシド−ジ−Ｐ−アミノベンゾエートなどの芳香族ポリアミン類が挙げられる。これらは、単独で用いても２種以上の硬化剤を配合して用いてもよい。さらに半導体装置の封止用途を考慮すると、耐熱性、電気的特性、機械的特性、密着性、耐湿性の観点から芳香族ポリアミン型硬化剤が一層好ましい。性状としては、熱硬化性液状封止樹脂組成物の流動性を確保するため液状の硬化剤が好ましいが、結果的に常温で液状の状態であれば固形の硬化剤を溶解させて用いることもできる。
アミン系硬化剤以外の硬化剤として、フェノール類、酸無水物、ポリアミド樹脂、ポリスルフィド樹脂などを併用してもよい。 The liquid sealing resin composition of the present invention contains an amine-based curing agent (B). Such as, for example, diethylenetriamine, triethylenetetraamine, tetraethylenepentamine, m-xylenediamine, trimethylhexamethylenediamine, 2-methylpentamethylenediamine aliphatic polyamine, isophoronediamine, 1,3-bisamino Cycloaliphatic polyamines such as methylcyclohexane, bis (4-aminocyclohexyl) methane, norbornenediamine, 1,2-diaminocyclohexane, N-aminoethylpiperazine, 1,4-bis (2-amino-2-methylpropyl) piperazine Piperazine type polyamines such as diaminodiphenylmethane, m-phenylenediamine, diaminodiphenylsulfone, diethyltoluenediamine, trimethylenebis (4-aminobenzoate), polytetramethy N'okishido - aromatic polyamines such as di -P- amino benzoate. These may be used alone or in combination with two or more curing agents. In consideration of the sealing application of the semiconductor device, an aromatic polyamine type curing agent is more preferable from the viewpoints of heat resistance, electrical characteristics, mechanical characteristics, adhesion, and moisture resistance. As a property, a liquid curing agent is preferable in order to ensure the fluidity of the thermosetting liquid sealing resin composition, but as a result, if it is in a liquid state at room temperature, a solid curing agent may be dissolved and used. it can.
As curing agents other than amine curing agents, phenols, acid anhydrides, polyamide resins, polysulfide resins and the like may be used in combination.

本発明の液状封止樹脂組成物は、無機充填材（Ｃ）として平均径０．５μｍ以上１．０μｍ未満の球状アルミナ（１）と平均径１．０μｍ以上３．０μｍ未満の球状アルミナ（２）との混合物を含む。球状アルミナ（１）の平均径が０．５μｍ以上であるとバンプ接続部の隙間への流入性を向上させる効果が高くなり、１．０μｍ未満であると熱伝導率を向上させる効果が高くなる。球状アルミナ（２）の平均径が１．０μｍ以上であると、バンプ接続部の隙間への流入性を向上させる効果が高くなり、３．０μｍ未満であると熱伝導率を向上させる効果が高くなる。   The liquid sealing resin composition of the present invention comprises, as the inorganic filler (C), spherical alumina (1) having an average diameter of 0.5 μm or more and less than 1.0 μm and spherical alumina having an average diameter of 1.0 μm or more and less than 3.0 μm (2 ). When the average diameter of the spherical alumina (1) is 0.5 μm or more, the effect of improving the inflow property to the gap of the bump connection portion is enhanced, and when it is less than 1.0 μm, the effect of improving the thermal conductivity is enhanced. . When the average diameter of the spherical alumina (2) is 1.0 μm or more, the effect of improving the inflow property to the gap of the bump connection portion is enhanced, and when it is less than 3.0 μm, the effect of improving the thermal conductivity is enhanced. Become.

無機充填材（Ｃ）は、高熱伝導と高隙間流入性とを兼備しており半導体装置の信頼性を十分保持可能で、バンプ接続部への流入が可能であれば含有量に制限はないが、含有量８０質量％以上で、そのうち無機充填剤（Ｃ）に占める０．５μｍ以上１．０μｍ未満の球状アルミナ（１）の割合が５質量％以上５０質量％未満であることが好ましい。無機充填剤（Ｃ）の含有量が８０質量％以上であると熱伝導率上昇効果が高くなり、そのうちアルミナ（１）の割合が５質量％以上であるとバンプ接続部の隙間への流入性を向上させる効果が高くなり、５０質量％未満であると熱伝導率を向上させる効果が高くなる。
球状アルミナ以外の無機充填材も、本発明の効果である高熱伝導と低誘電率、高隙間流入性とが得られる範囲で加えることができ、そのようなものとしては球状シリカ、窒化ケイ素や窒化アルミニウム、酸化マグネシウムなどを適宜併用することができる。 The inorganic filler (C) has both high thermal conductivity and high gap inflow, and can sufficiently maintain the reliability of the semiconductor device, and the content is not limited as long as it can flow into the bump connection portion. The content of the spherical alumina (1) having a content of 80% by mass or more and of which the inorganic filler (C) is 0.5 μm or more and less than 1.0 μm is preferably 5% by mass or more and less than 50% by mass. When the content of the inorganic filler (C) is 80% by mass or more, the effect of increasing the thermal conductivity is increased, and when the proportion of alumina (1) is 5% by mass or more, the inflow property to the gaps in the bump connecting portion. The effect of improving the thermal conductivity is increased, and if it is less than 50% by mass, the effect of improving the thermal conductivity is increased.
Inorganic fillers other than spherical alumina can be added as long as the effects of the present invention are high thermal conductivity, low dielectric constant, and high gap inflow, such as spherical silica, silicon nitride and nitride. Aluminum, magnesium oxide, or the like can be used in combination as appropriate.

本発明の液状封止樹脂組成物は塩基性化合物（Ｄ）を含有する。塩基性化合物とは、液状封止樹脂組成物に加えることで封止樹脂系全体のｐＨ値を塩基性方向へ移行させるように働き、そのことによって球状アルミナの表面電位をマイナス方向へ変位させることで各々の封止樹脂系への分散性を改善し、粘度を低下できるので隙間流入性を向上させることができる。それと同時に、球状アルミナ粒子同士の静電気的相互作用を弱められるので、未充填ボイドや巻き込みボイド、揮発ボイドなど熱伝導を妨げる各種ボイドの発生を抑制できることから、高い熱伝導率を得ることができる。   The liquid sealing resin composition of the present invention contains a basic compound (D). By adding to the liquid sealing resin composition, the basic compound acts to shift the pH value of the entire sealing resin system in the basic direction, thereby displacing the surface potential of the spherical alumina in the negative direction. Therefore, the dispersibility in each sealing resin system can be improved and the viscosity can be lowered, so that the gap inflow property can be improved. At the same time, since electrostatic interaction between spherical alumina particles can be weakened, generation of various voids that hinder heat conduction such as unfilled voids, entrained voids, and volatile voids can be suppressed, so that high thermal conductivity can be obtained.

従って、塩基性化合物（Ｄ）として、封止樹脂物全体のｐＨ値を塩基性方向へ移行し得るものであれば特に制限はないが、そのようなものとしては、例えばヘキシルアミン、ヘプチルアミン、オクチルアミンなどの１級アミン類、ジプロピルアミン、ジブチルアミン、イソプロピルベンジルアミン、ジヘキシルアミン、ジオクチルアミン、ジシクロヘキシルアミン、ジフェニルアミン、ジベンジルアミン、ジデシルアミンなどの２級アミン類、イミノジエタノール、エチルアミノエタノール、イソプロピルアミノエタノール、ベンジルエタノールアミン、ジブチルアミノエタノール、アニリノエタノール、２−アミノ−２−エチル−１，３−プロパンジオール、イソプロパノールアミン、アミノメチルプロパノール、エタノールアミン、アミノプロパノール、ヘキサノールアミン、アミノエトキシエタノール、トリスヒドロキシメチルアミノメタンなどの１級，２級，３級アミノアルコール類、N-2-（アミノエチル）-3-アミノプロピルメチルジメトキシシラン、N-2-（アミノエチル）-3-アミノプロピルトリメトキシシラン、N-2-（アミノエチル）-3-アミノプロピルトリエトキシシラン、3-アミノプロピルトリエトキシシラン、3-トリエトキシシリル-Ｎ-（1,3-ジメチル-ブチリデン）プロピルアミンとその部分加水分解物、3-トリメトキシシリル-Ｎ-（1,3-ジメチル-ブチリデン）プロピルアミンとその部分加水分解物、N-フェニル-3-アミノプロピルトリメトキシシランなどの各種塩基性カップリング剤や、1,8-ジアザビシクロ[5.4.0]ウンデカ-7-エン（ＤＢＵ）あるいはその塩、1,5-ジアザビシクロ[4.3.0]ノナ-5-エン（ＤＢＮ）あるいはその塩などの塩基性物質などを挙げる事ができる。
なかでも、1,8-ジアザビシクロ[5.4.0]ウンデカ-7-エン（ＤＢＵ）あるいはその塩、1,5-ジアザビシクロ[4.3.0]ノナ-5-エン（ＤＢＮ）あるいはその塩が封止樹脂系のｐＨ値を塩基性に移行させる効果がより高く好ましい。 Accordingly, the basic compound (D) is not particularly limited as long as the pH value of the entire encapsulating resin product can be shifted in the basic direction. Examples of such a compound include hexylamine, heptylamine, Primary amines such as octylamine, secondary amines such as dipropylamine, dibutylamine, isopropylbenzylamine, dihexylamine, dioctylamine, dicyclohexylamine, diphenylamine, dibenzylamine, didecylamine, iminodiethanol, ethylaminoethanol, Isopropylaminoethanol, benzylethanolamine, dibutylaminoethanol, anilinoethanol, 2-amino-2-ethyl-1,3-propanediol, isopropanolamine, aminomethylpropanol, ethanolamine, amino Primary, secondary, tertiary amino alcohols such as propanol, hexanolamine, aminoethoxyethanol, trishydroxymethylaminomethane, N-2- (aminoethyl) -3-aminopropylmethyldimethoxysilane, N-2- ( Aminoethyl) -3-aminopropyltrimethoxysilane, N-2- (aminoethyl) -3-aminopropyltriethoxysilane, 3-aminopropyltriethoxysilane, 3-triethoxysilyl-N- (1,3- Dimethyl-butylidene) propylamine and its partial hydrolyzate, 3-trimethoxysilyl-N- (1,3-dimethyl-butylidene) propylamine and its partial hydrolyzate, N-phenyl-3-aminopropyltrimethoxysilane Various basic coupling agents such as 1,8-diazabicyclo [5.4.0] undec-7-ene (DBU) or a salt thereof, 1,5-diazabicyclo [4.3 .0] Nona-5-ene (DBN) or a basic substance such as a salt thereof.
Among them, 1,8-diazabicyclo [5.4.0] undec-7-ene (DBU) or a salt thereof, 1,5-diazabicyclo [4.3.0] nona-5-ene (DBN) or a salt thereof is a sealing resin. The effect of shifting the pH value of the system to basic is higher and preferable.

塩基性化合物（Ｄ）の配合量は、封止樹脂物全体のｐＨ値を塩基性方向へ移行し得るものであれば特に制限はないが、０．００５質量％以上１．０質量％以下であることが好ましい。   The compounding amount of the basic compound (D) is not particularly limited as long as the pH value of the entire sealing resin product can be shifted in the basic direction, but is 0.005% by mass to 1.0% by mass. Preferably there is.

特に封止樹脂系のｐＨ値は、７を超えることが好ましく、そのことによって球状アルミナの樹脂系への分散性がいっそう向上し、粘度が低下して隙間流入性が向上する。それと同時に球状アルミナ粒子同士の静電気的相互作用がいっそう弱まるので、未充填ボイドや巻き込みボイド、揮発ボイドなど熱伝導を妨げる各種ボイドの発生が抑制され、高い熱伝導率を得ることができる。さらに好ましくは、ｐＨ値８より大きいことが、アルミナの等電点を上回るので、前記効果がいっそう高くなる。
ここでｐＨ値とは、水素イオン指数または水素イオン濃度指数を指す。ｐＨ値の決定方法は特に限定されないが、例えばリトマス試験紙などのｐＨ試験紙、ｐＨ指示薬、ｐＨ電極やｐＨセンサーなどを用いた一般的なものを使用することができる。なお、ｐＨ値の決定に際しては、液状封止樹脂組成物のｐＨ値を変動させない範囲で前処理を施したり、添加剤を加えたり、加熱や冷却などの操作も加えることができる。
本願では、液状封止樹脂組成物０．０１〜０．１ｍｌを、ｐＨメーターのセンサー部に乗せ、その上から純水を０．０２〜０．２ｍｌ加えて検体とした。さらに、センサー部を傾けるなどして全体が検体で覆われるようにし、ｐＨ値が安定するまで静置し、表示されたｐＨ値を液状樹脂組成物のｐＨ値とした。 In particular, the pH value of the sealing resin system is preferably more than 7, whereby the dispersibility of the spherical alumina in the resin system is further improved, the viscosity is lowered, and the gap inflow property is improved. At the same time, electrostatic interaction between the spherical alumina particles is further weakened, so that generation of various voids that hinder heat conduction such as unfilled voids, entrained voids, and volatile voids is suppressed, and high thermal conductivity can be obtained. More preferably, since the pH value greater than 8 exceeds the isoelectric point of alumina, the effect is further enhanced.
Here, the pH value refers to a hydrogen ion index or a hydrogen ion concentration index. The method for determining the pH value is not particularly limited. For example, a general method using a pH test paper such as a litmus test paper, a pH indicator, a pH electrode, a pH sensor, or the like can be used. In determining the pH value, pretreatment can be performed, additives can be added, and operations such as heating and cooling can be added within a range that does not change the pH value of the liquid sealing resin composition.
In the present application, 0.01 to 0.1 ml of the liquid sealing resin composition was placed on the sensor part of the pH meter, and 0.02 to 0.2 ml of pure water was added thereon to prepare a specimen. Furthermore, the sensor part was tilted so that the whole was covered with the specimen and allowed to stand until the pH value was stabilized, and the displayed pH value was used as the pH value of the liquid resin composition.

本発明の液状封止樹脂組成物には、エポキシ樹脂（Ａ）、硬化剤（Ｂ）、無機充填材（Ｃ）として平均径０．５μｍ以上１．０μｍ未満の球状アルミナ（１）と平均径１．０μｍ以上３．０μｍ未満の球状アルミナ（２）との混合物、塩基性化合物（Ｄ）を含有する以外に、必要に応じて密着助剤、分散剤、ブリード防止剤、着色剤、消泡剤、希釈剤、顔料、難燃剤、レベリング剤などの各種添加剤を用いることができる。ただし、それらの添加物によって塩基性化合物の働きが抑えられる場合は、適宜塩基性化合物（Ｄ）の配合量を増やすことで本発明の効果を維持できる。   In the liquid sealing resin composition of the present invention, the epoxy resin (A), the curing agent (B), and the inorganic filler (C) have a spherical alumina (1) having an average diameter of 0.5 μm or more and less than 1.0 μm and an average diameter. In addition to containing a mixture with spherical alumina (2) of 1.0 μm or more and less than 3.0 μm, basic compound (D), adhesion aid, dispersant, anti-bleeding agent, colorant, antifoaming as necessary Various additives such as an agent, a diluent, a pigment, a flame retardant, and a leveling agent can be used. However, when the action of the basic compound is suppressed by these additives, the effect of the present invention can be maintained by appropriately increasing the blending amount of the basic compound (D).

本発明の液状封止樹脂組成物は、上述した各成分、添加剤などをプラネタリーミキサー、三本ロール、二本熱ロール、ライカイ機などの装置を用いて分散混練したのち、真空下で脱泡処理して製造するなど、一般的に知られている製造方法を用いることができる。さらに、液状封止樹脂組成物の製造に際しては、必要に応じて原料投入工程、分散混練工程などにおいて、原料投入の順序や投入時間を調整することや、何度かに分けて原料投入や分散混練を行うこと、加温すること、熟成工程を付加することなども可能である。   The liquid sealing resin composition of the present invention is prepared by dispersing and kneading the above-described components and additives using an apparatus such as a planetary mixer, three rolls, two hot rolls, and a raikai machine, and then removed under vacuum. A generally known production method such as foam production can be used. Furthermore, in the production of the liquid sealing resin composition, the raw material charging process and the dispersion kneading process, if necessary, can adjust the raw material charging sequence and the charging time, or can divide the raw material and distribute it several times. It is also possible to perform kneading, heating, adding an aging step, and the like.

このような液状封止樹脂組成物は、半導体装置の製造プロセスにおける時間の短縮や半導体デバイスへの熱応力低減の観点から、１５０℃以下２時間以下の硬化条件でエポキシ樹脂の反応率が９５％以上であることが好ましい。その理由としては、反応率が９５％以上になると、高温保管などによる後硬化により、ガラス転移温度（Ｔｇ）や破壊靱性値などの物性が変化することが少なく、反りや剥離など半導体装置へ悪影響が低減されるからである。ここで硬化とは、エポキシ樹脂の熱硬化反応によって３次元網状構造を形成することを指し、その反応率（Ｙ）はＤＳＣ（示差走査熱量測定）により測定し、未硬化のサンプルの発熱量Ａ（ｍＪ／ｍｇ）と硬化後のサンプルの発熱量Ｂ（ｍＪ／ｍｇ）を測定し、Ｙ（％）＝（１−Ｂ／Ａ）×１００の計算式を用いて算出する。ＤＳＣによる発熱量測定はアルミパンにサンプルを２０ｍｇ秤量し蓋をした後、Ｓｅｉｋｏ Ｉｎｓｔｒｕｍｅｎｔｓ社製ＤＳＣ２２０を用い３０−３００℃の温度範囲を１０℃／ｍｉｎの昇温条件で測定し、横軸に温度（℃）縦軸にＤＳＣ（ｍＪ／ｍｇ）をとったグラフにおけるベースラインを底辺とした反応ピークの面積として求めることができる。   Such a liquid encapsulating resin composition has an epoxy resin reaction rate of 95% under curing conditions of 150 ° C. or less and 2 hours or less from the viewpoint of shortening the time in the manufacturing process of the semiconductor device and reducing thermal stress on the semiconductor device. The above is preferable. The reason for this is that when the reaction rate is 95% or more, physical properties such as glass transition temperature (Tg) and fracture toughness value are less likely to change due to post-curing due to high temperature storage, etc., and adversely affect semiconductor devices such as warping and peeling. It is because is reduced. Here, curing refers to forming a three-dimensional network structure by thermosetting reaction of an epoxy resin, the reaction rate (Y) is measured by DSC (differential scanning calorimetry), and the calorific value A of an uncured sample. (MJ / mg) and the calorific value B (mJ / mg) of the cured sample are measured and calculated using the formula Y (%) = (1−B / A) × 100. The calorific value is measured by DSC after weighing 20 mg of a sample on an aluminum pan, capping, and using a DSC220 manufactured by Seiko Instruments Co., Ltd., measuring a temperature range of 30-300 ° C. under a temperature rising condition of 10 ° C./min. (° C.) It can be determined as the area of the reaction peak with the base line in the graph with DSC (mJ / mg) on the vertical axis.

次に、半導体装置について説明する。
本発明の半導体装置は、上述した液状封止樹脂組成物を用いて製造される。
例えばフリップチップ接続のアンダーフィル材に適用した場合について説明すると、まず半田バンプを有する半導体素子と基板とを、リフロー装置を通して半田接続を行う。次に、半導体素子と基板との間隙に液状封止樹脂組成物を充填する。充填する方法としては、毛細管現象を利用する方法が一般的である。具体的には、半導体素子の一辺に上記液状封止樹脂組成物を塗布した後、半導体素子と基板との間隙に毛細管現象で流し込む方法、半導体素子の２辺に上記液状封止樹脂組成物を塗布した後、半導体素子と基板との間隙に毛細管現象で流し込む方法、半導体素子の中央部にスルーホールを開けておき、半導体素子の周囲に上記液状封止樹脂組成物を塗布した後、半導体素子と基板との間隙に毛細管現象で流し込む方法などが挙げられる。また、一度に全量を塗布するのではなく、２度に分けて塗布する方法なども行われる。次に、充填した上記液状封止樹脂組成物を硬化させる。硬化条件は、特に限定されないが、例えば１００℃〜１７０℃の温度範囲で１〜１２時間加熱を行うことにより硬化できる。さらに、例えば１００℃で１時間加熱した後、引き続き１５０℃で２時間加熱するような、段階的に温度を変化させながら加熱硬化を行っても良い。このようにして、半導体素子と基板との間が、液状封止樹脂組成物の硬化物で封止されている半導体装置を得ることができる。 Next, a semiconductor device will be described.
The semiconductor device of the present invention is manufactured using the liquid sealing resin composition described above.
For example, when applied to a flip-chip underfill material, a semiconductor element having a solder bump and a substrate are first solder-connected through a reflow apparatus. Next, the liquid sealing resin composition is filled in the gap between the semiconductor element and the substrate. As a filling method, a method utilizing a capillary phenomenon is common. Specifically, the liquid sealing resin composition is applied to one side of the semiconductor element and then poured into the gap between the semiconductor element and the substrate by a capillary phenomenon, and the liquid sealing resin composition is applied to the two sides of the semiconductor element. After coating, a method of pouring into the gap between the semiconductor element and the substrate by capillary action, a through hole is opened in the central part of the semiconductor element, the liquid sealing resin composition is applied around the semiconductor element, and then the semiconductor element And a method of pouring into the gap between the substrate and the substrate by capillary action. Further, instead of applying the whole amount at once, a method of applying in two steps is also performed. Next, the filled liquid sealing resin composition is cured. Although hardening conditions are not specifically limited, For example, it can harden | cure by heating for 1 to 12 hours in the temperature range of 100 to 170 degreeC. Furthermore, for example, after heating at 100 ° C. for 1 hour, heat curing may be performed while changing the temperature stepwise, such as heating at 150 ° C. for 2 hours. In this manner, a semiconductor device in which the space between the semiconductor element and the substrate is sealed with the cured product of the liquid sealing resin composition can be obtained.

このような半導体装置には、フリップチップ方式の半導体装置、キャビティーダウン型ＢＧＡ（Ｂａｌｌ Ｇｒｉｄ Ａｒｒａｙ）、ＰＯＰ（Ｐａｃｋａｇｅ ｏｎ Ｐａｃｋａｇｅ）型ＢＧＡ（Ｂａｌｌ Ｇｒｉｄ Ａｒｒａｙ）、ＴＡＢ（Ｔａｐｅ Ａｕｔｏｍａｔｅｄ Ｂｏｎｄｉｎｇ）型ＢＧＡ（Ｂａｌｌ Ｇｒｉｄ Ａｒｒａｙ）、ＣＳＰ（Ｃｈｉｐ Ｓｃａｌｅ Ｐａｃｋａｇｅ）等が挙げられる。   Such a semiconductor device includes a flip-chip type semiconductor device, a cavity down type BGA (Ball Grid Array), a POP (Package on Package) type BGA (Ball Grid Array), and a TAB (Tape Automated Bonding) type BGA (Ball). Grid Array) and CSP (Chip Scale Package).

以下、本発明を実施例および比較例に基づいて詳細に説明するが、本発明はこれに限定されるものではない。
（実施例１〜７）（比較例１〜５）
下記に示すエポキシ樹脂（Ａ）と硬化剤（Ｂ）、無機充填剤（Ｃ）として球状アルミナと球状シリカとの混合物、塩基性化合物（Ｄ）、その他に希釈溶剤、密着助剤を表１に示した組成で配合、それを３本ロールにて十分に混練分散した後、真空脱泡して液状封止樹脂組成物を得た。なお、塩基性化合物と希釈溶剤とは予め室温混合したものを用いた。 EXAMPLES Hereinafter, although this invention is demonstrated in detail based on an Example and a comparative example, this invention is not limited to this.
(Examples 1-7) (Comparative Examples 1-5)
Table 1 shows the epoxy resin (A) and curing agent (B) shown below, a mixture of spherical alumina and spherical silica as the inorganic filler (C), basic compound (D), diluting solvent, and adhesion aid. After blending with the indicated composition and kneading and dispersing it sufficiently with three rolls, vacuum degassing was performed to obtain a liquid sealing resin composition. In addition, the basic compound and the diluting solvent were previously mixed at room temperature.

○エポキシ樹脂（Ａ）
大日本インキ化学工業（株）製 （ＥＸＡ−８３０ＬＶＰ）
ジャパンエポキシレジン（株）製（ＪＥＲ−６３０）
○硬化剤（Ｂ）
日本化薬（株）製 （カヤハードＡＡ）
○無機充填材（Ｃ）
・球状アルミナ（１）
電気化学工業（株）製 （ＡＳＦＰ−２０：平均径０．２μｍ）
アドマテクス（株）製 （ＡＯ−５０２：平均径０．７μｍ）
・球状アルミナ（２）
昭和電工（株）製 （ＣＢ−Ｐ０２：平均径２．０μｍ）
昭和電工（株）製 （ＣＢ−Ａ０５Ｓ：平均径３．０μｍ）
昭和電工（株）製 （ＣＢ−Ｐ０５：平均径４．０μｍ）
○塩基性化合物（Ｄ）
１，８−ジアザビシクロ（５，４，０）ウンデセン−７（ＤＢＵ）
ＤＢＵ−フェノール塩 サンアプロ(株)製Ｕ−ＣＡＴ （ＳＡ−１）
１，５−ジアザビシクロ（４，３，０）ノネン−５ （ＤＢＮ）
○希釈溶剤
ブチルセロソルブアセテート（ＢＣＳＡ）
○密着助剤
信越化学（株）製 （ＫＢＭ−４０３） ○ Epoxy resin (A)
Dainippon Ink & Chemicals, Inc. (EXA-830LVP)
Made by Japan Epoxy Resin Co., Ltd. (JER-630)
○ Hardener (B)
Nippon Kayaku Co., Ltd. (Kayahard AA)
○ Inorganic filler (C)
・ Spherical alumina (1)
Manufactured by Denki Kagaku Kogyo Co., Ltd. (ASFP-20: average diameter 0.2 μm)
Admatechs Co., Ltd. (AO-502: average diameter 0.7μm)
・ Spherical alumina (2)
Showa Denko Co., Ltd. (CB-P02: average diameter 2.0 μm)
Showa Denko Co., Ltd. (CB-A05S: average diameter 3.0 μm)
Showa Denko Co., Ltd. (CB-P05: average diameter 4.0 μm)
○ Basic compounds (D)
1,8-diazabicyclo (5,4,0) undecene-7 (DBU)
DBU-phenol salt U-CAT (SA-1) manufactured by San Apro Co., Ltd.
1,5-diazabicyclo (4,3,0) nonene-5 (DBN)
○ Diluted solvent butyl cellosolve acetate (BCSA)
○ Adhesion aid Shin-Etsu Chemical Co., Ltd. (KBM-403)

（測定及び評価）
得られた液状封止樹脂組成物および半導体装置について、以下の測定及び評価を行った。得られた結果を表１に示す。 (Measurement and evaluation)
About the obtained liquid sealing resin composition and semiconductor device, the following measurement and evaluation were performed. The obtained results are shown in Table 1.

１．ｐＨの測定
各液状封止樹脂組成物０．０５ｍｌを、予め校正液を用いて校正されたＨＯＲＩＢＡ製コンパクトｐＨメーター「Ｂ−２１１」のセンサー部に乗せ、その上から純水約０．１ｍｌ加えて検体とした。さらに、センサー部を傾けるなどして全体が検体で覆われるようにし、センサー部の蓋を閉めてｐＨ値が安定したとの表示が出るまで静置した。表示されたｐＨ値を液状樹脂組成物のｐＨ値とした。 1. Measurement of pH 0.05 ml of each liquid encapsulating resin composition was placed on the sensor part of a compact pH meter “B-211” manufactured by HORIBA that was calibrated in advance using a calibration solution, and about 0.1 ml of pure water was added from above. Were used as specimens. Further, the entire sensor part was covered with a sample by tilting the sensor part, and the lid of the sensor part was closed and left to stand until an indication that the pH value was stable was obtained. The displayed pH value was defined as the pH value of the liquid resin composition.

２．熱伝導率の測定と評価
各液状封止樹脂組成物について、１５０℃雰囲気下で２時間加熱して得られる硬化物の熱拡散率α、密度ρおよび比熱Ｃｐを下記方法によってそれぞれ測定して求め、式（１）により熱伝導率λを算出した。
熱拡散率αは、熱拡散率測定装置ＬＦＡ４４７ Ｎａｎｏｆｌａｓｈ（ＮＥＴＺＳＣＨ社製）を用い、ＪＩＳ Ｒ １６１１：２０１１（最小二乗法）に準拠したレーザーフラッシュ法によって測定、密度ρはＪＩＳ Ｋ ７１１２Ａ法に準拠した水中置換法によって測定、また比熱Ｃｐについては示差走査熱量計 ＤＳＣ７（ＰＥＲＫＩＮ−ＥＬＭＥＲ社製）を用い、ＪＩＳ Ｋ ７１２３に準拠した方法によって測定した。
熱伝導率の評価については、熱伝導率値が１．５Ｗ／ｍ・Ｋ以上のものは良好、１．５Ｗ／ｍ・Ｋ未満のものは不可と判定した。
λ＝α×ρ×Ｃｐ ・・・・・・・・・・・式（１）
λ：熱伝導率（Ｗ／ｍ・Ｋ）
α：熱拡散率（ｍ２／ｓｅｃ）
ρ：密度（ｋｇ／ｍ３）
Ｃｐ：比熱（Ｊ／ｋｇ・Ｋ） 2. Measurement and Evaluation of Thermal Conductivity For each liquid sealing resin composition, the thermal diffusivity α, density ρ, and specific heat Cp of a cured product obtained by heating for 2 hours in an atmosphere at 150 ° C. are determined by the following methods. The thermal conductivity λ was calculated from the equation (1).
The thermal diffusivity α is measured by a laser flash method in accordance with JIS R 1611: 2011 (least square method) using a thermal diffusivity measuring device LFA447 Nanoflash (manufactured by NETZSCH), and the density ρ is in accordance with the JIS K 7112A method. It measured by the underwater substitution method, and the specific heat Cp was measured by a method based on JIS K 7123 using a differential scanning calorimeter DSC7 (manufactured by PERKIN-ELMER).
Regarding the evaluation of thermal conductivity, those having a thermal conductivity value of 1.5 W / m · K or higher were judged to be good, and those having a thermal conductivity of less than 1.5 W / m · K were judged to be impossible.
λ = α × ρ × Cp Equation (1)
λ: Thermal conductivity (W / m · K)
α: Thermal diffusivity (m 2 / sec)
ρ: Density (kg / m 3 )
Cp: Specific heat (J / kg · K)

３．隙間流入速度の測定と評価
１８ｍｍ×１８ｍｍのガラス板(上)とガラス板(下)とを７０±１０μｍの間隔が空くように張り合わせて、隙間のある平行平面を持つガラスセルを作製した。このガラスセルをホットプレートの上に置き、ガラス板(上)の上面温度が１１０±１℃になるよう温度調整しながら５分間静置した。その後、ガラスセルの一辺に、室温で２４時間静置した液状封止樹脂組成物０．０５〜０．１ｍＬを毛細管現象を利用して塗布し、１８ｍｍ流れきる時間（秒）を測定した。隙間流入時間が４００秒未満のものを良好、４００秒以上のものを不可と判定した。 3. Measurement and Evaluation of Gap Inflow Speed A glass cell having a parallel plane with a gap was prepared by bonding an 18 mm × 18 mm glass plate (upper) and a glass plate (lower) so that a space of 70 ± 10 μm was left therebetween. The glass cell was placed on a hot plate and allowed to stand for 5 minutes while adjusting the temperature so that the upper surface temperature of the glass plate (upper) was 110 ± 1 ° C. Thereafter, 0.05 to 0.1 mL of a liquid sealing resin composition that was allowed to stand at room temperature for 24 hours was applied to one side of the glass cell using a capillary phenomenon, and the time (seconds) required to flow 18 mm was measured. It was determined that a gap inflow time of less than 400 seconds was good, and a gap inflow time of 400 seconds or more was not acceptable.

４．隙間流入性の評価
バンプサイズ１００μｍ、バンプ数３８７２個の半田バンプが設けられた１５ｍｍ角の半導体素子と、ＢＴ基板（ビスマレイミドトリアジン基板、接続パッド：金メッキ表面）とを、ロジン系フラックス剤（タルチンケスター社製 Ｋｅｓｔｅｒ６５０２）を使用し、２６０℃で加熱して半田を溶融接合して得られた、半導体素子とＢＴ基板との隙間が８０μｍの半導体装置を、１１０℃に加熱した熱板上に乗せ、半導体素子とＢＴ基板との隙間に前記の液状封止樹脂組成物を半導体素子の一辺から毛細管現象を利用して充填した後、１５０℃で２時間硬化封止して半導体装置を得た。得られた半導体装置を、超音波深傷装置を用いて検査し、未充填部の無かったものを良好、未充填部のあったものを不可と判定した。 4). Evaluation of gap inflow property A 15 mm square semiconductor element provided with solder bumps having a bump size of 100 μm and a number of bumps of 3872, and a BT substrate (bismaleimide triazine substrate, connection pad: gold-plated surface) are combined with a rosin flux agent (tal Using a Kester 6502 manufactured by Chinster Co., Ltd., a semiconductor device having a gap between the semiconductor element and the BT substrate of 80 μm obtained by heating and melting at 260 ° C. on a hot plate heated to 110 ° C. The liquid sealing resin composition was filled into the gap between the semiconductor element and the BT substrate from one side of the semiconductor element using a capillary phenomenon, and then cured and sealed at 150 ° C. for 2 hours to obtain a semiconductor device. . The obtained semiconductor device was inspected using an ultrasonic deep wound device, and it was determined that there was no unfilled portion, and that there was an unfilled portion was unacceptable.

Figure 2012224799
Figure 2012224799

本発明は、高熱伝導率と低誘電率、高隙間流入性とを兼備した液状封止樹脂組成物、およびそれを用いた半導体装置を得ることに利用することができる。 INDUSTRIAL APPLICABILITY The present invention can be used to obtain a liquid sealing resin composition having both high thermal conductivity, low dielectric constant, and high gap inflow property, and a semiconductor device using the same.

Claims (6)

半導体装置の組立に用いる液状封止樹脂組成物であって、（Ａ）液状エポキシ樹脂、（Ｂ）アミン系硬化剤、（Ｃ）無機充填材を含有し、（Ｃ）無機充填材が平均径０．５μｍ以上１．０μｍ未満の球状アルミナ（１）と平均径１．０μｍ以上３．０μｍ未満の球状アルミナ（２）との混合物を含有し、且つ（Ｄ）塩基性化合物を含有することを特徴とする液状封止樹脂組成物。   A liquid encapsulating resin composition used for assembling a semiconductor device, comprising (A) a liquid epoxy resin, (B) an amine-based curing agent, (C) an inorganic filler, and (C) an inorganic filler having an average diameter Containing a mixture of spherical alumina (1) 0.5 μm or more and less than 1.0 μm and spherical alumina (2) having an average diameter of 1.0 μm or more and less than 3.0 μm, and (D) containing a basic compound. A liquid encapsulating resin composition. ｐＨ値が７を超えるものである請求項１記載の液状封止樹脂組成物。   The liquid sealing resin composition according to claim 1, which has a pH value exceeding 7. （Ｄ）塩基性化合物が、１，８−ジアザビシクロ（５．４．０）ウンデセン−７、１，５−ジアザビシクロ（４．３．０）ノネン−５、およびそれらの塩のうち少なくとも１種類である請求項1又は２記載の液状封止樹脂組成物。 (D) the basic compound is at least one of 1,8-diazabicyclo (5.4.0) undecene-7, 1,5-diazabicyclo (4.3.0) nonene-5, and salts thereof; The liquid sealing resin composition according to claim 1 or 2. （Ｃ）無機充填材の含有量が８０質量％以上であって、そのうち（Ｃ）無機充填剤に占める０．５μｍ以上１．０μｍ未満の球状アルミナ（１）の割合が５質量％以上５０質量％未満である請求項１〜３いずれか一項に記載の液状封止樹脂組成物。 (C) The content of the inorganic filler is 80% by mass or more, of which the proportion of spherical alumina (1) of 0.5 μm or more and less than 1.0 μm in the (C) inorganic filler is 5% by mass or more and 50% by mass. The liquid sealing resin composition according to claim 1, wherein the liquid sealing resin composition is less than%. 請求項１〜４いずれか一項に記載の液状封止樹脂組成物の硬化物で封止されていることを特徴とする半導体装置。   It is sealed with the hardened | cured material of the liquid sealing resin composition as described in any one of Claims 1-4, The semiconductor device characterized by the above-mentioned. 請求項１〜４いずれか一項に記載の液状封止樹脂組成物を充填する充填工程を有することを特徴とする半導体装置の製造方法。 A method for manufacturing a semiconductor device, comprising a filling step of filling the liquid sealing resin composition according to claim 1.
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