JP2008088378A - Liquid epoxy resin composition for semiconductor encapsulation, its manufacturing method and semiconductor device - Google Patents
Liquid epoxy resin composition for semiconductor encapsulation, its manufacturing method and semiconductor device Download PDFInfo
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本発明は、半導体装置のポッティングやコーティング材に適しており、特にフリップチップ用アンダーフィル材等として速硬化性に優れており、隙間侵入性に優れた半導体封止用液状エポキシ樹脂組成物、その製造方法、及びこの組成物の硬化物をアンダーフィル材として封止した半導体装置に関するものである。 The present invention is suitable for potting and coating materials for semiconductor devices, and in particular, it is excellent in fast curability as an underfill material for flip chip and the like, and is a liquid epoxy resin composition for semiconductor sealing excellent in gap penetration properties, and its The present invention relates to a manufacturing method and a semiconductor device in which a cured product of this composition is sealed as an underfill material.
電気機器の小型化、軽量化、高性能化にともない、半導体の実装方法もピン挿入タイプから表面実装、そしてベアチップ実装が主流になってきている。ベアチップ実装の一つにフリップチップ（ＦＣ）実装がある。ＦＣ実装とは、ＬＳＩチップの配線パターン面に高さ１０μｍから１００μｍ程度のバンプといわれる電極を数個から数千個形成し、基板の電極を導電ペーストあるいは半田等で接合する方式である。従来の粉末状イミダゾール系硬化促進剤を用いたフリップチップ用アンダーフィル材は、その硬化促進剤が粉末であることから、潜在性を呈している利点により使用されてきたが、粉末であるがゆえに充填材としての機能も付与せざるを得ない。そのため、触媒量とはいえ、その粒径によってはアンダーフィル特有の毛細管現象を阻害する要因にもなり兼ねない。実際、細かすぎるとチキソ性を発現するため、侵入性が悪くなる。
以上の理由より、品質管理の点から、安定的に良好な侵入性を呈する液状エポキシ樹脂組成物が望まれていた。
Along with the miniaturization, weight reduction, and performance enhancement of electrical equipment, semiconductor mounting methods are becoming mainstream from pin insertion type to surface mounting and bare chip mounting. One type of bare chip mounting is flip chip (FC) mounting. The FC mounting is a system in which several to several thousand electrodes called bumps having a height of about 10 μm to 100 μm are formed on the wiring pattern surface of an LSI chip, and the electrodes on the substrate are joined with a conductive paste or solder. Conventional flip-chip underfill materials using powdery imidazole-based curing accelerators have been used because of their potential advantages because the curing accelerators are powders. A function as a filler must also be imparted. Therefore, although it is the amount of catalyst, depending on the particle size, it may be a factor that inhibits capillary phenomenon peculiar to underfill. In fact, if it is too fine, thixotropy will be manifested, resulting in poor penetration.
For these reasons, a liquid epoxy resin composition that stably exhibits good penetration properties has been desired from the viewpoint of quality control.
なお、本発明に関連する公知文献としては、下記のものがある。
本発明は、上記事情に鑑みなされたもので、アンダーフィルする際、安定的に良好な隙間侵入性を付与する半導体封止用液状エポキシ樹脂組成物、その製造方法、及びこの組成物の硬化物をアンダーフィル材として封止した半導体装置を提供することを目的とする。 The present invention has been made in view of the above circumstances, and when underfilling, a liquid epoxy resin composition for semiconductor encapsulation that stably imparts good gap penetration properties, a method for producing the same, and a cured product of the composition An object of the present invention is to provide a semiconductor device sealed with an underfill material.
本発明者は、上記目的を達成するため鋭意検討を重ねた結果、（ａ）液状エポキシ樹脂，（ｂ）無機質充填剤，（ｃ）２−フェニル−４，５−ジヒドロキシメチルイミダゾール硬化促進剤を必須成分とし、（ｃ）成分の２−フェニル−４，５−ジヒドロキシメチルイミダゾール硬化促進剤として、常温において固体で、不溶解性であり、その平均粒径が３〜５μｍであるものを用い、更に、上記成分を混合・混練して得られた組成物を２０〜３０℃で７２〜３３６時間熟成することにより、安定的に良好な隙間侵入性を呈する液状エポキシ樹脂組成物が得られることを知見した。
更に、この液状エポキシ樹脂組成物をアンダーフィル材として適用した場合、その生産管理上、安定性において優れたものであることを見出し、本発明をなすに至ったものである。
As a result of intensive studies to achieve the above object, the present inventor has obtained (a) a liquid epoxy resin, (b) an inorganic filler, and (c) 2-phenyl-4,5-dihydroxymethylimidazole curing accelerator. As an essential component, (c) component 2-phenyl-4,5-dihydroxymethylimidazole curing accelerator that is solid at room temperature, is insoluble, and has an average particle size of 3 to 5 μm, Furthermore, by aging the composition obtained by mixing and kneading the above components at 20 to 30 ° C. for 72 to 336 hours, it is possible to obtain a liquid epoxy resin composition that stably exhibits good gap penetration properties. I found out.
Furthermore, when this liquid epoxy resin composition is applied as an underfill material, it has been found that it is excellent in stability in terms of production management, and has led to the present invention.
従って、本発明は、下記に示す半導体封止用液状エポキシ樹脂組成物、その製造方法及び半導体装置を提供する。
〔１〕 （ａ）液状エポキシ樹脂，
（ｂ）無機質充填剤，
（ｃ）２−フェニル−４，５−ジヒドロキシメチルイミダゾール（２ＰＨＺ）硬化促進剤
を必須成分とする半導体封止用液状エポキシ樹脂組成物であって、（ｃ）成分である硬化促進剤の平均粒径が３〜５μｍであり、上記（ａ）〜（ｃ）成分を含む混合・混練物が２０〜３０℃で７２〜３３６時間熟成されてなることを特徴とする半導体封止用液状エポキシ樹脂組成物。
〔２〕 （ａ）液状エポキシ樹脂，
（ｂ）無機質充填剤，
（ｃ）２−フェニル−４，５−ジヒドロキシメチルイミダゾール（２ＰＨＺ）硬化促進剤
を必須成分とする半導体封止用液状エポキシ樹脂組成物の製造方法であって、（ｃ）成分である硬化促進剤の平均粒径が３〜５μｍであり、上記（ａ）〜（ｃ）を含む混合物を混練した後、２０〜３０℃で７２〜３３６時間熟成することを特徴とする半導体封止用液状エポキシ樹脂組成物の製造方法。
〔３〕 〔１〕に記載の液状エポキシ樹脂組成物の硬化物をアンダーフィル材として封止した半導体装置。
Therefore, this invention provides the liquid epoxy resin composition for semiconductor sealing shown below, its manufacturing method, and a semiconductor device.
[1] (a) Liquid epoxy resin,
(B) inorganic filler,
(C) A liquid epoxy resin composition for semiconductor encapsulation containing 2-phenyl-4,5-dihydroxymethylimidazole (2PHZ) curing accelerator as an essential component, and (c) average particle of curing accelerator as component Liquid epoxy resin composition for semiconductor encapsulation, characterized in that the mixed and kneaded material containing 3 to 5 μm in diameter is aged for 72 to 336 hours at 20 to 30 ° C., containing the above components (a) to (c) object.
[2] (a) Liquid epoxy resin,
(B) inorganic filler,
(C) A method for producing a liquid epoxy resin composition for semiconductor encapsulation having 2-phenyl-4,5-dihydroxymethylimidazole (2PHZ) curing accelerator as an essential component, wherein (c) the curing accelerator is a component The liquid epoxy resin for semiconductor encapsulation is characterized in that it has an average particle diameter of 3 to 5 μm and is aged at 20 to 30 ° C. for 72 to 336 hours after kneading the mixture containing the above (a) to (c) A method for producing the composition.
[3] A semiconductor device in which a cured product of the liquid epoxy resin composition according to [1] is sealed as an underfill material.
本発明の液状エポキシ樹脂組成物は、安定的に良好な隙間侵入性を呈し、速硬化性に優れるものであり、この組成物の硬化物をアンダーフィル材として封止した半導体装置は、生産管理上、安定性において優れたものである。 The liquid epoxy resin composition of the present invention stably exhibits good gap penetration and is excellent in rapid curability. A semiconductor device in which a cured product of this composition is sealed as an underfill material is produced and controlled. Moreover, it is excellent in stability.
本発明に用いられる液状のエポキシ樹脂（ａ）は、１分子中に２個以上のエポキシ基があればいかなるものでも使用可能であるが、特にビスフェノールＡ型エポキシ樹脂、ビスフェノールＦ型エポキシ樹脂、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、ナフタレン型エポキシ樹脂、ビフェニル型エポキシ樹脂、シクロペンタジエン型エポキシ樹脂などが例示される。この中でも室温で液状のエポキシ樹脂が望ましい。 As the liquid epoxy resin (a) used in the present invention, any liquid epoxy resin having two or more epoxy groups in one molecule can be used. In particular, bisphenol A type epoxy resin, bisphenol F type epoxy resin, phenol Examples include novolac type epoxy resins, cresol novolac type epoxy resins, naphthalene type epoxy resins, biphenyl type epoxy resins, cyclopentadiene type epoxy resins and the like. Among these, a liquid epoxy resin at room temperature is desirable.
また、下記構造のエポキシ樹脂も使用することができる。
本発明に用いるエポキシ樹脂の全塩素含有量は、１，５００ｐｐｍ以下、望ましくは１，０００ｐｐｍ以下であることが好ましい。また、１００℃で５０％エポキシ樹脂濃度における２０時間での抽出水塩素が１０ｐｐｍ以下であることが好ましい。全塩素含有量が１，５００ｐｐｍを超え、あるいは抽出水塩素が１０ｐｐｍを超える場合は、半導体素子の信頼性、特に耐湿性に悪影響を与えるおそれがある。 The total chlorine content of the epoxy resin used in the present invention is preferably 1,500 ppm or less, more preferably 1,000 ppm or less. Moreover, it is preferable that the extraction water chlorine in 20 hours in the 50% epoxy resin density | concentration at 100 degreeC is 10 ppm or less. When the total chlorine content exceeds 1,500 ppm or the extracted water chlorine exceeds 10 ppm, the reliability of the semiconductor element, particularly the moisture resistance, may be adversely affected.
本発明には、膨張係数を小さくする目的から、従来より知られている各種の無機質充填剤（ｂ）を添加する。無機質充填剤としては、溶融シリカ、結晶シリカ、アルミナ、ボロンナイトライド、アルミニウムナイトライド、シリコンナイトライド、マグネシア、マグネシウムシリケートなどが好適に使用される。 For the purpose of reducing the expansion coefficient, various conventionally known inorganic fillers (b) are added to the present invention. As the inorganic filler, fused silica, crystalline silica, alumina, boron nitride, aluminum nitride, silicon nitride, magnesia, magnesium silicate and the like are preferably used.
本発明においては、侵入性の向上と低線膨張化の両立を図るため、半導体装置のフリップチップギャップ幅（基板と半導体チップとの隙間）に対して平均粒径約１／５以下、特に１／２０以下、最大粒径が２／３以下、特に１／２以下である無機質充填剤を使用することが好ましい。平均粒径がフリップチップギャップ幅の１／５より大きい、また最大粒径がフリップチップギャップ幅の２／３より大きいと、侵入性の低下を引き起こし、ボイドが発生するおそれがある。 In the present invention, in order to achieve both improved penetration and low linear expansion, the average particle size is about 1/5 or less, particularly 1 with respect to the flip chip gap width (gap between the substrate and the semiconductor chip) of the semiconductor device. / 20 or less, and it is preferable to use an inorganic filler having a maximum particle size of 2/3 or less, particularly 1/2 or less. If the average particle size is larger than 1/5 of the flip chip gap width and the maximum particle size is larger than 2/3 of the flip chip gap width, the penetration may be reduced and voids may be generated.
ここで、本発明において、平均粒径は、例えばレーザー光回折法等による重量平均値（又はメディアン径）等として求めることができ、最大粒径も同様にレーザー光回折法等により求めることができる。また、リード間隔サイズの２／３を超える粒径のものがないことを確認する方法としては、例えば、無機質充填剤と純水を１：９の割合で混合し、超音波処理により凝集物を十分に崩し、これをリード間隔サイズの２／３の目開きフィルターで篩い、無機質充填剤がフィルター上に残らないことを確認する方法が採用される（以下同様）。 Here, in the present invention, the average particle diameter can be determined as, for example, a weight average value (or median diameter) by a laser light diffraction method or the like, and the maximum particle diameter can be similarly determined by a laser light diffraction method or the like. . Further, as a method for confirming that there is no particle having a particle size exceeding 2/3 of the lead interval size, for example, an inorganic filler and pure water are mixed at a ratio of 1: 9, and the aggregate is formed by ultrasonic treatment. A method is adopted in which the material is sufficiently broken and sieved with a 2/3 aperture filter of the lead interval size to confirm that the inorganic filler does not remain on the filter (the same applies hereinafter).
無機質充填剤（ｂ）の配合量としては、（ａ）液状エポキシ樹脂１００質量部に対して１００〜４００質量部含まれることが好ましく、特に１５０〜２５０質量部の範囲が好ましい。１００質量部未満では、膨張係数が大きく冷熱テストにおいてクラックの発生を誘発させるおそれがある。４００質量部より多いと、粘度が高くなり、薄膜侵入性の低下をもたらす場合がある。 As a compounding quantity of an inorganic filler (b), it is preferable that 100-400 mass parts is contained with respect to 100 mass parts of (a) liquid epoxy resins, and the range of 150-250 mass parts is especially preferable. If the amount is less than 100 parts by mass, the coefficient of expansion is large and there is a risk of inducing cracks in the cooling test. When the amount is more than 400 parts by mass, the viscosity becomes high and the thin film penetration may be lowered.
また、本発明の液状エポキシ樹脂組成物には、２−フェニル−４，５−ジヒドロキシメチルイミダゾール（２ＰＨＺ）硬化促進剤（ｃ）を配合する。２−フェニル−４，５−ジヒドロキシメチルイミダゾール硬化促進剤の平均粒径は３〜５μｍであり、好ましくは３〜４μｍである。３μｍ未満であるとチキソ性が発現し、侵入性を阻害する。５μｍを超えると侵入ゲートでの詰まりが生じ、作業性及び組成のバランスが崩れる等の問題が生ずる。 Moreover, 2-phenyl-4,5-dihydroxymethylimidazole (2PHZ) hardening accelerator (c) is mix | blended with the liquid epoxy resin composition of this invention. The average particle diameter of 2-phenyl-4,5-dihydroxymethylimidazole curing accelerator is 3 to 5 μm, preferably 3 to 4 μm. If it is less than 3 μm, thixotropy is expressed and the invasion is inhibited. If it exceeds 5 μm, clogging occurs at the intrusion gate, causing problems such as the balance between workability and composition being lost.
２−フェニル−４，５−ジヒドロキシメチルイミダゾール硬化促進剤の使用量は、エポキシ樹脂１００質量部に対して０．０１〜１０質量部、特に０．５〜５質量部の範囲で添加することが好適である。添加量が０．０１質量部に満たないと硬化性が低下する場合があり、１０質量部を超えると硬化性に優れるが保存性が低下する場合がある。 The amount of 2-phenyl-4,5-dihydroxymethylimidazole curing accelerator used may be 0.01 to 10 parts by weight, particularly 0.5 to 5 parts by weight, based on 100 parts by weight of the epoxy resin. Is preferred. If the addition amount is less than 0.01 parts by mass, the curability may be lowered, and if it exceeds 10 parts by mass, the curability is excellent but the storage stability may be lowered.
本発明のエポキシ樹脂組成物には、応力を低下させる目的で、シリコーンゴム、シリコーンオイルや液状のポリブタジエンゴムなどを配合してもよい。アルケニル基含有エポキシ樹脂又はフェノール樹脂のアルケニル基と下記平均組成式（１）で示される１分子中の珪素原子の数が２０〜４００であり、珪素原子に直接結合した水素原子（ＳｉＨ基）の数が１〜５であるオルガノポリシロキサンのＳｉＨ基との付加反応により得られる共重合体からなるシリコーン変性樹脂を配合することが好ましい。
ＨaＲbＳｉＯ(4-a-b)/2 （１）
（但し、式中Ｒは置換又は非置換の一価の炭化水素基、ａは０．０１〜０．１、ｂは１．８〜２．２、１．８１≦ａ＋ｂ≦２．３である。）
The epoxy resin composition of the present invention may contain silicone rubber, silicone oil, liquid polybutadiene rubber, or the like for the purpose of reducing stress. The number of silicon atoms in one molecule represented by the following average composition formula (1) and the alkenyl group of the alkenyl group-containing epoxy resin or phenol resin is 20 to 400, and the hydrogen atom (SiH group) directly bonded to the silicon atom It is preferable to blend a silicone-modified resin made of a copolymer obtained by addition reaction with an SiH group of an organopolysiloxane having a number of 1 to 5.
H a R b SiO (4-ab) / 2 (1)
Wherein R is a substituted or unsubstituted monovalent hydrocarbon group, a is 0.01 to 0.1, b is 1.8 to 2.2, and 1.81 ≦ a + b ≦ 2.3. .)
なお、Ｒの置換又は非置換の一価炭化水素基としては、脂肪族不飽和基を含まない炭素数１〜１０、特に１〜８のものが好ましく、メチル基、エチル基、プロピル基、イソプロピル基、ブチル基、イソブチル基、ｔｅｒｔ−ブチル基、ヘキシル基、オクチル基、デシル基等のアルキル基、フェニル基、キシリル基、トリル基等のアリール基、ベンジル基、フェニルエチル基、フェニルプロピル基等のアラルキル基などや、これらの炭化水素基の水素原子の一部又は全部を塩素、フッ素、臭素等のハロゲン原子で置換したフロロメチル基、ブロモエチル基、トリフルオロプロピル基等のハロゲン置換一価炭化水素基を挙げることができる。 The substituted or unsubstituted monovalent hydrocarbon group for R preferably has 1 to 10 carbon atoms, particularly 1 to 8 carbon atoms not containing an aliphatic unsaturated group, and is preferably a methyl group, ethyl group, propyl group or isopropyl group. Group, butyl group, isobutyl group, tert-butyl group, hexyl group, octyl group, decyl group and other alkyl groups, phenyl group, xylyl group, tolyl group and other aryl groups, benzyl group, phenylethyl group, phenylpropyl group, etc. Haloalkyl-substituted monovalent hydrocarbons such as fluoromethyl groups, bromoethyl groups, trifluoropropyl groups, etc., in which some or all of the hydrogen atoms of these hydrocarbon groups are substituted with halogen atoms such as chlorine, fluorine, bromine, etc. The group can be mentioned.
この共重合体としては特に下記式で示されるものが好適である。
上記共重合体をジオルガノポリシロキサン単位がエポキシ樹脂１００質量部に対して２〜１５質量部含まれるように配合することで応力をより一層低下させることができる。 The stress can be further reduced by blending the copolymer so that the diorganopolysiloxane unit is contained in an amount of 2 to 15 parts by mass with respect to 100 parts by mass of the epoxy resin.
本発明の組成物には、更に必要に応じ、接着向上用炭素官能性シラン、カーボンブラックなどの顔料、染料、酸化防止剤、表面処理剤（γ−グリシドキシプロピルトリメトキシシランなど）、その他の添加剤を配合することができる。 If necessary, the composition of the present invention may further include a carbon functional silane for improving adhesion, a pigment such as carbon black, a dye, an antioxidant, a surface treating agent (such as γ-glycidoxypropyltrimethoxysilane), and the like. Additives can be blended.
本発明のエポキシ樹脂組成物は、例えば、液状エポキシ樹脂と無機質充填剤と硬化促進剤を、同時に又は別々に必要により加熱処理を加えながら攪拌、溶解、混合、分散させる。これら混合、攪拌、分散等の装置は特に限定されないが、攪拌、加熱装置を備えたライカイ機、３本ロール、ボールミル、プラネタリーミキサー等を用いることができる。これら装置を適宜組み合わせてもよい。 In the epoxy resin composition of the present invention, for example, a liquid epoxy resin, an inorganic filler, and a curing accelerator are stirred, dissolved, mixed, and dispersed at the same time or separately while applying heat treatment as necessary. There are no particular limitations on the apparatus for mixing, stirring, dispersing, and the like, but a raikai machine equipped with a stirring and heating apparatus, a three roll, a ball mill, a planetary mixer, and the like can be used. You may combine these apparatuses suitably.
得られた液状エポキシ樹脂組成物は、熟成工程を必要とするが、これは２−フェニル−４，５−ジヒドロキシメチルイミダゾール硬化促進剤が、適当な粒度分布を形成し、流動性を良好なものとするために必要な工程と考えられる。熟成は、２０〜３０℃、好ましくは２２〜２７℃で７２〜３３６時間、好ましくは９６〜１６８時間とする。この工程の温度が２０℃未満であると熟成の効果が見られず、侵入性が悪くなり、３０℃を超えると液状エポキシ樹脂との触媒の界面からの反応が進み、高粘度化にともない侵入性が悪化する。また、熟成時間が７２時間未満であると熟成の効果が見られず、侵入性が悪くなり、３３６時間を超えると高粘度化にともない侵入性が悪化する。 The obtained liquid epoxy resin composition requires an aging step. This is because 2-phenyl-4,5-dihydroxymethylimidazole curing accelerator forms an appropriate particle size distribution and has good fluidity. This is considered a necessary process. Aging is carried out at 20 to 30 ° C., preferably 22 to 27 ° C. for 72 to 336 hours, preferably 96 to 168 hours. If the temperature in this step is less than 20 ° C., the effect of aging is not observed, and the penetration property deteriorates. If the temperature exceeds 30 ° C., the reaction proceeds from the interface of the catalyst with the liquid epoxy resin, and the intrusion occurs as the viscosity increases. Sex worsens. Further, when the aging time is less than 72 hours, the effect of aging is not observed, and the penetration property is deteriorated. When the aging time is longer than 336 hours, the penetration property is deteriorated as the viscosity is increased.
得られた液状エポキシ樹脂組成物の粘度は、特にアンダーフィル材として用いる場合に、１００℃において６００〜１０５０ｍＰａ・ｓ、特に７５０〜１０００ｍＰａ・ｓであることが好ましい。なお、本発明において、粘度はブルックフィールド社製Ｅ型粘時計にて、コーンＮｏ４２を使用し、回転数が２０ｒｐｍにて測定することができる。 The viscosity of the obtained liquid epoxy resin composition is preferably 600 to 1050 mPa · s, particularly 750 to 1000 mPa · s at 100 ° C., particularly when used as an underfill material. In the present invention, the viscosity can be measured with a Brookfield E-type viscometer using Corn No. 42 and a rotational speed of 20 rpm.
また、この組成物の成形方法、成形条件は常法とすることができるが、成形条件として好ましくは、先に１４０〜１７０℃、特に１５０〜１６０℃で、１〜５時間、特に２〜４時間の条件で熱オーブンキュアを行う。 The molding method and molding conditions of this composition can be conventional methods, but the molding conditions are preferably 140-170 ° C., particularly 150-160 ° C., 1-5 hours, especially 2-4. Heat oven cure under time conditions.
ここで、デバイスへの封止条件であるが、上記で得られたエポキシ樹脂組成物で封止する際、デバイスの温度条件は６０℃〜１２０℃であることが好ましく、より好ましくは７０℃〜１００℃である。デバイスの温度が６０℃未満であると、組成物の粘度が高いため、基板とチップの隙間を侵入させることができない場合があり、また、１２０℃を超えると反応が生起し、やはり侵入を妨げる原因となるおそれがある。 Here, although it is sealing conditions to a device, when sealing with the epoxy resin composition obtained above, it is preferable that the temperature conditions of a device are 60 degreeC-120 degreeC, More preferably, it is 70 degreeC- 100 ° C. If the temperature of the device is less than 60 ° C., the viscosity of the composition is so high that the gap between the substrate and the chip may not be allowed to enter. If the temperature exceeds 120 ° C., a reaction occurs, which also prevents the penetration. May cause this.
以下、本発明の実施例及び比較例を示して具体的に説明するが、本発明は下記実施例に制限されるものではない。なお、下記表において、部は質量部を示す。 EXAMPLES Hereinafter, the present invention will be specifically described with reference to examples and comparative examples, but the present invention is not limited to the following examples. In the table below, “part” means “part by mass”.
［実施例１〜５、比較例１〜６］
表１，２に示すように、液状エポキシ樹脂としてビスフェノールＦ型エポキシ樹脂（エポトートＹＤＦ−８１７０：東都化成社製）を１００質量部、溶融シリカ（ＬＶＳ−５０１Ｎ、平均粒径５．１μｍ、最大粒径２４μｍ：龍森社製）を２５０質量部、シランカップリング剤（ＫＢＭ４０３、γ−グリシドキシプロピルトリメトキシシラン：信越化学工業社製）を１質量部、各種硬化促進剤（２−フェニル−４，５−ジヒドロキシメチルイミダゾール（２ＰＨＺ）、四国化成製）を１質量部配合し、均一に混練し、表１，２に示す温度及び時間熟成することにより、エポキシ樹脂組成物を得た。
得られたエポキシ樹脂組成物は、１００℃における粘度及び１５０℃におけるゲル化時間の測定を行うとともに、隙間侵入性をチェックした。ここで、粘度はブルックフィールド社製Ｅ型粘度計（コーンＮｏ４２、回転数：２０ｒｐｍ）により測定し、ゲル化時間はスクラッチ法（熱板温度：１５０℃）により測定した。また、隙間侵入性は、得られたエポキシ樹脂組成物を二枚のガラスで４０μｍの隙間をもつデバイスに、１００℃でディスペンスし、１時間後の侵入距離を測定した。これらの結果を表１，２に示す。
[Examples 1-5, Comparative Examples 1-6]
As shown in Tables 1 and 2, 100 parts by mass of bisphenol F type epoxy resin (Epototo YDF-8170: manufactured by Tohto Kasei Co., Ltd.) as a liquid epoxy resin, fused silica (LVS-501N, average particle size 5.1 μm, maximum particle) Diameter 24 μm: Tatsumori Co., Ltd.) 250 parts by mass, silane coupling agent (KBM403, γ-glycidoxypropyltrimethoxysilane: Shin-Etsu Chemical Co., Ltd.) 1 part by mass, various curing accelerators (2-phenyl- An epoxy resin composition was obtained by blending 1 part by mass of 4,5-dihydroxymethylimidazole (2PHZ, manufactured by Shikoku Kasei), kneading uniformly, and aging at the temperatures and times shown in Tables 1 and 2.
The obtained epoxy resin composition was measured for viscosity at 100 ° C. and gelation time at 150 ° C., and checked for gap penetration. Here, the viscosity was measured with a Brookfield E-type viscometer (Cone No. 42, rotation speed: 20 rpm), and the gelation time was measured by a scratch method (hot plate temperature: 150 ° C.). The gap penetration property was determined by dispensing the obtained epoxy resin composition into a device having a gap of 40 μm with two sheets of glass at 100 ° C. and measuring the penetration distance after 1 hour. These results are shown in Tables 1 and 2.
Claims (3)
（ｂ）無機質充填剤，
（ｃ）２−フェニル−４，５−ジヒドロキシメチルイミダゾール硬化促進剤
を必須成分とする半導体封止用液状エポキシ樹脂組成物であって、（ｃ）成分である硬化促進剤の平均粒径が３〜５μｍであり、上記（ａ）〜（ｃ）成分を含む混合・混練物が２０〜３０℃で７２〜３３６時間熟成されてなることを特徴とする半導体封止用液状エポキシ樹脂組成物。 (A) liquid epoxy resin,
(B) inorganic filler,
(C) A liquid epoxy resin composition for semiconductor encapsulation containing 2-phenyl-4,5-dihydroxymethylimidazole curing accelerator as an essential component, wherein the average particle size of the curing accelerator (c) is 3 A liquid epoxy resin composition for semiconductor encapsulation, characterized in that the mixed and kneaded product containing the components (a) to (c) is aged at 20 to 30 ° C. for 72 to 336 hours.
（ｂ）無機質充填剤，
（ｃ）２−フェニル−４，５−ジヒドロキシメチルイミダゾール硬化促進剤
を必須成分とする半導体封止用液状エポキシ樹脂組成物の製造方法であって、（ｃ）成分である硬化促進剤の平均粒径が３〜５μｍであり、上記（ａ）〜（ｃ）を含む混合物を混練した後、２０〜３０℃で７２〜３３６時間熟成することを特徴とする半導体封止用液状エポキシ樹脂組成物の製造方法。 (A) liquid epoxy resin,
(B) inorganic filler,
(C) A method for producing a liquid epoxy resin composition for semiconductor encapsulation containing 2-phenyl-4,5-dihydroxymethylimidazole curing accelerator as an essential component, and (c) average particle of curing accelerator as component A liquid epoxy resin composition for semiconductor encapsulation characterized by having a diameter of 3 to 5 μm and aging the mixture at 20 to 30 ° C. for 72 to 336 hours after kneading the mixture containing (a) to (c) above Production method.
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| US9670377B2 (en) | 2014-03-04 | 2017-06-06 | Namics Corporation | Underfill composition for encapsulating a bond line |
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