JPH06184283A - Resin composition for sealing semiconductor - Google Patents

Resin composition for sealing semiconductor

Info

Publication number
JPH06184283A
JPH06184283A JP34014692A JP34014692A JPH06184283A JP H06184283 A JPH06184283 A JP H06184283A JP 34014692 A JP34014692 A JP 34014692A JP 34014692 A JP34014692 A JP 34014692A JP H06184283 A JPH06184283 A JP H06184283A
Authority
JP
Japan
Prior art keywords
resin
epoxy
resin composition
epoxy resin
inorganic filler
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP34014692A
Other languages
Japanese (ja)
Other versions
JP2716636B2 (en
Inventor
Yoshio Fujieda
義雄 藤枝
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Bakelite Co Ltd
Original Assignee
Sumitomo Bakelite Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sumitomo Bakelite Co Ltd filed Critical Sumitomo Bakelite Co Ltd
Priority to JP34014692A priority Critical patent/JP2716636B2/en
Publication of JPH06184283A publication Critical patent/JPH06184283A/en
Application granted granted Critical
Publication of JP2716636B2 publication Critical patent/JP2716636B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Abstract

PURPOSE:To obtain the subject composition having excellent curability and storage stability by using a specific epoxy resin, a specific microcapsule, a novolak phenolic resin hardener and an inorganic filler as essential components. CONSTITUTION:This resin composition contains, as essential components, (A) an epoxy resin having >=2 epoxy groups in one molecule, e.g. biphenyl-type epoxy compound, (B) a novolak-type phenolic resin hardener, (C) preferably 0.1-0.5wt.% (based on the total composition) of a microcapsule having a releasing temperature of 100-150 deg.C and produced by encapsulating a cure accelerator with a capsule base composed of an acrylic rubber and an inorganic composite material and (D) preferably 70-90wt.% of an inorganic filler such as fused silica powder.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は硬化性と常温での貯蔵安
定性に優れる半導体封止用エポキシ樹脂組成物に関する
ものである。
FIELD OF THE INVENTION The present invention relates to an epoxy resin composition for semiconductor encapsulation which is excellent in curability and storage stability at room temperature.

【0002】[0002]

【従来の技術】一般に半導体封止用エポキシ樹脂組成物
においては、硬化性を向上させるために、硬化促進剤を
使用している。このため常温で放置すると流動性が劣る
等の欠点があり、通常は低温での輸送あるいは低温での
保管により硬化性と貯蔵安定性の両立を図ってきた。し
かしながら、このような低温での輸送あるいは保管は大
幅なコストアップになる。このため硬化性と常温での貯
蔵安定性の両立が強く望まれていた。従来、この硬化性
と貯蔵安定性の両立を図るため、潜在性硬化促進剤の研
究が盛んに行われてきた。その結果テトラ置換ホスホニ
ウム・テトラボレート類(特公昭60−56172号公
報)、4級アンモニウムトリアゾレート化合物(特公昭
60−235828号公報、特公昭60−235830
号公報)等が提案された。しかしながらこれらはいずれ
も硬化性と常温での貯蔵安定性の両立が不可能であっ
た。
2. Description of the Related Art Generally, in a semiconductor encapsulating epoxy resin composition, a curing accelerator is used in order to improve curability. For this reason, there are drawbacks such as poor fluidity when left at room temperature. Usually, both curability and storage stability have been achieved by transporting at low temperature or storing at low temperature. However, transportation or storage at such a low temperature significantly increases the cost. Therefore, it has been strongly desired to achieve both curability and storage stability at room temperature. Conventionally, in order to achieve both curability and storage stability, research on latent curing accelerators has been actively conducted. As a result, tetra-substituted phosphonium tetraborates (Japanese Patent Publication No. 60-56172), quaternary ammonium triazolate compounds (Japanese Patent Publication No. 60-235828, Japanese Patent Publication No. 60-235830).
No. gazette) was proposed. However, it was impossible to achieve both curability and storage stability at room temperature.

【0003】[0003]

【発明が解決しようとする課題】本発明は従来技術で不
可能であった硬化性と常温での貯蔵安定性の両立を目的
として研究した結果、硬化促進剤をマイクロカプセル化
することにより貯蔵安定性が向上するとの知見を得、更
にこの知見に基づき種々の研究を進めて本発明を完成す
るに至ったものである。
The present invention was studied for the purpose of achieving both curability and storage stability at room temperature, which were not possible with the prior art, and as a result, storage stability was improved by encapsulating a curing accelerator. The present invention has been completed by obtaining the knowledge that the property is improved, and further advancing various researches based on this knowledge.

【0004】[0004]

【課題を解決するための手段】本発明は、(A)1分子
中にエポキシ基を少なくとも2個以上有するエポキシ樹
脂、(B)ノボラック型フェノール樹脂硬化剤、(C)
アクリルゴムと無機質複合体からなるカプセル基材で硬
化促進剤を被包してなる溶出温度が100〜150℃の
マイクロカプセルおよび、(D)無機充填材を必須成分
とする半導体封止用樹脂組成物である。
The present invention provides (A) an epoxy resin having at least two epoxy groups in one molecule, (B) a novolac type phenol resin curing agent, (C).
A microcapsule having an elution temperature of 100 to 150 ° C., which is obtained by encapsulating a curing accelerator in a capsule base material made of acrylic rubber and an inorganic composite, and (D) an inorganic filler resin composition for semiconductor encapsulation. It is a thing.

【0005】本発明に用いるエポキシ樹脂は、1分子中
に少なくともエポキシ基を2個以上有するエポキシ樹脂
全般をいう。半導体封止用樹脂組成物に通常用いられる
ものであればよく、例えば、ビフェニル型エポキシ化合
物、ビスフェノール型エポキシ化合物、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、トリフェノールメタン型エポキシ化合物、アル
キル変性トリフェノールメタン型エポキシ化合物及びト
リアジン核含有エポキシ樹脂等が挙げられるが、これら
に限定されるものではない。
The epoxy resin used in the present invention refers to all epoxy resins having at least two epoxy groups in one molecule. What is normally used for the resin composition for semiconductor encapsulation may be used, for example, a biphenyl type epoxy compound, a bisphenol type epoxy compound, a phenol novolac type epoxy resin, a cresol novolac type epoxy resin, a triphenolmethane type epoxy compound, an alkyl modification. Examples thereof include, but are not limited to, triphenolmethane type epoxy compounds and triazine nucleus-containing epoxy resins.

【0006】本発明に用いるノボラック型フェノール樹
脂硬化剤は、半導体封止用樹脂組成物に通常用いられる
ものであればよく、例えば、フェノールノボラック樹
脂、クレゾールノボラック樹脂、ジシクロペンタジエン
変性フェノール樹脂、パラキシレン変性フェノール樹
脂、ナフトール変性フェノール樹脂、フェノール類とベ
ンズアルデヒドあるいはナフチルアルデヒドとの縮合
物、トリフェノールメタン化合物等が挙げが、これらに
限定されるものではない。また、これらの硬化剤の配合
量としてはエポキシ樹脂のエポキシ当量とノボラック型
フェノール樹脂硬化剤の水酸基当量を合わせるように配
合することが好ましい。
The novolac type phenolic resin curing agent used in the present invention may be any one which is usually used in a resin composition for semiconductor encapsulation, and examples thereof include phenol novolac resin, cresol novolac resin, dicyclopentadiene modified phenolic resin and para-novolac resin. Examples thereof include, but are not limited to, a xylene-modified phenol resin, a naphthol-modified phenol resin, a condensate of phenols with benzaldehyde or naphthylaldehyde, and a triphenolmethane compound. Further, it is preferable to mix these curing agents so that the epoxy equivalent of the epoxy resin and the hydroxyl equivalent of the novolac type phenol resin curing agent are matched.

【0007】本発明に用いるマイクロカプセルは、硬化
促進剤をアクリルゴムと無機質複合体からなるカプセル
基材で被包されており、溶出温度が100〜150℃で
あることが必須である。カプセル基材の一成分である無
機質複合体は、一般的な無機質の充填材で溶融シリカ、
結晶シリカ、窒化ケイ素等が挙げられる。硬化促進剤と
しては、トリフェニルホスフィン、ジアザビシクロウン
デセン、トリフェニルホスフィン、2−メチルイミダゾ
ール、ジメチルベンゼンアミン等が挙げられる。
The microcapsules used in the present invention are coated with a curing accelerator in a capsule base material composed of acrylic rubber and an inorganic composite, and it is essential that the elution temperature is 100 to 150 ° C. The inorganic composite, which is one component of the capsule base material, is a common inorganic filler, fused silica,
Examples include crystalline silica and silicon nitride. Examples of the curing accelerator include triphenylphosphine, diazabicycloundecene, triphenylphosphine, 2-methylimidazole, dimethylbenzenamine and the like.

【0008】アクリルゴムと無機質複合体以外のカプセ
ル基材としては、例えばメラミン樹脂、フェノール樹脂
のような材料が考えられるが、これらは耐湿性に影響を
及ぼしたり添加量によっては硬化性に悪影響を及ぼす場
合があるので好ましくない。マイクロカプセルについて
は、粒径の厚みが重要な技術的ポイントである。マイク
ロカプセルの粒径としては20μm以下が好ましい。2
0μmを越えると分散性が悪く、硬化にむらが生じてし
まう。更にカプセル基材の殻厚みは0.5〜5μmが好
ましい。0.5μm未満だと混合・混練時に硬化促進剤
が溶出してしまう。また5μmを越えると成形時に硬化
促進剤が溶出しない。ここでいう溶出温度とは、マイク
ロカプセル化された硬化促進剤が殻を通して外部に溶出
あるいは殻が破壊されることにより、外部に溶出する温
度のことをいう。
As the capsule base material other than the acrylic rubber and the inorganic composite, materials such as melamine resin and phenol resin are conceivable. However, these affect the moisture resistance or the curability depending on the added amount. It may cause adverse effects, which is not preferable. Regarding the microcapsules, the thickness of the particle size is an important technical point. The particle size of the microcapsules is preferably 20 μm or less. Two
If it exceeds 0 μm, the dispersibility is poor and uneven curing occurs. Further, the shell thickness of the capsule base material is preferably 0.5 to 5 μm. If it is less than 0.5 μm, the curing accelerator will be eluted during mixing and kneading. If it exceeds 5 μm, the curing accelerator does not elute during molding. The elution temperature as used herein means the temperature at which the microcapsule-cured curing accelerator is eluted to the outside through the shell or is destroyed by breaking the shell.

【0009】即ち、組成物の混合・混練時には、硬化促
進剤が溶出せず、成形時に溶出することにより硬化促進
剤の触媒作用を引き出すものが好ましい。更に、エポキ
シ樹脂以外の材料であれば、半導体封止用エポキシ樹脂
組成物に対して、異種、異物であり、成形性及び半導体
封止後の物性に悪影響を及ぼしてしまう恐れが大きい。
また、マイクロカプセル化法としては、界面沈殿法、
界面重合法があり、アクリルゴムに無機質複合体を予め
混合したカプセル基材で硬化促進剤を被包しカプセル化
するものである。ここでいうカプセル中の無機質複合体
はアクリルゴムと無機質複合体の全量に対し、30〜9
0%がよく、30%未満だと100〜150℃で硬化促
進剤が容易に溶出してしまう。90%を越えると硬化促
進剤のカプセル化が難しくなる。硬化促進剤の添加量
は、エポキシ樹脂組成物の総量中に0.1〜0.5重量
%であることが好ましい。この範囲以外だと所望の硬化
性が得られない。
That is, it is preferable that the curing accelerator does not elute at the time of mixing and kneading the composition, and the catalytic action of the curing accelerator is brought out by elution at the time of molding. Furthermore, if it is a material other than the epoxy resin, it is different from the epoxy resin composition for semiconductor encapsulation and is a foreign substance, and there is a great possibility that the moldability and the physical properties after semiconductor encapsulation are adversely affected.
As the microencapsulation method, an interfacial precipitation method,
There is an interfacial polymerization method, in which a curing accelerator is encapsulated in a capsule base material in which an acrylic rubber is premixed with an inorganic composite material to encapsulate it. The inorganic composite in the capsule here is 30 to 9 based on the total amount of the acrylic rubber and the inorganic composite.
0% is good, and if it is less than 30%, the curing accelerator easily elutes at 100 to 150 ° C. If it exceeds 90%, it becomes difficult to encapsulate the curing accelerator. The addition amount of the curing accelerator is preferably 0.1 to 0.5% by weight in the total amount of the epoxy resin composition. Outside of this range, the desired curability cannot be obtained.

【0010】本発明で用いる無機充填材としては、溶融
シリカ粉末、球状シリカ粉末、結晶シリカ粉末、2次凝
集シリカ粉末、多孔質シリカ粉末、アルミナ等が挙げら
れ、特に溶融シリカ粉末、球状シリカ粉末、及び溶融シ
リカ粉末と球状シリカ粉末との混合物が好ましい。ま
た、無機充填材の配合量としては、耐半田クラック性と
成形性及び流動性のバランスから総樹脂組成物量に対し
て70〜90重量%が好ましい。
Examples of the inorganic filler used in the present invention include fused silica powder, spherical silica powder, crystalline silica powder, secondary agglomerated silica powder, porous silica powder, alumina and the like, and particularly fused silica powder and spherical silica powder. , And a mixture of fused silica powder and spherical silica powder are preferred. Further, the blending amount of the inorganic filler is preferably 70 to 90% by weight based on the total amount of the resin composition in view of the balance between solder crack resistance, moldability and fluidity.

【0011】本発明の樹脂組成物はエポキシ樹脂、マイ
クロカプセル、および無機充填材を必須成分とするが、
これ以外に必要に応じてシランカップリング剤、ブロム
化エポキシ樹脂、三酸化アンチモン、ヘキサブロムベン
ゼン等の難燃剤、カーボンブラック、ベンガラ等の着色
剤、天然ワックス、合成ワックス等の離型剤及びシリコ
ーンオイル、ゴム等の低応力添加剤等の種々の添加剤を
適宜配合しても差し支えがない。
The resin composition of the present invention contains an epoxy resin, microcapsules, and an inorganic filler as essential components.
In addition to these, silane coupling agents, brominated epoxy resins, flame retardants such as antimony trioxide and hexabromene, colorants such as carbon black and red iron oxide, mold release agents such as natural wax and synthetic wax, and silicones as required. Various additives such as low stress additives such as oil and rubber may be appropriately blended.

【0012】また、本発明の半導体封止用樹脂組成物を
成形材料として製造するには、エポキシ樹脂、マイクロ
カプセル、無機充填材、その他の添加剤をミキサー等に
よって充分に均一に混合した後、更に熱ロールまたはニ
ーダー等で溶融混練し、冷却後粉砕して封止材料とする
ことができる。これらの成形材料は電気部品あるいは電
子部品であるトランジスタ、集積回路等の被覆、絶縁、
封止等に適用することができる。
Further, in order to produce the resin composition for semiconductor encapsulation of the present invention as a molding material, epoxy resin, microcapsules, inorganic fillers and other additives are sufficiently uniformly mixed with a mixer or the like, Further, it can be melt-kneaded with a hot roll or a kneader, cooled, and then pulverized to obtain a sealing material. These molding materials are used to coat and insulate transistors, integrated circuits, etc., which are electrical or electronic components.
It can be applied to sealing and the like.

【0013】以下本発明を実施例で具体的に説明する。 実施例1、2 オルソクレゾールノボラックエポキシ樹脂(軟化点65℃、エポキシ当量20 0) 20重量部 フェノールノボラック樹脂(軟化点95℃、水酸基当量104)10重量部 溶融シリカ 70重量部 脂環式エポキシシラン(日本ユニカー(株)製A−186) 0.5重量部 カーボンブラック 0.5重量部 カルナバワックス 0.5重量部 を表1に示したマイクロカプセル化した硬化促進剤が
0.2重量部となるように添加してブレンダーを用いて
均一に混合し、その後100℃の熱ロールで3分間混練
し、表2に示した組合せの6種類の半導体封止用エポキ
シ樹脂組成物を得た。 これらの成形材料の保存性及び
硬化性の評価結果を表2に示す。
The present invention will be specifically described below with reference to examples. Examples 1 and 2 Orthocresol novolac epoxy resin (softening point 65 ° C., epoxy equivalent 200) 20 parts by weight Phenol novolac resin (softening point 95 ° C., hydroxyl equivalent 104) 10 parts by weight fused silica 70 parts by weight Alicyclic epoxysilane (A-186 manufactured by Nippon Unicar Co., Ltd.) 0.5 parts by weight Carbon black 0.5 parts by weight Carnauba wax 0.5 parts by weight The microcapsulated curing accelerator shown in Table 1 was 0.2 parts by weight. The mixture was added as described above and uniformly mixed using a blender, and then kneaded with a hot roll at 100 ° C. for 3 minutes to obtain 6 kinds of epoxy resin compositions for semiconductor encapsulation in the combinations shown in Table 2. Table 2 shows the evaluation results of the storability and curability of these molding materials.

【0014】評価方法 硬化性:JIS・K6911(成形材料を175℃で成
形し、型開き10秒後の成形品のバコール硬度) 保存性:成形材料を40℃に保管した時に、スパイラル
フローが初期に比べて10%低下するまでの日数)
Evaluation method Curability: JIS K6911 (Bacol hardness of the molding after molding the molding material at 175 ° C. and 10 seconds after mold opening) Storability: When the molding material was stored at 40 ° C., the spiral flow was initially set. 10% less than the number of days)

【0015】比較例1〜7 実施例の組成において、マイクロカプセル化した硬化促
進剤の代わりにトリフェニルホスフィンを用いた以外
は、実施例と同様にして半導体封止用エポキシ樹脂組成
物を得た。これらの成形材料の保存性及び硬化性の評価
結果を表2に示す。
Comparative Examples 1 to 7 Epoxy resin compositions for semiconductor encapsulation were obtained in the same manner as in the examples, except that triphenylphosphine was used instead of the microencapsulated curing accelerator. . Table 2 shows the evaluation results of the storability and curability of these molding materials.

【0016】[0016]

【表1】 [Table 1]

【0017】[0017]

【表2】 [Table 2]

【0018】[0018]

【発明の効果】本発明によると、従来技術をそのまま利
用し、かつ従来技術では両立できなかった硬化性と常温
での貯蔵保存性に優れる半導体封止用エポキシ樹脂組成
物を得ることができる。半導体封止用途では、ますます
プラスチックパッケージ化が進み、そのために硬化性と
常温での貯蔵保存性の両立した半導体封止用エポキシ樹
脂は産業上に非常に有益である。
According to the present invention, it is possible to obtain an epoxy resin composition for semiconductor encapsulation which utilizes the conventional technique as it is and is excellent in curability and storage stability at room temperature, which were not compatible with the conventional technique. In semiconductor encapsulation applications, plastic packaging has been increasingly advanced, and therefore epoxy resin for semiconductor encapsulation, which has both curability and storage stability at room temperature, is very useful in industry.

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】(A)1分子中にエポキシ基を少なくとも
2個以上有するエポキシ樹脂、(B)ノボラック型フェ
ノール樹脂硬化剤、(C)アクリルゴムと無機質複合体
からなるカプセル基材で硬化促進剤を被包してなる溶出
温度が100〜150℃のマイクロカプセルおよび、
(D)無機充填材を必須成分とすることを特徴とする半
導体封止用樹脂組成物。
1. Accelerating curing with (A) an epoxy resin having at least two epoxy groups in one molecule, (B) a novolac-type phenol resin curing agent, and (C) a capsule base material composed of an acrylic rubber and an inorganic composite. A microcapsule having an elution temperature of 100 to 150 ° C., which is formed by encapsulating the agent, and
(D) A resin composition for semiconductor encapsulation, which comprises an inorganic filler as an essential component.
JP34014692A 1992-12-21 1992-12-21 Resin composition for semiconductor encapsulation Expired - Fee Related JP2716636B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP34014692A JP2716636B2 (en) 1992-12-21 1992-12-21 Resin composition for semiconductor encapsulation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP34014692A JP2716636B2 (en) 1992-12-21 1992-12-21 Resin composition for semiconductor encapsulation

Publications (2)

Publication Number Publication Date
JPH06184283A true JPH06184283A (en) 1994-07-05
JP2716636B2 JP2716636B2 (en) 1998-02-18

Family

ID=18334170

Family Applications (1)

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Country Status (1)

Country Link
JP (1) JP2716636B2 (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1009025A2 (en) * 1998-12-08 2000-06-14 Nitto Denko Corporation Epoxy resin composition for encapsulation of semiconductor devices
US6506494B2 (en) 1999-12-20 2003-01-14 3M Innovative Properties Company Ambient-temperature-stable, one-part curable epoxy adhesive
WO2006112396A1 (en) * 2005-04-15 2006-10-26 Hitachi Chemical Co., Ltd. Curing accelerating compound-silica composite material, method for producing curing accelerating compound-silica composite material, curing accelerator, curable resin composition, and electronic component
JP2011225666A (en) * 2010-04-16 2011-11-10 Sekisui Chem Co Ltd Epoxy resin composition

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1009025A2 (en) * 1998-12-08 2000-06-14 Nitto Denko Corporation Epoxy resin composition for encapsulation of semiconductor devices
EP1009025A3 (en) * 1998-12-08 2002-08-28 Nitto Denko Corporation Epoxy resin composition for encapsulation of semiconductor devices
US6506494B2 (en) 1999-12-20 2003-01-14 3M Innovative Properties Company Ambient-temperature-stable, one-part curable epoxy adhesive
WO2006112396A1 (en) * 2005-04-15 2006-10-26 Hitachi Chemical Co., Ltd. Curing accelerating compound-silica composite material, method for producing curing accelerating compound-silica composite material, curing accelerator, curable resin composition, and electronic component
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