JPH04132726A - Epoxy resin composition - Google Patents
Epoxy resin compositionInfo
- Publication number
- JPH04132726A JPH04132726A JP25297590A JP25297590A JPH04132726A JP H04132726 A JPH04132726 A JP H04132726A JP 25297590 A JP25297590 A JP 25297590A JP 25297590 A JP25297590 A JP 25297590A JP H04132726 A JPH04132726 A JP H04132726A
- Authority
- JP
- Japan
- Prior art keywords
- epoxy resin
- bisphenol
- spherical silica
- resin composition
- type epoxy
- 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
Links
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 32
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 32
- 239000000203 mixture Substances 0.000 title claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000945 filler Substances 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- 239000011342 resin composition Substances 0.000 claims description 2
- 239000003566 sealing material Substances 0.000 abstract description 7
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 description 7
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 3
- 238000004191 hydrophobic interaction chromatography Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000008393 encapsulating agent Substances 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- DGUJJOYLOCXENZ-UHFFFAOYSA-N 4-[2-[4-(oxiran-2-ylmethoxy)phenyl]propan-2-yl]phenol Chemical compound C=1C=C(OCC2OC2)C=CC=1C(C)(C)C1=CC=C(O)C=C1 DGUJJOYLOCXENZ-UHFFFAOYSA-N 0.000 description 1
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- -1 isocyanuric anhydride Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
Abstract
Description
【発明の詳細な説明】 （産業上の利用分野） この発明は、エポキシ樹脂組成物に関するものである。[Detailed description of the invention] (Industrial application field) TECHNICAL FIELD This invention relates to an epoxy resin composition.
さらに詳しくは、この発明は、半導体素子や電子部品、
特に水晶振動子用ＨＩＣの封止材等に有用な無溶剤−液
性のエポキシ樹脂組成物に関するものである。More specifically, the present invention relates to semiconductor devices, electronic components,
In particular, the present invention relates to a solvent-free liquid epoxy resin composition useful as a sealing material for HIC for crystal resonators.
（従来の技術）
近年、半導体素子や電子部品の高機能化、高集積化とと
もに、これらに用いる封止材の特性向上が強く求められ
てきており、信頼性向上のための様々な改善が精力的に
進められてきもている。(Conventional technology) In recent years, as semiconductor elements and electronic components have become more sophisticated and highly integrated, there has been a strong demand for improved characteristics of the sealing materials used in these devices, and efforts are being made to make various improvements to improve reliability. There are also progress being made.
たとえば水晶振動子用ＨＩＣについてみると、その生産
は年率で２桁以上の伸びを示し、計算機能、タイマー機
能用等としてその応用範囲が拡大し、これに用いる封止
材に対する特性要求レベルは増々高くなってきている。For example, when looking at HICs for crystal resonators, their production has been growing at an annual rate of more than two digits, and their range of applications has expanded to include calculation functions, timer functions, etc., and the level of performance requirements for the encapsulant used for these is increasing. It's getting expensive.
これまで、これらの水晶振動子用ＨＩＣ等に用いる封止
材としては、封止作業性や信頼性を向上させるためにエ
ポキシ樹脂を主たるものとした溶剤型の封止用樹脂が使
用されてきている。Up until now, solvent-based encapsulation resins mainly made of epoxy resin have been used as encapsulation materials for HICs for crystal resonators, etc. in order to improve encapsulation workability and reliability. There is.
これらの封止用樹脂は、低粘性で、硬化時に溶剤が発散
して充填材が７０〜８０％程度の封止材となるため、低
膨張率、低ガス発生という特徴があり、信頼性も比較的
良好なものであった。These encapsulating resins have low viscosity, and when cured, the solvent is released and the filler becomes a encapsulating material of about 70 to 80%, so they are characterized by low expansion coefficients and low gas generation, and are highly reliable. It was relatively good.
（発明が解決しようとする課題）
しかしながら、この従来の溶剤型エポキシ樹脂封止材の
場合には、充填材が沈降し、粘度変化が生じることが避
けられず、硬化時にはガスが発生して危険であるばかり
か、硬化条件も多段階に設定しなければならないという
封止作業上の難しさがあった。(Problem to be solved by the invention) However, in the case of this conventional solvent-based epoxy resin encapsulant, the filler inevitably settles and changes in viscosity, and gas is generated during curing, which is dangerous. Not only this, but also the curing conditions had to be set in multiple stages, which created difficulties in the sealing process.
また、この従来の封止材の場合には、溶剤が硬化物中に
残るため、これが原因となってガスが発生し、周波数変
動等の障害をもたらしていた。Furthermore, in the case of this conventional sealing material, the solvent remains in the cured product, which causes gas to be generated, causing problems such as frequency fluctuations.
この発明は、以上の通りの事情に鑑みてなされたもので
あり、従来の溶剤型エポキシ樹脂封止材の欠点を改善し
、低粘性、低膨張率であるとともに、粘度変化がな（、
封止作業性が良好で、かつ、ガス発生による障害もなく
、信頼性に優れている封止材を実現することのできる、
無溶剤−液性の新しいエポキシ樹脂組成物を提供するこ
とを目的としている。This invention was made in view of the above-mentioned circumstances, and improves the drawbacks of conventional solvent-type epoxy resin sealants, and provides low viscosity and low expansion coefficient, as well as no change in viscosity.
It is possible to create a sealing material that has good sealing workability, has no problems due to gas generation, and has excellent reliability.
The purpose is to provide a new solvent-free epoxy resin composition.
（課題を解決するための手段）
この発明は、上記の課題を解決するものとして、エポキ
シ樹脂としてビスフェノールＦ型エポキシ樹脂を主たる
ものとし、７０〜８０重量％の粒径の異なる複数種の球
状シリカ充填材を配合してなることを特徴とする無溶剤
−液性のエポキシ樹脂組成物を提供する。(Means for Solving the Problems) This invention solves the above problems by using bisphenol F type epoxy resin as the epoxy resin as the main epoxy resin, and using 70 to 80% by weight of multiple types of spherical silica with different particle sizes. Provided is a solvent-free, liquid-based epoxy resin composition characterized by containing a filler.
また、この発明においては、粒径５〜５０μｍの粒径の
異なる複数種の球状シリカを配合することを好ましい態
様としてもいる。Further, in the present invention, it is a preferred embodiment to blend a plurality of types of spherical silica having different particle sizes of 5 to 50 μm.
ビスフェノールＦ型エポキシ樹脂は、これまでに知られ
ているものを使用することができ、エポキシ樹脂の全量
に対して、少（とも６０重量％、さらに好ましくは７０
〜１００重量％の割合で使用する。この場合、従来より
使用されているビスフェノールＡ型エポキシ樹脂等を上
記の範囲内において適宜に配合することができる。難燃
性を付与したハロゲン化エポキシ樹脂の配合も可能であ
る。As the bisphenol F type epoxy resin, those known so far can be used, and a small amount (at least 60% by weight, more preferably 70% by weight) of the total amount of epoxy resin can be used.
It is used in a proportion of ~100% by weight. In this case, conventionally used bisphenol A type epoxy resins and the like can be appropriately blended within the above range. It is also possible to incorporate a halogenated epoxy resin that has flame retardancy.
粘度１０．０００ｃｐｓ程度のビスフェノールＡ型エポ
キシ樹脂等の従来主流となっていたエポキシ樹脂に代え
て、粘度１．０ＯＯｃｐｓ程度のビスフェノールＦ型エ
ポキシ樹脂を主たるものとすることによって、低粘度化
とともに充填材の最密充填を可能とし、保存時の低粘度
化、充填材沈降や粘度変化の抑制が可能となる。By using bisphenol F type epoxy resin, which has a viscosity of about 1.0OO cps, as the main material instead of the conventionally mainstream epoxy resin such as bisphenol A type epoxy resin, which has a viscosity of about 10.000 cps, the viscosity can be lowered and the filler material can be improved. It is possible to achieve the closest packing of fillers, reduce viscosity during storage, and suppress filler sedimentation and viscosity changes.
また、このビスフェノールＦ型エポキシ樹脂への粒径の
異なる複数種の球状シリカ充填材の配合は、上記の低粘
度化や粘度変化の抑制をさらに効果的なものとする。糸
切れ性も良好となる。Further, the blending of a plurality of types of spherical silica fillers with different particle sizes into this bisphenol F type epoxy resin makes the above-mentioned reduction in viscosity and suppression of viscosity change more effective. Thread breakability is also improved.
この場合の球状シリカ充填材は、その形状が球状であっ
て、かつ、粒径が異なる複数種のものを使用する。その
粒径は、−船釣には８０μｍ以下から選択するのが好ま
しく、たとえば、５μｍ〜５０μｍ程度の範囲から選択
する。この範囲の粒径のシリカ充填材を、２種、３種等
の複数種使用することとする。なお、破砕状シリカの場
合には所期の効果は充分に得られない。In this case, a plurality of types of spherical silica fillers having a spherical shape and different particle sizes are used. The particle size is preferably selected from a range of 80 μm or less for boat fishing, for example, from a range of approximately 5 μm to 50 μm. Two or three types of silica fillers having a particle size within this range are used. In addition, in the case of crushed silica, the desired effect cannot be sufficiently obtained.
また、これらの球状シリカ充填材は、組成物全量に対し
て７０〜８０重量％の範囲となるように配合する。１０
重量％以下の範囲内において、アルミナ、タルク等の他
の無機充填材を配合してもよい。Further, these spherical silica fillers are blended in an amount of 70 to 80% by weight based on the total amount of the composition. 10
Other inorganic fillers such as alumina and talc may be blended within the range of % by weight or less.
溶剤、稀釈剤は、この発明の組成物においては使用しな
い。このため、ガス発生の危険性はな（、周波数変動等
の障害も生じない、硬化時にポーラスにならないため、
ＰＣＴ耐湿信頼性も良好となる。Solvents and diluents are not used in the compositions of this invention. Therefore, there is no risk of gas generation (no problems such as frequency fluctuations, and no porous formation during curing).
PCT moisture resistance reliability is also improved.
もちろん、封止作業性は一段と向上する。Of course, the sealing workability is further improved.
ビスフェノールＦ型エポキシ樹脂、球状シリカ充填材の
他、この発明の組成物には、硬化剤、硬化助剤、その他
の添加剤を適宜に加えることができる。In addition to the bisphenol F type epoxy resin and the spherical silica filler, a curing agent, a curing aid, and other additives can be appropriately added to the composition of the present invention.
硬化剤としては、酸無水物を好適なものとして例示する
ことができる。たとえば、メチルへキサヒドロ無水フタ
ル酸、５−（２，５−ジオキソテトラヒドロ−３−フラ
ニル）−３−メチル−３７シクロヘキセンー１．２−ジ
カルボン酸無水物などが例示される。Suitable examples of the curing agent include acid anhydrides. Examples include methylhexahydrophthalic anhydride, 5-(2,5-dioxotetrahydro-3-furanyl)-3-methyl-37cyclohexene-1,2-dicarboxylic anhydride, and the like.
硬化助材としては、２，４−ジアミノ−６［２′−メチ
ルイミダゾリル−（１）’］エチルー８−トリアジン・
イソシアヌール酸無水物などが例示される。As a curing aid, 2,4-diamino-6[2'-methylimidazolyl-(1)']ethyl-8-triazine.
Examples include isocyanuric anhydride.
以上のこの発明の液状エポキシ樹脂組成物は、たとえば
、前記のような成分を混合した後に、口・−ル、デイス
パー、アジホモミキサー、プラネタリ−ミキサー、ニー
グー、らいかい機などで混練して製造することができる
。この際、粘度が高すぎる時は５０℃程度まで加温して
もよい。なお、混練中および混練後、減圧下で樹脂組成
物中に含まれる気泡を脱気するようにするのが好ましい
。The above-mentioned liquid epoxy resin composition of the present invention can be produced by, for example, mixing the above-mentioned components and then kneading the mixture in a mill, disper, ajihomo mixer, planetary mixer, Nigu, or sieve machine. can do. At this time, if the viscosity is too high, it may be heated to about 50°C. Note that during and after kneading, it is preferable to degas the air bubbles contained in the resin composition under reduced pressure.
実施例１〜５
表１に示した配合割合で、ビスフェノールＦ型エポキシ
樹脂としてビスフェノールＦグリシジルエーテル（エポ
キシ当量１５０、粘度１０００ｃｐｓ）を主たるものと
するエポキシ樹脂組成物を作製した。Examples 1 to 5 Epoxy resin compositions containing bisphenol F glycidyl ether (epoxy equivalent: 150, viscosity: 1000 cps) as the main component of the bisphenol F type epoxy resin were prepared at the blending ratios shown in Table 1.
球状シリカ充填材としては、平均粒径５０μｍ、２０μ
ｍおよび５μｍの３種のものを組合せて使用した。As a spherical silica filler, the average particle size is 50μm, 20μm.
A combination of three types, 5 μm and 5 μm, was used.
このエポキシ樹脂組成物について、その物性、作業性、
信頼性について評価した。その結果を示したものが表２
である。Regarding this epoxy resin composition, its physical properties, workability,
Reliability was evaluated. Table 2 shows the results.
It is.
後述の比較例との対比からも明らかなように、実施例１
〜５のこの発明の組成物の場合には、線膨張率も低く、
物性が良好であるとともに、デイスペンサー吐出性、糸
切れ性の作業性に優れ、しかも、信頼性にも優れた封止
材が得られる。As is clear from the comparison with the comparative example described below, Example 1
In the case of the composition of this invention of ~5, the coefficient of linear expansion is also low,
It is possible to obtain a sealing material that has good physical properties, excellent workability in terms of dispenser dischargeability and thread breakability, and also excellent reliability.
比較例１〜４
比較のために、表１に示した配合のエポキシ樹脂組成物
を作製した。Comparative Examples 1 to 4 For comparison, epoxy resin compositions having the formulations shown in Table 1 were prepared.
ビスフェノールＡ型エポキシ樹脂としては、ビスフェノ
ールＡグリシジルエーテル（エポキシ当量２１０、粘度
１０．０００ｃｐｓ）を使用し、また、反応性稀釈剤と
してはフェニルグリシジルエーテルを、溶剤としてはメ
チルエチルケトンを使用した。Bisphenol A glycidyl ether (epoxy equivalent: 210, viscosity: 10.000 cps) was used as the bisphenol A type epoxy resin, phenyl glycidyl ether was used as the reactive diluent, and methyl ethyl ketone was used as the solvent.
破砕状シリカは、５０μｍ平均粒径のものを使用した。The crushed silica used had an average particle size of 50 μm.
実施例１〜５と同様にして、特性、作業性、信頼性を評
価したが、表２に示した通り、その結果はいずれも実施
例１〜５に比べて劣っていた。Characteristics, workability, and reliability were evaluated in the same manner as Examples 1 to 5, but as shown in Table 2, the results were all inferior to Examples 1 to 5.
（発明の効果）
以上詳しく説明した通り、この発明によって、保存時の
充填材の沈降や粘度変化の心配がなく、硬化時の多段硬
化が必要でないため、従来法に比べてはるかに作業性の
良好な封止材が実現される。(Effects of the invention) As explained in detail above, with this invention, there is no need to worry about settling of the filler or viscosity change during storage, and there is no need for multi-stage curing during curing, so workability is much improved compared to conventional methods. A good sealing material is realized.
また、ガス発生の危険もない。ポーラスにならないため
、ＰＣＴ耐湿信頼性も良好である。There is also no risk of gas generation. Since it does not become porous, the PCT moisture resistance reliability is also good.
さらにまた、硬化物中への溶剤の残存もないため、高湿
保存テストにおいてもガス発生による周波数変動も抑制
される。Furthermore, since no solvent remains in the cured product, frequency fluctuations due to gas generation are suppressed even in high-humidity storage tests.
Claims (2)
樹脂を主たるものとし、７０〜８０重量％の粒径の異な
る複数種の球状シリカ充填材を配合してなることを特徴
とする無溶剤−液性のエポキシ樹脂組成物。(1) A solvent-free, liquid-based epoxy characterized by containing bisphenol F type epoxy resin as the epoxy resin and blending 70 to 80% by weight of multiple types of spherical silica fillers with different particle sizes. Resin composition.
状シリカ充填材を配合してなる請求項（１）記載のエポ
キシ樹脂組成物。(2) The epoxy resin composition according to claim (1), which comprises a plurality of types of spherical silica fillers having different average particle diameters of 5 to 50 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2252975A JP3061141B2 (en) | 1990-09-22 | 1990-09-22 | Epoxy resin composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2252975A JP3061141B2 (en) | 1990-09-22 | 1990-09-22 | Epoxy resin composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04132726A true JPH04132726A (en) | 1992-05-07 |
| JP3061141B2 JP3061141B2 (en) | 2000-07-10 |
Family
ID=17244759
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2252975A Expired - Lifetime JP3061141B2 (en) | 1990-09-22 | 1990-09-22 | Epoxy resin composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3061141B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002275355A (en) * | 2001-03-22 | 2002-09-25 | Sumitomo Bakelite Co Ltd | Epoxy resin composition and semiconductor device |
| JP2010100726A (en) * | 2008-10-23 | 2010-05-06 | Kyocera Chemical Corp | Epoxy resin composition for impregnation casting of molded coil, molded coil device and method for producing molded coil device |
| CN113652188A (en) * | 2021-09-24 | 2021-11-16 | 苏州艾迪亨斯新材料科技有限公司 | Single-component thermosetting packaging adhesive and preparation method thereof |
-
1990
- 1990-09-22 JP JP2252975A patent/JP3061141B2/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002275355A (en) * | 2001-03-22 | 2002-09-25 | Sumitomo Bakelite Co Ltd | Epoxy resin composition and semiconductor device |
| JP2010100726A (en) * | 2008-10-23 | 2010-05-06 | Kyocera Chemical Corp | Epoxy resin composition for impregnation casting of molded coil, molded coil device and method for producing molded coil device |
| CN113652188A (en) * | 2021-09-24 | 2021-11-16 | 苏州艾迪亨斯新材料科技有限公司 | Single-component thermosetting packaging adhesive and preparation method thereof |
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| Publication number | Publication date |
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| JP3061141B2 (en) | 2000-07-10 |
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