JPH0313250B2 - - Google Patents
Info
- Publication number
- JPH0313250B2 JPH0313250B2 JP31417586A JP31417586A JPH0313250B2 JP H0313250 B2 JPH0313250 B2 JP H0313250B2 JP 31417586 A JP31417586 A JP 31417586A JP 31417586 A JP31417586 A JP 31417586A JP H0313250 B2 JPH0313250 B2 JP H0313250B2
- Authority
- JP
- Japan
- Prior art keywords
- epoxy resin
- resistance
- heat cycle
- weight
- silicone
- 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.)
- Expired
Links
- 239000000203 mixture Substances 0.000 claims description 23
- 229920002050 silicone resin Polymers 0.000 claims description 15
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- 239000008096 xylene Substances 0.000 claims description 9
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 claims description 8
- 239000011256 inorganic filler Substances 0.000 claims description 6
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 6
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 6
- 239000003822 epoxy resin Substances 0.000 description 15
- 229920000647 polyepoxide Polymers 0.000 description 15
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 125000001183 hydrocarbyl group Chemical group 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000004014 plasticizer Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- -1 aromatic amine compounds Chemical class 0.000 description 2
- 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 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 238000001723 curing Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000005350 fused silica glass Substances 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000003566 sealing material Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000008065 acid anhydrides Chemical class 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
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- QBNMGMSLXRJOOX-UHFFFAOYSA-N diphenyl-bis(trimethylsilyloxy)silane Chemical compound C=1C=CC=CC=1[Si](O[Si](C)(C)C)(O[Si](C)(C)C)C1=CC=CC=C1 QBNMGMSLXRJOOX-UHFFFAOYSA-N 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 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 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- ZQTYRTSKQFQYPQ-UHFFFAOYSA-N trisiloxane Chemical compound [SiH3]O[SiH2]O[SiH3] ZQTYRTSKQFQYPQ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Description
〔産業上の利用分野〕
本発明は、セラミツク基板を中心にしたハイブ
リツドIC、ダイオード、回路モジユール、パワ
ートランジスタ、ICリレー等の電子部品を注型
封止する液状エポキシ樹脂組成物に関するもので
ある。
〔従来技術〕
電気・電子部品の封止材料に関する必要特性と
して、耐水性と耐ヒートサイクル性が２大特性と
して挙げられる。これらは、互いに相反する特性
であることが認識されている。
ヒートサイクルを向上させる方法としてエポキ
シ樹脂組成物の場合、可撓性を付与するが、低膨
張にするかの２通りが考えられる。
可撓性を付与する手段としては、種々挙げら
れ、主なものとして
可撓性を有するエポキシ樹脂を使用する。
可撓性を有する硬化剤を使用する。
可塑剤を添加して、可撓性を与える等、
があるが、いずれの手段においても、耐湿性特
に、プレツシヤークツカ処理において経時劣化が
激しく実用性に乏しいものになる。
一方、低膨張する組成物を得んとする場合、線
膨張係数の低い無機充填剤を添加し、組成物の熱
膨張を抑える方法が考えられる。しかし、この場
合、無機充填剤の添加にも限界があり、添加量を
多くすると高粘度なものになつてしまい実用化が
難しいのが現状である。
近年、電子部品の信頼性への要求が一段と厳し
くなつてきており、必要特性として耐ヒートサイ
クル性−55℃／150℃位、更にそれと同時に、プ
レツシヤークツカ処理時間が200〜500時間までに
なつてきて、それに対応した絶縁材料が要求され
ている。
耐ヒートサイクル性の改良方法としてエポキシ
樹脂にキシレン樹脂を配合すること（特開昭57−
174944）も提案されているが、これは耐ヒートサ
イクル性はある程度改善されるが、耐プレツシヤ
ークツカ性で未だ十分でない。
〔発明の目的〕
このように、従来耐プレツシヤークツカ性とヒ
ートサイクル性のバランスの取れた適切な材料が
ほとんどなかつたが、本発明はその要求に対応す
べく、研究を重ねた結果、キシレン樹脂及び特定
のシリコン化合物を併用することにより、耐ヒー
トサイクル性と耐プレツシヤークツカ性のバラン
スが取れた材料として液状エポキシ樹脂組成物を
提供するに至つた。
〔発明の構成〕
本発明は、無機充填剤を含有するエポキシ樹脂
組成物において、(a)キシレン樹脂を、好ましくは
組成物全体に対して0.1〜20重量％、及び(b)下記
一般式(1)のシリコン樹脂を、好ましくは組成物全
体に対して0.01〜５重量％含有することを特徴と
する液状エポキシ樹脂組成物であつて、電気・電
子部品を注型封止するのに適したものである。
一般式(1)
（式中、R1，R2，R3，R4，R5，R6，R7，R8，
はそれぞれメチル基またはフエニル基で、これら
のうちメチル基は２〜６個、フエニル基は２〜６
個である。）
本発明に用いられるエポキシ樹脂としては、室
温で液状であることが必須の条件であり、無機充
填剤を高充填できるものが好ましい。そのため比
較的低粘度（300pors／25℃以下）のものがよく、
ビスフエノールＡ型及びビスフエノールＦ型エポ
キシ樹脂で、分子量350〜450程度のものが好まし
い。
硬化剤に関しても、同様に室温で液状のものが
好ましく、加熱硬化タイプが好ましく、比較的
Tg点の高いものがよい。一般的にいえば、芳香
族アミン化合物か、酸無水物がよい。無機充填剤
としては、耐ヒートサイクル性を向上させること
が重要であり、一般的にはシリカ、熔融シリカ、
アルミナ等が挙げられ、不純物を考慮する場合、
一般にそれの少いシリカ系が好ましい。
シリコン樹脂はケイ素原子と酸素原子とが結合
したユニツトを繰返し単位とする主鎖を有し、ケ
イ素原子の酸素原子とを結合していない結合手は
メチル基、フエニル基などの炭化水素基と結合し
ているものである。
シリコン樹脂は電気絶縁性、耐熱性に優れ、且
つ吸湿性が著しく低いため、シリコン樹脂単独で
電気電子部品及び半導体などの絶縁封止材料とし
て用いられている。
しかし本来シリコン樹脂はエポキシ樹脂組成物
と全く相溶性を示さず、このためシリコン樹脂に
種々の有機基を結合させ、変性シリコン樹脂とし
てエポキシ樹脂組成物との相溶性を改良してい
る。しかしこのような変性を施すことにより、シ
リコン樹脂本来の優れた性質が失われることも又
避けられない。
本発明者等はシリコン樹脂の分子量及びケイ素
原子と結合する炭化水素基が特別に限定された範
囲の場合、エポキシ樹脂組成物と良好な相溶性を
有することを発見した。即ち、シリコン樹脂の繰
返し単位が３量体であるトリシロキサンであり、
合計８個の炭化水素基において、メチル基が２個
乃至６個であり、フエニル基が６個乃至２個であ
る場合、エポキシ樹脂組成物と良好な相溶性を有
し、この特別に限定されたシリコン樹脂はエポキ
シ樹脂組成物に対しシリコン樹脂の優れた性質を
維持しつつ、良好なヒートサイクル性向上の効果
を発揮するのである。シリコン樹脂の含有率とし
ては、エポキシ樹脂組成物全体に対し、0.01〜５
重量％が適当である。更に好ましくは、0.3〜3.5
重量％である。含有率が0.01重量％未満では配合
効果が表れない。又含有率が５重量％を越えると
シリコン樹脂の浮き出しなどの非反応性可塑剤と
しての欠点が表われる。
また、本発明に用いられるキシレン樹脂は、室
温において液状であることが好ましい。分子量が
大きくなると共に、液状エポキシ樹脂との相溶性
が悪くなり、耐ヒートサイクル性の向上が不十分
となる傾向にある。従つて、キシレン樹脂は分子
量300〜500が好ましい。具体的には三菱瓦斯化学
(株)のキシレン樹脂「ニカノール」Ｌ，LL，LLL，
Ｈ等が挙げられる。キシレン樹脂の含有率として
は、エポキシ樹脂組成物全体に対して0.1〜20重
量％が適当であり、更に好ましくは、２〜15重量
％である。含有率が0.1重量％未満では配合の効
果が表われないし、20重量％を越えると、キシレ
ン樹脂の浮き出しなどの非反応性可塑剤としての
欠点が表われる。
〔発明の効果〕
本発明の液状エポキシ樹脂組成物は耐ヒートサ
イクルと耐湿性（特に耐プレツシヤークツカ性）
が共にすぐれており、注型材料特に、電気・電子
部品の注型材料に適しており、それらの部品の信
頼性を高めることができる。即ち、従来の液状エ
ポキシ樹脂組成物と比べて、耐ヒートサイクル性
において、３〜４倍以上向上し、かつ、耐プレツ
シヤークツカ性においてもかなりの向上がみられ
る。
〔実施例〕
以下に本発明を実施例を用いて具体的に説明す
る。
表−１に示した様な二液型エポキシ樹脂配合物
で、充填剤含有率はすべて60％に統一し、浴融シ
リカ（平均粒径約20μｍ）を用いた。硬化条件は
120℃５時間である。
その特性結果を表−１の下欄に示した。
[Industrial Application Field] The present invention relates to a liquid epoxy resin composition for casting and sealing electronic components such as hybrid ICs, diodes, circuit modules, power transistors, and IC relays mainly on ceramic substrates. [Prior Art] Water resistance and heat cycle resistance are two major characteristics required for sealing materials for electrical and electronic components. It is recognized that these are mutually contradictory properties. In the case of epoxy resin compositions, there are two possible ways to improve the heat cycle: impart flexibility or reduce expansion. There are various means for imparting flexibility, and epoxy resin having flexibility is mainly used. Use a flexible hardener. There are methods such as adding a plasticizer to impart flexibility, but either method results in severe deterioration over time in moisture resistance, especially in pressure treatment, making it impractical. On the other hand, when it is desired to obtain a composition with low expansion, it is possible to add an inorganic filler having a low coefficient of linear expansion to suppress the thermal expansion of the composition. However, in this case, there is a limit to the addition of inorganic fillers, and increasing the amount added results in high viscosity, making it difficult to put it into practical use. In recent years, the requirements for the reliability of electronic components have become even more stringent, and the required characteristics are heat cycle resistance of -55℃/150℃, and at the same time, pressure processing time of 200 to 500 hours. Insulating materials that meet this trend are in demand. As a method of improving heat cycle resistance, adding xylene resin to epoxy resin (Japanese Patent Application Laid-Open No. 1987-
174944) has also been proposed, but although this improves the heat cycle resistance to some extent, the pressure resistance is still insufficient. [Object of the Invention] As described above, there have been few suitable materials with a good balance between pressure resistance and heat cycle resistance, but the present invention has been developed as a result of repeated research to meet these demands. By using a xylene resin and a specific silicone compound in combination, we have been able to provide a liquid epoxy resin composition as a material with a good balance of heat cycle resistance and pressure scratch resistance. [Structure of the Invention] The present invention provides an epoxy resin composition containing an inorganic filler, in which (a) xylene resin is preferably contained in an amount of 0.1 to 20% by weight based on the entire composition, and (b) the following general formula ( A liquid epoxy resin composition characterized by containing the silicone resin of 1), preferably 0.01 to 5% by weight based on the entire composition, and suitable for casting and sealing electrical and electronic parts. It is something. General formula (1) (In the formula, R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 ,
are each a methyl group or a phenyl group, of which 2 to 6 methyl groups and 2 to 6 phenyl groups
It is individual. ) The epoxy resin used in the present invention must be liquid at room temperature, and is preferably one that can be highly filled with an inorganic filler. Therefore, it is best to use one with a relatively low viscosity (300pors/25℃ or less).
Bisphenol A type and bisphenol F type epoxy resins having a molecular weight of about 350 to 450 are preferred. Regarding the curing agent, similarly, a liquid at room temperature is preferable, a heat-curing type is preferable, and it is relatively hard to use.
One with a high Tg point is better. Generally speaking, aromatic amine compounds or acid anhydrides are preferred. As an inorganic filler, it is important to improve heat cycle resistance, and generally silica, fused silica,
Examples include alumina, and when considering impurities,
In general, silica-based materials with less oxidation are preferred. Silicone resin has a main chain consisting of repeating units in which silicon atoms and oxygen atoms are bonded, and the bonds of silicon atoms that are not bonded to oxygen atoms are bonded to hydrocarbon groups such as methyl groups and phenyl groups. This is what we are doing. Silicone resin has excellent electrical insulation properties and heat resistance, and extremely low moisture absorption, so silicone resin alone is used as an insulating sealing material for electrical and electronic parts, semiconductors, and the like. However, silicone resins originally show no compatibility with epoxy resin compositions, and therefore various organic groups are bonded to silicone resins to improve their compatibility with epoxy resin compositions as modified silicone resins. However, by carrying out such modification, it is also inevitable that the original excellent properties of the silicone resin will be lost. The present inventors have discovered that silicone resin has good compatibility with epoxy resin compositions when its molecular weight and the hydrocarbon group bonded to silicon atoms are within a particularly limited range. That is, the repeating unit of the silicone resin is trisiloxane which is a trimer,
When there are 2 to 6 methyl groups and 6 to 2 phenyl groups among a total of 8 hydrocarbon groups, it has good compatibility with the epoxy resin composition, and this specially limited This silicone resin maintains the excellent properties of silicone resin compared to epoxy resin compositions and exhibits the effect of improving heat cycle properties. The content of silicone resin is 0.01 to 5% relative to the entire epoxy resin composition.
Weight % is appropriate. More preferably 0.3 to 3.5
Weight%. If the content is less than 0.01% by weight, the blending effect will not be apparent. Moreover, if the content exceeds 5% by weight, defects as a non-reactive plasticizer such as embossment of the silicone resin will appear. Further, the xylene resin used in the present invention is preferably liquid at room temperature. As the molecular weight increases, the compatibility with liquid epoxy resin deteriorates, and heat cycle resistance tends to be insufficiently improved. Therefore, the xylene resin preferably has a molecular weight of 300 to 500. Specifically, Mitsubishi Gas Chemical
Co., Ltd.'s xylene resin "Nicanol" L, LL, LLL,
Examples include H. The content of the xylene resin is suitably 0.1 to 20% by weight, more preferably 2 to 15% by weight, based on the entire epoxy resin composition. If the content is less than 0.1% by weight, the effect of the blend will not be apparent, and if it exceeds 20% by weight, defects as a non-reactive plasticizer such as xylene resin embossment will appear. [Effects of the Invention] The liquid epoxy resin composition of the present invention has excellent heat cycle resistance and moisture resistance (especially pressure resistance).
Both of these properties are excellent, making it suitable for casting materials, especially for electrical and electronic components, and can improve the reliability of those components. That is, compared to conventional liquid epoxy resin compositions, the heat cycle resistance is improved by 3 to 4 times or more, and the pressure and scratch resistance is also significantly improved. [Example] The present invention will be specifically described below using Examples. The two-component epoxy resin formulations shown in Table 1 had filler contents of 60%, and bath-fused silica (average particle size of about 20 μm) was used. The curing conditions are
120℃ for 5 hours. The characteristic results are shown in the lower column of Table 1.
【表】
エポキシ樹脂に対し等当量配
東レシリコン(株)製SH−702(ヘキサメチル−ジフ
エニルトリシロキサン）
〔試験方法〕
(1) 耐プレツシヤークツカ試験
条件：125℃、2.3気圧のスチームバスの中で試
験片（50mmφ×３mm）を処理し、外観及
び重量変化を観察した。
(2) ヒートサイクル性
試験片：Ｃワツシヤー（SUS製、径20mm）を
埋め込んだ硬化物（50mmφ×10mm）
処理条件：−50℃／150℃各１時間外観（クラ
ツクの発生有無）を観察した（ｎ＝５）。[Table] Equivalent distribution to epoxy resin SH-702 (hexamethyl-diphenyltrisiloxane) manufactured by Toray Silicon Co., Ltd.
[Test method] (1) Pressure resistance test Conditions: A test piece (50 mmφ x 3 mm) was treated in a steam bath at 125°C and 2.3 atm, and the appearance and weight change were observed. (2) Heat cycle properties Test piece: Cured product (50mmφ x 10mm) embedded with C washers (made of SUS, diameter 20mm) Processing conditions: -50℃/150℃ for 1 hour each The appearance (presence of cracks) was observed (n=5).
Claims (1)
物であつて、該組成物に(a)キシレン樹脂及び(b)下
記一般式(1)のシリコン樹脂を配合することを特徴
とする液状エポキシ樹脂組成物。 一般式(1) （式中、R1，R2，R3，R4，R5，R6，R7，R8，
はそれぞれメチル基またはフエニル基で、これら
のうちメチル基は２〜６個、フエニル基は２〜６
個である。）[Scope of Claims] 1. A liquid epoxy resin composition containing an inorganic filler, characterized in that (a) a xylene resin and (b) a silicone resin represented by the following general formula (1) are blended into the composition. A liquid epoxy resin composition. General formula (1) (In the formula, R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 ,
are each a methyl group or a phenyl group, of which 2 to 6 methyl groups and 2 to 6 phenyl groups
It is individual. )
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31417586A JPS63168426A (en) | 1986-12-27 | 1986-12-27 | Liquid epoxy resin composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31417586A JPS63168426A (en) | 1986-12-27 | 1986-12-27 | Liquid epoxy resin composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63168426A JPS63168426A (en) | 1988-07-12 |
| JPH0313250B2 true JPH0313250B2 (en) | 1991-02-22 |
Family
ID=18050153
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31417586A Granted JPS63168426A (en) | 1986-12-27 | 1986-12-27 | Liquid epoxy resin composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63168426A (en) |
-
1986
- 1986-12-27 JP JP31417586A patent/JPS63168426A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63168426A (en) | 1988-07-12 |
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