JP2001234033A - Epoxy resin composition for optical semiconductor sealing use and optical semiconductor device - Google Patents
Epoxy resin composition for optical semiconductor sealing use and optical semiconductor deviceInfo
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- JP2001234033A JP2001234033A JP2000047441A JP2000047441A JP2001234033A JP 2001234033 A JP2001234033 A JP 2001234033A JP 2000047441 A JP2000047441 A JP 2000047441A JP 2000047441 A JP2000047441 A JP 2000047441A JP 2001234033 A JP2001234033 A JP 2001234033A
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- fatty acid
- epoxy resin
- resin composition
- optical semiconductor
- main chain
- Prior art date
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- Compositions Of Macromolecular Compounds (AREA)
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- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、透明性、光学的均
一性、離型性および耐半田性にすぐれる光半導体封止用
エポキシ樹脂組成物およびその硬化物にて封止された光
半導体装置に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an epoxy resin composition for optical semiconductor encapsulation having excellent transparency, optical uniformity, mold release properties and soldering resistance, and an optical semiconductor encapsulated with a cured product thereof. It concerns the device.
【０００２】[0002]
【従来の技術】半導体封止用エポキシ樹脂に用いる内部
離型剤としては、カルナバワックス等の天然の化合物、
ステアリン酸、ポリオレフィン、脂肪酸エステル、界面
活性剤のような合成化合物などがその目的に応じて使い
分けされている。とりわけ光半導体に用いるエポキシ樹
脂組成物については、樹脂組成物の濁りや着色が極力少
ないことが望まれており、それに合致した内部離型剤を
選択しようとすると、その種類や添加量に制約を受ける
ことがしばしばである。従来、半導体の離型剤として広
く用いられていたカルナバワックスや、その他多くの天
然の化合物は、不純物を含有していることから有色の場
合が多く、光半導体封止用エポキシ樹脂組成物の内部離
型剤としては不適切なことが多い。2. Description of the Related Art As an internal release agent used for an epoxy resin for semiconductor encapsulation, natural compounds such as carnauba wax,
Synthetic compounds such as stearic acid, polyolefins, fatty acid esters and surfactants are properly used depending on the purpose. In particular, for epoxy resin compositions used in optical semiconductors, it is desired that the turbidity and coloring of the resin composition be as low as possible. Often receive. Conventionally, carnauba wax, which has been widely used as a mold release agent for semiconductors, and many other natural compounds are often colored because of containing impurities. Often unsuitable as a release agent.
【０００３】反面、合成により得られた単一の化合物を
用いた場合、樹脂成分との相溶性が非常に問題となる。
離型剤成分が効果を十分に発揮するには、樹脂硬化物の
表面にこれが析出し、金型との界面において作用するこ
とが重要である。硬化時の樹脂との相溶性の低い化合物
を添加すれば、樹脂硬化物と金型の界面に離型剤が析出
し易くなるが、硬化物の表面に析出しなかった成分は、
樹脂硬化物中に粒状で存在し、これが外観上、白濁とな
って、硬化物の透明性を低下させる。On the other hand, when a single compound obtained by synthesis is used, compatibility with the resin component becomes very problematic.
In order for the release agent component to exert its effect sufficiently, it is important that it is deposited on the surface of the cured resin and acts at the interface with the mold. If a compound having low compatibility with the resin at the time of curing is added, the release agent tends to precipitate at the interface between the cured resin and the mold, but the component that did not precipitate on the surface of the cured product is
Granules are present in the cured resin, which becomes opaque in appearance and lowers the transparency of the cured product.
【０００４】これを防ぐためには、離型剤成分が樹脂中
では均一に分散し、硬化物の表面にも析出するような樹
脂組成物とすることが必要である。従来の光半導体向け
エポキシ樹脂組成物では、離型性に関与する成分を樹脂
組成物に均一に分散するために、界面活性剤を添加して
いる。このような界面活性剤としては、脂肪酸エステル
類、高級アルコール類などが用いられているが、これら
を用いて離型剤を均一に分散し、かつ適切な離型性を維
持しようとするには、多量の界面活性剤および過剰な離
型剤を添加せねばならず、そのことによる硬化物物性の
低下が大きな問題となる。In order to prevent this, it is necessary to prepare a resin composition in which the release agent component is uniformly dispersed in the resin and also precipitates on the surface of the cured product. In a conventional epoxy resin composition for an optical semiconductor, a surfactant is added in order to uniformly disperse components relating to mold release properties in the resin composition. As such surfactants, fatty acid esters, higher alcohols, and the like are used. To use these to uniformly disperse the release agent and maintain appropriate release properties. In addition, a large amount of a surfactant and an excessive release agent must be added, which causes a serious problem that the physical properties of the cured product deteriorate.
【０００５】また、界面活性剤に離型性効果を有した化
合物も発案されており、特許第２７８１２７９号では、
樹脂への親和性を持つポリエーテル基と、離型性効果を
発現する高級脂肪酸部からなる界面活性剤を添加するこ
とで、透明性と離型性の両立を狙っている。しかし、こ
の界面活性剤は離型性に関与する成分と相溶性に関与す
る部分との比率を調整するのが非常に難しく、分子設計
レベルでの検討が必要な上、通常の離型剤に比べてその
離型性が低いために、十分な離型性を得るためにはおの
ずと添加量を増やさねばならず、樹脂の耐半田性が劣化
することが知られている。Also, a compound having a releasing effect on a surfactant has been proposed. Japanese Patent No. 2781279 discloses a compound.
By adding a surfactant consisting of a polyether group having an affinity for the resin and a higher fatty acid moiety exhibiting a releasing effect, the aim is to achieve both transparency and releasing property. However, it is very difficult for this surfactant to adjust the ratio between the components involved in release properties and the parts involved in compatibility. It is known that, since the releasability is low, the amount of addition must be increased in order to obtain sufficient releasability, and the solder resistance of the resin deteriorates.
【０００６】[0006]
【発明が解決しようとする課題】本発明は、透明性、光
学的均一性、離型性および耐半田性にすぐれる光半導体
封止用エポキシ樹脂組成物およびその硬化物にて封止さ
れた光半導体装置を提供することを目的とするものであ
る。SUMMARY OF THE INVENTION The present invention relates to an epoxy resin composition for encapsulating an optical semiconductor having excellent transparency, optical uniformity, mold releasability and soldering resistance, and a cured product thereof. It is an object to provide an optical semiconductor device.
【０００７】[0007]
【課題を解決するための手段】本発明者らは、上記の目
的を達成すべく、鋭意検討の結果、特定の飽和脂肪酸を
離型剤に用いることにより、樹脂硬化物の硬化性や物理
特性を低下させることなく、かつ離型性及び透明性にも
優れた光半導体装置用エポキシ樹脂組成物が得られるこ
と見出し、本発明を完成するに至ったのである。Means for Solving the Problems The present inventors have conducted intensive studies in order to achieve the above object, and as a result, by using a specific saturated fatty acid as a release agent, the curability and physical properties of a cured resin product have been improved. The present inventors have found that an epoxy resin composition for an optical semiconductor device having excellent mold release properties and excellent transparency can be obtained without lowering the composition, and the present invention has been completed.
【０００８】すなわち、本発明は、エポキシ樹脂、硬化
剤、硬化促進剤、及び離型剤からなる光半導体封止用エ
ポキシ樹脂組成物において、離型剤が主鎖の炭素数が２
２を越える一価の飽和脂肪酸（Ａ）を必須とし、且つ、
主鎖の炭素数が１６を越え２２以下の一価の飽和脂肪酸
（Ｂ）及び主鎖の炭素数が１６以下の一価の飽和脂肪酸
（Ｃ）からなる群より少なくとも一つ選ばれることを特
徴とする光半導体封止用エポキシ樹脂組成物、That is, the present invention relates to an epoxy resin composition for encapsulating an optical semiconductor comprising an epoxy resin, a curing agent, a curing accelerator, and a release agent, wherein the release agent has 2 carbon atoms in the main chain.
Require two or more monovalent saturated fatty acids (A), and
It is characterized in that at least one is selected from the group consisting of monovalent saturated fatty acids (B) having a main chain carbon number of more than 16 and 22 or less and monovalent saturated fatty acids (C) having a main chain carbon number of 16 or less. Epoxy resin composition for optical semiconductor encapsulation to be
【０００９】エポキシ樹脂、硬化剤、硬化促進剤、及び
離型剤からなる光半導体封止用エポキシ樹脂組成物にお
いて、離型剤が主鎖の炭素数が２２を越える一価の飽和
脂肪酸（Ａ）、主鎖の炭素数が１６を越え２２以下の一
価の飽和脂肪酸（Ｂ）、及び主鎖の炭素数が１６以下の
一価の飽和脂肪酸（Ｃ）からなる群より少なくとも１種
ずつ選ばれることを特徴とする光半導体封止用エポキシ
樹脂組成物、In an epoxy resin composition for encapsulating an optical semiconductor comprising an epoxy resin, a curing agent, a curing accelerator, and a release agent, the release agent is a monovalent resin having a main chain having more than 22 carbon atoms. At least one of the group consisting of a saturated fatty acid (A), a monovalent saturated fatty acid having a main chain carbon number of 16 or more and 22 or less (B), and a monovalent saturated fatty acid (C) having a main chain carbon number of 16 or less. An epoxy resin composition for optical semiconductor encapsulation, which is selected one by one;
【００１０】及び前記いずれかの光半導体封止用エポキ
シ樹脂組成物の硬化物を用いて封止された光半導体装置
である。[0010] An optical semiconductor device encapsulated by using a cured product of any one of the epoxy resin compositions for optical semiconductor encapsulation described above.
【００１１】[0011]
【発明の実施の形態】本発明に用いるエポキシ樹脂とし
ては、一般的に光半導体封止用樹脂組成物に用いられる
エポキシ樹脂であればその種類に何ら制約を受けること
はない。具体的には、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、ビスフェノール
ＡＤ型エポキシ樹脂、ビスフェノールＳ型エポキシ樹脂
などのビスフェノール型エポキシ樹脂、クレゾールノボ
ラック樹脂、フェノールノボラック樹脂などのエポキシ
化フェノール樹脂、トリグリシジルイソシアネート樹
脂、水添ビスフェノールＡ型樹脂などの脂環式エポキシ
樹脂、および脂肪族エポキシ樹脂などがあげられる。BEST MODE FOR CARRYING OUT THE INVENTION The type of epoxy resin used in the present invention is not particularly limited as long as it is an epoxy resin generally used for a resin composition for encapsulating an optical semiconductor. Specifically, bisphenol type epoxy resins such as bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol AD type epoxy resin and bisphenol S type epoxy resin, epoxidized phenol resins such as cresol novolak resin and phenol novolak resin, and Examples thereof include alicyclic epoxy resins such as glycidyl isocyanate resin, hydrogenated bisphenol A type resin, and aliphatic epoxy resin.
【００１２】本発明に用いる硬化剤は、光半導体封止用
エポキシ樹脂に、通常用いられるものであれば、その種
類に何ら制約を受けることはなく、具体的には無水フタ
ル酸、無水マレイン酸、無水トリメリット酸、無水ピロ
メリット酸、ヘキサヒドロ無水フタル酸、３−メチル−
ヘキサヒドロ無水フタル酸、４−メチル−ヘキサヒドロ
無水フタル酸、あるいは３−メチル−ヘキサヒドロ無水
フタル酸と、４−メチル−ヘキサヒドロ無水フタル酸と
の混合物、テトラヒドロ無水フタル酸、無水ナジック
酸、無水メチルナジック酸などの酸無水物硬化剤、フェ
ノールノボラック、クレゾールノボラック、フェノール
アラルキル樹脂、テルペン変性フェノール樹脂、ビスフ
ェノールＡ型ノボラック樹脂、などのフェノール系硬化
剤があげられる。これらの硬化剤は、各々単独であるい
は複数を併用しても構わないThe type of the curing agent used in the present invention is not particularly limited as long as it is generally used in an epoxy resin for encapsulating an optical semiconductor. Examples thereof include phthalic anhydride and maleic anhydride. , Trimellitic anhydride, pyromellitic anhydride, hexahydrophthalic anhydride, 3-methyl-
Hexahydrophthalic anhydride, 4-methyl-hexahydrophthalic anhydride, or a mixture of 3-methyl-hexahydrophthalic anhydride and 4-methyl-hexahydrophthalic anhydride, tetrahydrophthalic anhydride, nadic anhydride, methylnadic anhydride And phenol-based curing agents such as phenol novolak, cresol novolak, phenol aralkyl resin, terpene-modified phenol resin, and bisphenol A type novolak resin. These curing agents may be used alone or in combination of two or more.
【００１３】本発明において、離型剤に用いる一価の飽
和脂肪酸は、その主鎖骨格の炭素数により構成する群が
分けられる。ここで、主鎖骨格とは、飽和脂肪酸のカル
ボキシル基すなわちＣＯＯＨ以外の部位を構成する、飽
和アルキル基のことをさす。In the present invention, the monovalent saturated fatty acids used for the release agent are classified into groups constituted by the number of carbon atoms in the main chain skeleton. Here, the main chain skeleton refers to a saturated alkyl group constituting a site other than the carboxyl group of saturated fatty acid, that is, COOH.
【００１４】本発明に用いる主鎖の炭素数が２２を越え
る一価の飽和脂肪酸（Ａ）としては、リグノセリン酸、
セロチン酸、モンタン酸、メリシン酸などがあげられ
る。これら一価の飽和脂肪酸（Ａ）は、単独でエポキシ
樹脂組成物の離型剤として十分使用できるだけの離型性
を発現する化合物であり、その反面、単独の添加では硬
化物の白濁や表面への過剰な浮き出しが生じることがあ
る。The monovalent saturated fatty acid (A) having a main chain having more than 22 carbon atoms in the present invention includes lignoceric acid,
Cerotic acid, montanic acid, melicic acid and the like. These monovalent saturated fatty acids (A) are compounds that exhibit releasability enough to be used alone as a mold release agent for an epoxy resin composition. Excessive embossing may occur.
【００１５】本発明に用いる主鎖の炭素数が１６を越え
２２以下の一価の飽和脂肪酸（Ｂ）としては、ステアリ
ン酸、アラキジン酸、ベヘニン酸などがあげられる。こ
れら一価の飽和脂肪酸（Ｂ）は、樹脂の種類によっては
単独でも離型性を発揮することができ、一価の飽和脂肪
酸（Ａ）に比べると樹脂への相溶性が良い。しかし、こ
れら一価の飽和脂肪酸（Ｂ）も単独で使用する場合は、
硬化物に濁りを生じずに十分な離型性を得ることは難し
い。The monovalent saturated fatty acid (B) having a carbon number of the main chain of more than 16 and not more than 22 used in the present invention includes stearic acid, arachidic acid, behenic acid and the like. These monovalent saturated fatty acids (B) can exhibit releasability even if used alone depending on the type of the resin, and have better compatibility with the resin than the monovalent saturated fatty acids (A). However, when these monovalent saturated fatty acids (B) are used alone,
It is difficult to obtain sufficient release properties without causing turbidity in the cured product.
【００１６】また、本発明に用いる主鎖の炭素数が１６
以下の一価の飽和脂肪酸（Ｃ）としては、カプリン酸、
ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン
酸などがあげられる。これらＣ群の化合物は、十分な離
型性を発揮することはできないが、樹脂に対する相溶性
に優れており、一価の飽和脂肪酸（Ａ）及び（Ｂ）をエ
ポキシ樹脂へ相溶させる効果を及ぼす。The main chain used in the present invention has 16 carbon atoms.
The following monovalent saturated fatty acids (C) include capric acid,
Lauric acid, myristic acid, palmitic acid, stearic acid and the like can be mentioned. These compounds of Group C cannot exhibit sufficient mold releasability, but are excellent in compatibility with resins, and have an effect of making monovalent saturated fatty acids (A) and (B) compatible with epoxy resins. Exert.
【００１７】これら一価の飽和脂肪酸（Ａ）〜（Ｃ）の
配合比としては、一価の脂肪酸（Ａ）と、（Ｂ）及び
（Ｃ）のうち少なくとも１種で構成され、特に（Ａ）〜
（Ｃ）のすべての群より離型剤が構成されるように調整
されることが望ましい。一価の飽和脂肪酸（Ａ）、
（Ｂ）及び（Ｃ）のうち、一価の飽和脂肪酸（Ａ）が含
まれなければ、樹脂組成物に十分な離型性を与えること
ができず、離型剤としての効果が発揮されない。一価の
飽和脂肪酸（Ｂ）及び（Ｃ）が含まれなければ、樹脂組
成物への相溶性が乏しくなり、白濁を生じてしまう。ま
た、一価の飽和脂肪酸（Ａ）と、一価の飽和脂肪酸
（Ｂ）及び（Ｃ）の配合比率がかけ離れていると、個々
成分の特性の違いから、離型剤全体としての均一性に問
題が生じてしまい、成分がお互いに十分に効果作用を発
揮できなくなる恐れがある。この混合比は、お互いに十
分な作用を及ぼすためには、特定の成分が極端に少なく
なる事は好ましくなく、一価の飽和脂肪酸（Ａ）〜
（Ｃ）からなる群より選ばれる離型剤の各群の合計量
が、それぞれ離型剤全体にたいし１０重量％以上が構成
されるように調整されることが望ましい。こうして各群
の成分が平衡し作用して、本発明で用いられる離型剤
は、光半導体封止用透明エポキシ樹脂組成物に最適な、
離型性と透明性を両立する事ができる。The monovalent saturated fatty acids (A) to (C) are composed of a monovalent fatty acid (A) and at least one of (B) and (C). ) ~
It is desirable to adjust so that the release agent is constituted from all the groups of (C). Monovalent saturated fatty acids (A),
If the monovalent saturated fatty acid (A) is not contained in (B) and (C), sufficient release properties cannot be given to the resin composition, and the effect as a release agent cannot be exhibited. If the monovalent saturated fatty acids (B) and (C) are not contained, the compatibility with the resin composition will be poor, resulting in cloudiness. Further, if the mixing ratio of the monovalent saturated fatty acid (A) and the monovalent saturated fatty acids (B) and (C) are far apart, the uniformity of the release agent as a whole due to the difference in the characteristics of the individual components. A problem may occur and the components may not be able to exert their full effect on each other. In order to exert a sufficient action on each other, it is not preferable that the specific components be extremely small.
It is desirable that the total amount of each group of the release agent selected from the group consisting of (C) is adjusted so as to constitute 10% by weight or more of the entire release agent. The components of each group thus act in equilibrium, and the release agent used in the present invention is optimal for a transparent epoxy resin composition for encapsulating an optical semiconductor.
Both release properties and transparency can be achieved.
【００１８】本発明の離型剤の、代表的な添加量として
は、エポキシ樹脂、及び硬化剤からなる樹脂成分１００
重量部に対し、０．５〜１０重量部が好ましいが、最適
な添加量は前記樹脂成分と離型剤の相溶性により異なる
ため、本特許発明の樹脂組成物が良好な特性を得るため
には、この範囲に限定されるものではない。The typical addition amount of the release agent of the present invention is a resin component 100 composed of an epoxy resin and a curing agent.
With respect to parts by weight, the amount is preferably 0.5 to 10 parts by weight, but the optimum amount to be added depends on the compatibility between the resin component and the release agent, so that the resin composition of the present invention obtains good properties. Is not limited to this range.
【００１９】本発明の光半導体封止用エポキシ樹脂組成
物は、必要に応じて酸化防止剤やカップリング剤、また
特性に影響しない範囲で他の離型剤等、当業者にて公知
の添加剤、副資材を組み合わせることは何らさしつかえ
ない。The epoxy resin composition for encapsulating an optical semiconductor of the present invention may contain, if necessary, an antioxidant or a coupling agent, or other release agents as long as the properties are not affected. Combining agents and sub-materials can be any problem.
【００２０】本発明の樹脂組成物の代表的な製法として
は、エポキシ樹脂、硬化剤、硬化促進剤、離型剤を粉砕
し、混合したのち、加熱ロール等により混練して、冷却
後に再度粉砕して樹脂組成物が得られるが、成形するの
に、タブレット状など必要に応じた形態に加工して用い
る。As a typical method for producing the resin composition of the present invention, an epoxy resin, a curing agent, a curing accelerator, and a release agent are pulverized, mixed, kneaded by a heating roll or the like, cooled, and then pulverized again. The resin composition is obtained by processing into a required form such as a tablet for use in molding.
【００２１】このようにして得られた光半導体封止用エ
ポキシ樹脂組成物を用いての封止は、一般的な方法でで
きるが、例えば、トランスファー成形法等により、光半
導体素子を封止して、エポキシ樹脂組成物の硬化物で封
止された光半導体装置を得ることができる。The optical semiconductor encapsulating epoxy resin composition thus obtained can be encapsulated by a general method. For example, the optical semiconductor element is encapsulated by a transfer molding method or the like. Thus, an optical semiconductor device sealed with a cured product of the epoxy resin composition can be obtained.
【００２２】[0022]
【実施例】以下に、実施例により本発明を更に詳しく説
明するが、本発明は何らこれらに限定されない。EXAMPLES The present invention will be described in more detail with reference to the following Examples, but it should not be construed that the invention is limited thereto.
【００２３】実施例１ 主鎖炭素数２７のモンタン酸を主としてなる脂肪酸（ク
ラリアントジャパン製リコワックスＳ）５０重量部と、
主鎖炭素数１１のラウリン酸を主としてなる脂肪酸（日
本油脂製ＮＡＡ−３１２）５０重量部とを、１５０℃で
加熱混合し、冷却した後にこれを粉砕し、目的の脂肪酸
組成物（１）を得た。この組成物のうち、一価の飽和脂
肪酸（Ａ）（以下Ａ群）、一価の飽和脂肪酸（Ｂ）（以
下Ｂ群）、及び一価の飽和脂肪酸（Ｃ）（以下Ｃ群）に
属する成分の比率は、５０：０：５０（重量％）であっ
た。ビスフェノールＡ型エポキシ樹脂（油化シェル製エ
ピコート１００１、エポキシ当量４５０）７８重量部、
テトラヒドロ無水フタル酸（新日本理化製リカシッド
ＴＨ）２２重量部、上記で得られた脂肪酸組成物（１）
２重量部、２−メチル−４−イミダゾール（四国化成製
２ＭＺ−Ｐ）０．５重量部、トリフェニルホスフェート
（住友化学製スミライザーＴＰＰ）２重量部、２，６−
ジーｔ−ブチル−ｐ−クレゾール（住友化学製スミライ
ザーＢＨＴ−Ｐ）０．５重量部を、ドライブレンドした
後、加熱ロ−ルにて６０℃で溶融混練し、冷却粉砕し
て、エポキシ樹脂組成物を得た後に、タブレット打錠し
評価した。Example 1 50 parts by weight of a fatty acid mainly composed of montanic acid having a main chain carbon number of 27 (Licowax S manufactured by Clariant Japan),
50 parts by weight of a fatty acid (NAA-312 manufactured by NOF Corporation) mainly composed of lauric acid having a main chain carbon number of 11 was heated and mixed at 150 ° C., cooled, and then pulverized to obtain a target fatty acid composition (1). Obtained. Among this composition, it belongs to monovalent saturated fatty acids (A) (hereinafter group A), monovalent saturated fatty acids (B) (hereinafter group B), and monovalent saturated fatty acids (C) (hereinafter group C). The ratio of the components was 50: 0: 50 (% by weight). 78 parts by weight of bisphenol A type epoxy resin (Epicoat 1001, made by Yuka Shell, epoxy equivalent 450),
22 parts by weight of tetrahydrophthalic anhydride (Likacid TH manufactured by Nippon Rika), the fatty acid composition (1) obtained above
2 parts by weight, 0.5 parts by weight of 2-methyl-4-imidazole (2MZ-P manufactured by Shikoku Chemicals), 2 parts by weight of triphenyl phosphate (Sumilyzer TPP manufactured by Sumitomo Chemical), 2,6-
0.5 parts by weight of g-tert-butyl-p-cresol (Sumitomo Chemical Sumitizer BHT-P) was dry-blended, melt-kneaded at 60 ° C. with a heating roll, and cooled and pulverized to obtain an epoxy resin composition. After obtaining the product, it was evaluated by tablet compression.
【００２４】実施例２ 主鎖炭素数２７のモンタン酸を主としてなる脂肪酸（ク
ラリアントジャパン製品 リコワックスＳ）３０重量
部、Ｂ群を含む、主鎖炭素数２１のベヘニン酸を主とし
てなる脂肪酸（日本油脂製品 ＮＡＡ−２２２Ｓ）７０
重量部を、１５０℃で加熱混合し、冷却した後にこれを
粉砕し、目的の脂肪酸組成物（２）を得た。この組成物
のうち、Ａ群、Ｂ群、Ｃ群に属する成分の比率は、３
０：７０：０（重量％）であった。実施例１において用
いた脂肪酸組成物（１）を上記で得た脂肪酸組成物
（２）に代えた以外は、全て実施例１と同様にして、樹
脂組成物を作製し、評価した。Example 2 Fatty acid mainly composed of montanic acid having 27 main chain carbon atoms (Licowax S manufactured by Clariant Japan), 30 parts by weight, fatty acid mainly containing behenic acid having 21 main chain carbon atoms, including Group B (Nippon Yushi) Product NAA-222S) 70
The parts by weight were heated and mixed at 150 ° C., cooled and then pulverized to obtain a desired fatty acid composition (2). In this composition, the ratio of the components belonging to Group A, Group B, and Group C is 3
0: 70: 0 (% by weight). A resin composition was prepared and evaluated in the same manner as in Example 1, except that the fatty acid composition (1) used in Example 1 was replaced with the fatty acid composition (2) obtained above.
【００２５】実施例３ 主鎖炭素数２７のモンタン酸を主としてなる組成物（ク
ラリアントジャパン製リコワックスＳ）２５重量部、Ｂ
群を含む、主鎖炭素数２１のベヘニン酸を主としてなる
脂肪酸（日本油脂製ＮＡＡ−２２２Ｓ）２５重量部、Ｂ
群及びＣ群を含む、主鎖炭素数１７のステアリン酸を主
としてなる脂肪酸（日本油脂製ＮＡＡ−１７５Ｓ）２５
重量部、Ｃ群を含む主鎖炭素数１１のラウリン酸を主と
してなる脂肪酸（日本油脂製ＮＡＡ−３１２）２５重量
部を、１５０℃で加熱混合し、冷却した後にこれを粉砕
し、目的の脂肪酸組成物（３）を得た。この組成物のう
ち、Ａ群、Ｂ群、Ｃ群に属する成分の比率は、２５：３
６：３９（重量％）であった。実施例１において用いた
脂肪酸組成物（１）を上記で得た脂肪酸組成物（３）に
代えた以外は、全て実施例１と同様にして、樹脂組成物
を作製し、評価した。Example 3 25 parts by weight of a composition mainly composed of montanic acid having a main chain carbon number of 27 (Lycowax S manufactured by Clariant Japan), B
25 parts by weight of a fatty acid (NAA-222S manufactured by NOF Corporation) mainly containing behenic acid having 21 main chain carbon atoms,
Fatty acids (NAA-175S, manufactured by NOF Corporation) containing main group stearic acid having 17 carbon atoms, including group C and group C
25 parts by weight of a fatty acid mainly composed of lauric acid having 11 main carbon atoms including group C (NAA-312 manufactured by NOF Corporation) is heated and mixed at 150 ° C., cooled, crushed, and crushed to obtain the desired fatty acid. Composition (3) was obtained. In this composition, the ratio of the components belonging to Group A, Group B, and Group C was 25: 3.
6:39 (% by weight). A resin composition was prepared and evaluated in the same manner as in Example 1, except that the fatty acid composition (1) used in Example 1 was replaced with the fatty acid composition (3) obtained above.
【００２６】実施例４ 主鎖炭素数２７のモンタン酸を主としてなる脂肪酸（ク
ラリアントジャパン製リコワックスＳ）２０重量部、Ｂ
群を含む成分として、主鎖炭素数２１のベヘニン酸を主
としてなる脂肪酸（日本油脂製ＮＡＡ−２２２Ｓ）４０
重量部、Ｂ群及びＣ群を含む主鎖炭素数１１のパルチミ
ン酸を主としてなる脂肪酸（日本油脂製ＮＡＡ−１７
１）４０重量部を、粉砕後に混合し、目的の脂肪酸組成
物（４）を得た。この組成物のうち、Ａ群、Ｂ群、Ｃ群
に属する成分の比率は、２０：４８：３２（重量％）で
あった。実施例１において用いた脂肪酸組成物（１）を
上記で得た脂肪酸組成物（４）に代えた以外は、全て実
施例１と同様にして樹脂組成物を作製し、評価した。Example 4 20 parts by weight of a fatty acid mainly composed of montanic acid having a main chain carbon number of 27 (Licowax S manufactured by Clariant Japan), B
Fatty acids (NAA-222S, manufactured by NOF Corporation) 40 mainly containing behenic acid having a main chain carbon number of 21 as a component containing a group.
Fatty acid mainly composed of partimic acid having main chain carbon number 11 including parts by weight, groups B and C (NAA-17 manufactured by NOF Corporation)
1) 40 parts by weight were mixed after pulverization to obtain a desired fatty acid composition (4). In this composition, the ratio of the components belonging to Group A, Group B, and Group C was 20:48:32 (% by weight). A resin composition was prepared and evaluated in the same manner as in Example 1 except that the fatty acid composition (1) used in Example 1 was replaced with the fatty acid composition (4) obtained above.
【００２７】実施例５ 主鎖炭素数２７のモンタン酸を主としてなる組成物（ク
ラリアントジャパン製リコワックスＳ）３０重量部、Ｂ
群及びＣ群を含む成分として、主鎖炭素数１７のステア
リン酸を主としてなる脂肪酸（日本油脂製ＮＡＡ−１７
５Ｓ）１５重量部、Ｃ群を含む成分として主鎖炭素数１
３のミスチリン酸を主としてなる脂肪酸（日本油脂製Ｎ
ＡＡ−１４２）を５５重量部を、粉砕後に混合し、目的
の脂肪酸組成物（５）を得た。この組成物のうち、Ａ
群、Ｂ群、Ｃ群に属する成分の比率は、３０：８：６２
（重量％）であった。実施例１において用いた脂肪酸組
成物（１）を上記で得た脂肪酸組成物（５）に代えた以
外は、全て実施例１と同様にして樹脂組成物を作製し、
評価した。Example 5 30 parts by weight of a composition mainly composed of montanic acid having a main chain carbon number of 27 (Licowax S manufactured by Clariant Japan), B
Fatty acids mainly containing stearic acid having a main chain carbon number of 17 (NAA-17 manufactured by NOF CORPORATION)
5S) 15 parts by weight, having a main chain carbon number of 1 as a component containing Group C
Fatty acid mainly containing mystyric acid (Nippon Oil & Fats N
AA-142) was mixed with 55 parts by weight after pulverization to obtain a desired fatty acid composition (5). Of this composition, A
The ratio of the components belonging to the group, group B, and group C is 30: 8: 62.
(% By weight). A resin composition was prepared in the same manner as in Example 1, except that the fatty acid composition (1) used in Example 1 was replaced with the fatty acid composition (5) obtained above.
evaluated.
【００２８】比較例１ 実施例１において用いた脂肪酸組成物（１）を、主鎖炭
素数２７のモンタン酸を主としてなる脂肪酸（クラリア
ントジャパン製リコワックスＳ）１００重量部に代えた
以外は、全て実施例１と同様にして樹脂組成物を作製
し、評価した。Comparative Example 1 All of the fatty acid composition (1) used in Example 1 was replaced with 100 parts by weight of a fatty acid mainly composed of montanic acid having 27 carbon atoms in the main chain (Lycowax S manufactured by Clariant Japan). A resin composition was prepared and evaluated in the same manner as in Example 1.
【００２９】比較例２ 実施例１において用いた脂肪酸組成物（１）を、特許第
２７８１２７９号公報に示される界面活性剤（表１に記
載）のポリエーテル鎖とアルキル鎖からなる化合物（ポ
リエーテル繰り返し数１３．５、アルキル鎖炭素数３
６）１００重量部に代えた以外は、全て実施例１と同様
にして樹脂組成物を作製し、評価した。Comparative Example 2 The fatty acid composition (1) used in Example 1 was replaced with a compound (polyether) composed of a polyether chain and an alkyl chain of a surfactant (described in Table 1) disclosed in Japanese Patent No. 2781279. Repetition number 13.5, alkyl chain carbon number 3
6) A resin composition was prepared and evaluated in the same manner as in Example 1 except that the amount was changed to 100 parts by weight.
【００３０】比較例３ 主鎖炭素数２７のモンタン酸を主としてなる脂肪酸（ク
ラリアントジャパン製リコワックスＳ）２０重量部、界
面活性剤として、ステアリン酸エステル組成物（理研ビ
タミン製リケマールＳ−１００）８０重量部を、粉砕後
に混合し、目的の脂肪酸組成物（６）を得た。この組成
物のうち、Ａ群、Ｂ群、Ｃ群に属する成分の比率は、２
０：０：０（重量％）であった。実施例１において用い
た脂肪酸組成物（１）を、上記で得た脂肪酸組成物
（６）に代えた以外は全て実施例１と同様にして樹脂組
成物を作製し、評価した。Comparative Example 3 20 parts by weight of a fatty acid mainly composed of montanic acid having a main chain carbon number of 27 (Lycowax S manufactured by Clariant Japan) and a stearic acid ester composition (Likemar S-100 manufactured by Riken Vitamin Co.) 80 as a surfactant The parts by weight were mixed after pulverization to obtain a desired fatty acid composition (6). In this composition, the ratio of the components belonging to Group A, Group B, and Group C is 2
0: 0: 0 (% by weight). A resin composition was prepared and evaluated in the same manner as in Example 1 except that the fatty acid composition (1) used in Example 1 was replaced with the fatty acid composition (6) obtained above.
【００３１】比較例４ Ｂ群およびＣ群の成分を含む、主鎖炭素数１７のステア
リン酸を主としてなる脂肪酸（日本油脂製ＮＡＡ−１７
５Ｓ）４０重量部と、Ｃ群の成分を含む、主鎖炭素数１
３のミスチリン酸を主としてなる脂肪酸（日本油脂製Ｎ
ＡＡ−１４２）６０重量部とを、１５０℃で加熱混合
し、冷却した後にこれを粉砕し、目的の脂肪酸組成物
（７）を得た。この組成物のうち、Ａ群、Ｂ群、Ｃ群に
属する成分の比率は、０：２１：７９（重量％）であっ
た。実施例１において用いた脂肪酸組成物（１）を、上
記で得た脂肪酸組成物（７）に代えた以外は全て実施例
１と同様にして樹脂組成物を作製し、評価した。COMPARATIVE EXAMPLE 4 A fatty acid mainly containing stearic acid having a main chain carbon number of 17 and containing components of Groups B and C (NAA-17 manufactured by NOF Corporation)
5S) 40 parts by weight and a main chain carbon number of 1 containing a component of Group C
Fatty acid mainly containing mystyric acid (Nippon Oil & Fats N
AA-142) and 150 parts by weight were heated and mixed at 150 ° C., cooled, and then pulverized to obtain a desired fatty acid composition (7). In this composition, the ratio of the components belonging to Group A, Group B, and Group C was 0:21:79 (% by weight). A resin composition was prepared and evaluated in the same manner as in Example 1 except that the fatty acid composition (1) used in Example 1 was replaced with the fatty acid composition (7) obtained above.
【００３２】評価方法は、次のように行い、結果を表１
に示す。 ［光学特性の評価］上記で得た樹脂組成物タブレット
を、金型温度１５０℃、タブレット余熱７０℃、型締め
圧１４．７ＭＰａ（１５０ｋｇ／ｃｍ2）、射出圧力
６．８６ＭＰａ、成形時間３分でトランスファ−成形
し、外形２５×１０×１ｍｍの成形品を得た。この成形
品を目視で確認し、明らかに曇りがかって見えるものを
光学特性不良（×印）、透明性が得られるものを光学特
性良（○印）として、硬化物の光学特性を評価した。The evaluation was performed as follows, and the results are shown in Table 1.
Shown in [Evaluation of optical properties] The resin composition tablet obtained above was subjected to a mold temperature of 150 ° C, a tablet residual heat of 70 ° C, a mold clamping pressure of 14.7 MPa (150 kg / cm 2 ), an injection pressure of 6.86 MPa, and a molding time of 3 minutes. To obtain a molded product having an outer shape of 25 × 10 × 1 mm. The molded product was visually confirmed, and the optical characteristics of the cured product were evaluated as those having a clear cloudy appearance as poor optical characteristics (marked by x) and those exhibiting transparency as good optical characteristics (marked with o).
【００３３】［離型性・耐半田性の評価］上記樹脂組成
物タブレットを、メラミン樹脂クリーニング材によりク
リーニング済みの光半導体用１２ｐＳＯＰタイプパッケ
ージ（４×５ｍｍ、厚み１．２ｍｍ、チップサイズ１．
５ｍｍ×２．０ｍｍ、リードフレーム４２アロイ製）を
用いて、金型温度１７５℃、射出圧力６．８６ＭＰａ、
硬化時間１分の条件でトランスファー成形し、１０ショ
ット目の離型性を評価した。すなわち型開き後イジェク
ターピンが動作した際にカル、ランナー、キャビティー
の各部がひっかかることなく一様に離型すれば○、一部
でもひっかかったり折れたりした場合×とした。耐半田
性評価は同じパッケージを用いて耐半田性評価サンプル
を成形、１５０℃２時間後硬化させた。得られたパッケ
ージを、８５℃、相対湿度６０％の環境下で、１６８時
間吸湿処理し、その後２４０℃のＩＲリフロー処理を行
った。処理したパッケージを顕微鏡及び超音波探傷装置
でクラック、チップと樹脂との剥離の有無を確認。クラ
ック、剥離が発生したものを不良（×印）と判定した。[Evaluation of Releasability and Solder Resistance] The above resin composition tablet was cleaned with a melamine resin cleaning material in a 12 pSOP type package for optical semiconductors (4 × 5 mm, thickness 1.2 mm, chip size 1.
5 mm × 2.0 mm, made of a lead frame 42 alloy), a mold temperature of 175 ° C., an injection pressure of 6.86 MPa,
Transfer molding was performed under the condition of a curing time of 1 minute, and the releasability of the 10th shot was evaluated. That is, when the ejector pin was operated after the mold was opened, each part of the cull, runner, and cavity was uniformly released without being caught, and x was given when any part was caught or broken. For the evaluation of soldering resistance, a sample for evaluating soldering resistance was molded using the same package, and cured at 150 ° C. for 2 hours. The obtained package was subjected to a moisture absorption treatment in an environment of 85 ° C. and a relative humidity of 60% for 168 hours, and then subjected to an IR reflow treatment at 240 ° C. The processed package was checked with a microscope and ultrasonic flaw detector for cracks and peeling of the chip from the resin. Those having cracks and peeling were judged to be defective (x mark).
【００３４】［樹脂組成物の硬化性の評価］上記樹脂組
成物タブレット打錠前のパウダーを用いて、１７５℃熱
板上でこの樹脂組成物がゲル化を始めるまでの時間（ゲ
ルタイム）を観測し、樹脂組成物の硬化性を評価した。[Evaluation of Curability of Resin Composition] Using a powder before tableting the resin composition tablet, a time (gel time) until the resin composition starts to gel on a hot plate at 175 ° C. was observed. The curability of the resin composition was evaluated.
【００３５】[0035]
【表１】 [Table 1]
【００３６】表１記載の評価結果からも明らかなよう
に、本発明による離型剤を用いた樹脂組成物は、その透
明性、離型性、および耐半田性において良好な特性を得
ることができる。それに対し、比較例１では、脂肪酸と
してＡ群に含まれる成分のみを添加したため、離型性に
は優れるが透明性は極端に低くかった。比較例２の、離
型性を有する界面活性剤では、透明性、離型性は得られ
るものの、その物理強度への悪影響が、耐半田性試験で
の不良となった。比較例３では、Ａ群に含まれる、離型
性に優れる脂肪酸類と、界面活性剤の組み合わせによ
る、従来の技術を再現しているが、透明性には優れてい
るが、離型性は十分とはいえず、また速硬化の阻害、耐
半田性の低下などが生じた。比較例４では、Ａ群の成分
を含まず、Ｂ群とＣ群の成分のみで構成された脂肪酸組
成物を用いているが、離型性が十分に得られなかった。As is clear from the evaluation results shown in Table 1, the resin composition using the release agent according to the present invention can obtain good properties in terms of transparency, release property and solder resistance. it can. On the other hand, in Comparative Example 1, since only the components contained in Group A as the fatty acid were added, the releasability was excellent, but the transparency was extremely low. In the surfactant having the releasability of Comparative Example 2, although the transparency and the releasability were obtained, the adverse effect on the physical strength was poor in the solder resistance test. Comparative Example 3 reproduces a conventional technique using a combination of a fatty acid having excellent releasability contained in Group A and a surfactant, but has excellent transparency, but has excellent releasability. It could not be said to be sufficient, and rapid curing was inhibited and solder resistance was lowered. In Comparative Example 4, although the fatty acid composition which does not contain the component of the group A and is composed only of the components of the group B and the group C is used, the releasability was not sufficiently obtained.
【００３７】[0037]
【発明の効果】本発明の光半導体封止用エポキシ樹脂組
成物は、透明性、光学的均一性、離型性および耐半田性
にすぐれ、光半導体の封止に用いるエポキシ樹脂組成物
として優れた性能を発揮することができる。The epoxy resin composition for encapsulating an optical semiconductor according to the present invention is excellent in transparency, optical uniformity, release property and solder resistance, and is excellent as an epoxy resin composition used for encapsulating optical semiconductors. Performance can be demonstrated.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｈ０１Ｌ 33/00 Ｈ０１Ｌ 23/30 Ｆ (72)発明者 瀬川 聡 東京都品川区東品川２丁目５番８号 住友 ベークライト株式会社内 Ｆターム(参考） 4J002 CC032 CD011 CD021 CD051 CD061 CD141 CE002 EF116 EF126 EG017 FD142 FD146 FD158 FD167 GQ05 4J036 AA01 AA02 AD01 AF01 DA04 DB15 FA10 JA07 4M109 AA01 EB09 EC05 EC10 EC11 EC20 GA01 5F041 DA44 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) H01L 33/00 H01L 23 / 30F (72) Inventor Satoshi Segawa 2-5-28 Higashishinagawa, Shinagawa-ku, Tokyo No. Sumitomo Bakelite Co., Ltd. F-term (reference) 4J002 CC032 CD011 CD021 CD051 CD061 CD141 CE002 EF116 EF126 EG017 FD142 FD146 FD158 FD167 GQ05 4J036 AA01 AA02 AD01 AF01 DA04 DB15 FA10 JA07 4M109 AA01 EB09 EC05 EC10 EC10 EC05 EC10
Claims (4)
び離型剤からなる光半導体封止用エポキシ樹脂組成物に
おいて、離型剤が主鎖の炭素数が２２を越える一価の飽
和脂肪酸（Ａ）を必須とし、且つ、主鎖の炭素数が１６
を越え２２以下の一価の飽和脂肪酸（Ｂ）及び主鎖の炭
素数が１６以下の一価の飽和脂肪酸（Ｃ）からなる群よ
り少なくとも一つ選ばれることを特徴とする光半導体封
止用エポキシ樹脂組成物。1. An epoxy resin composition for optical semiconductor encapsulation comprising an epoxy resin, a curing agent, a curing accelerator, and a release agent, wherein the release agent is a monovalent saturated fatty acid having a main chain having more than 22 carbon atoms. (A) is essential and the number of carbon atoms in the main chain is 16
At least one selected from the group consisting of a monovalent saturated fatty acid (B) having a carbon number of not more than 16 and a monovalent saturated fatty acid (C) having a main chain of 16 or less. Epoxy resin composition.
び離型剤からなる光半導体封止用エポキシ樹脂組成物に
おいて、離型剤が主鎖の炭素数が２２を越える一価の飽
和脂肪酸（Ａ）、主鎖の炭素数が１６を越え２２以下の
一価の飽和脂肪酸（Ｂ）、及び主鎖の炭素数が１６以下
の一価の飽和脂肪酸（Ｃ）からなる群より少なくとも１
種ずつ選ばれることを特徴とする光半導体封止用エポキ
シ樹脂組成物。2. An epoxy resin composition for optical semiconductor encapsulation comprising an epoxy resin, a curing agent, a curing accelerator, and a release agent, wherein the release agent is a monovalent saturated fatty acid having a main chain having more than 22 carbon atoms. (A) a monovalent saturated fatty acid having a main chain carbon number of more than 16 and not more than 22 (B); and a monovalent saturated fatty acid having a main chain carbon number of not more than 16 (C).
An epoxy resin composition for encapsulating an optical semiconductor, which is selected by species.
（Ａ）〜（Ｃ）からなる群から少なくとも１種ずつ選ば
れる離型剤の各群の合計量が、全離型剤中に各々１０重
量％以上含まれることを特徴とする請求項２記載の光半
導体封止用エポキシ樹脂組成物。3. The release agent according to claim 2, wherein the total amount of each release agent selected from the group consisting of monovalent saturated fatty acids (A) to (C) is at least one in each of all release agents. The epoxy resin composition for optical semiconductor encapsulation according to claim 2, which is contained in an amount of 10% by weight or more.
体封止用エポキシ樹脂組成物の硬化物を用いて封止され
た光半導体装置。4. An optical semiconductor device encapsulated with a cured product of the epoxy resin composition for optical semiconductor encapsulation according to claim 1.
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|---|---|---|---|
| JP2000047441A JP4543477B2 (en) | 2000-02-24 | 2000-02-24 | Epoxy resin composition for optical semiconductor encapsulation and optical semiconductor device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000047441A JP4543477B2 (en) | 2000-02-24 | 2000-02-24 | Epoxy resin composition for optical semiconductor encapsulation and optical semiconductor device |
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|---|---|
| JP2001234033A true JP2001234033A (en) | 2001-08-28 |
| JP4543477B2 JP4543477B2 (en) | 2010-09-15 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007002233A (en) * | 2005-05-24 | 2007-01-11 | Shin Etsu Chem Co Ltd | Epoxy/silicone resin composition, its cured product and light-emitting semiconductor device encapsulated and protected with the composition |
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| JPH11236489A (en) * | 1998-02-23 | 1999-08-31 | Matsushita Electric Works Ltd | Epoxy resin composition for sealing and semiconductor device |
| JPH11236490A (en) * | 1998-02-23 | 1999-08-31 | Matsushita Electric Works Ltd | Epoxy resin composition for sealing and semiconductor device |
| JPH11269351A (en) * | 1998-03-23 | 1999-10-05 | Nitto Denko Corp | Epoxy resin composition for sealing optical semiconductor element and optical semiconductor device using the same |
| JP2001207027A (en) * | 2000-01-25 | 2001-07-31 | Sumitomo Bakelite Co Ltd | Epoxy resin composition for sealing optical semiconductor and optical semiconductor device |
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2000
- 2000-02-24 JP JP2000047441A patent/JP4543477B2/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06151652A (en) * | 1992-11-16 | 1994-05-31 | Nitto Denko Corp | Semiconductor device |
| JPH11209571A (en) * | 1998-01-26 | 1999-08-03 | Matsushita Electric Works Ltd | Epoxy resin composition for sealing and sealing of semiconductor device |
| JPH11236487A (en) * | 1998-02-23 | 1999-08-31 | Matsushita Electric Works Ltd | Reclaimed powder used in epoxy resin composition for sealing and use thereof |
| JPH11236489A (en) * | 1998-02-23 | 1999-08-31 | Matsushita Electric Works Ltd | Epoxy resin composition for sealing and semiconductor device |
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| JP2001207027A (en) * | 2000-01-25 | 2001-07-31 | Sumitomo Bakelite Co Ltd | Epoxy resin composition for sealing optical semiconductor and optical semiconductor device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007002233A (en) * | 2005-05-24 | 2007-01-11 | Shin Etsu Chem Co Ltd | Epoxy/silicone resin composition, its cured product and light-emitting semiconductor device encapsulated and protected with the composition |
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|---|---|
| JP4543477B2 (en) | 2010-09-15 |
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