JP2000319633A - Silica filter for epoxy resin sealing material - Google Patents

Silica filter for epoxy resin sealing material

Info

Publication number
JP2000319633A
JP2000319633A JP13121999A JP13121999A JP2000319633A JP 2000319633 A JP2000319633 A JP 2000319633A JP 13121999 A JP13121999 A JP 13121999A JP 13121999 A JP13121999 A JP 13121999A JP 2000319633 A JP2000319633 A JP 2000319633A
Authority
JP
Japan
Prior art keywords
silica
epoxy resin
sealing material
filler
particle diameter
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.)
Pending
Application number
JP13121999A
Other languages
Japanese (ja)
Inventor
Yasuhisa Ikeda
泰久 池田
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.)
CI Kasei Co Ltd
Original Assignee
CI Kasei 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 CI Kasei Co Ltd filed Critical CI Kasei Co Ltd
Priority to JP13121999A priority Critical patent/JP2000319633A/en
Publication of JP2000319633A publication Critical patent/JP2000319633A/en
Pending legal-status Critical Current

Links

Abstract

PROBLEM TO BE SOLVED: To obtain a silica filler which can give a sealing material having improved flowability and realizing reduction in burr formation, etc., which filler comprises spherical amorphous silica microparticles having a mean particle diameter in a specified range. SOLUTION: This filler comprises spherical amorphous silica microparticles having a mean particle diameter of 8-65 nm. Desirably, the filler comprises spherical amorphous silica microparticles (A) having a mean particle diameter of 8-65 nm and silica particles (B) having a mean particle diameter of 0.5-40 μm. Desirably, the mixing ratio of component A to component B is such that (A)/[(A)+(B)]=0.01-0.5 by mole. Amorphous silica microparticles A are properly spherical amorphous microparticles produced by a DC arc plasma process and produced by oxidizing silicon in a plasma state and cooling the product and has a specific surface area in a range of 45-300 m2/g (as measured by the BET method).

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、半導体チップ、薄形パ
ッケージの表面実装型樹脂封止型半導体装置に用いられ
るエポキシ樹脂系封止材料用シリカ系充填材に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a silica-based filler for an epoxy resin-based sealing material used for a surface-mounted resin-sealed semiconductor device of a semiconductor chip or a thin package.

【0002】[0002]

【従来の技術】産業の米と言われるまで発展してきた樹
脂封止型半導体装置には、従来、成形硬化後のガラス転
移点Tgが150〜180℃、無機充填剤として天然の
結晶性シリカ粒子又は溶融シリカ粒子あるいはこれら充
填剤の混合物を50〜85重量%含有したエポキシ樹脂
系封止材が使用されている。無機充填材の配合割合が5
0重量%未満では線膨張係数の低減効果が小さく、85
重量%を超えると樹脂組成物の粘度が上昇し、流動性が
低下するという問題がある。また、四塩化珪素の酸水素
焔中での高温加水分解法(気相法)によって得られるア
エロジルのような比表面積が100〜300m2 /gの
ような大きな比表面積を有するシリカ微粒子が従来より
バリ止め対策として数%添加されている。しかし、上記
の製法による比表面積の大きなシリカ微粒子を使用する
と流動性が著しく低下するという欠点がある。
2. Description of the Related Art Conventionally, a resin-encapsulated semiconductor device which has been developed to be called rice in the industry has a glass transition point Tg after molding and curing of 150 to 180 ° C., and natural crystalline silica particles as an inorganic filler. Alternatively, an epoxy resin-based sealing material containing 50 to 85% by weight of fused silica particles or a mixture of these fillers is used. The compounding ratio of the inorganic filler is 5
If the amount is less than 0% by weight, the effect of reducing the coefficient of linear expansion is small.
If the content is more than 10% by weight, there is a problem that the viscosity of the resin composition increases and the fluidity decreases. Further, silica fine particles having a large specific surface area such as Aerosil obtained by a high-temperature hydrolysis method (gas phase method) of silicon tetrachloride in an oxyhydrogen flame have a large specific surface area such as 100 to 300 m 2 / g. Several percent is added as a deburring measure. However, the use of silica fine particles having a large specific surface area according to the above-mentioned production method has a drawback that the fluidity is significantly reduced.

【0003】特に、高実装密度化に対応するため半導体
のパッケージが薄型化する傾向にあるため、封止材の流
動性が高く、バリの発生の少ないポキシ樹脂系封止材料
が求められている。
[0003] In particular, since semiconductor packages tend to be thinner in order to cope with higher packaging densities, there is a need for a oxy-resin-based sealing material that has a high fluidity of the sealing material and less burrs. .

【0004】[0004]

【発明が解決しようとする課題】本発明は、従来の問題
点を解決するため鋭意研究を重ねた結果、エポキシ樹脂
系封止材に使用される充填剤として、(A)平均粒径8
〜65nmの非晶質シリカ微粒子を使用することにより
封止材の流動性を向上させると共に、バリの低減等を実
現できるエポキシ樹脂系封止材料となることを見いだし
たものである。
SUMMARY OF THE INVENTION The present invention has been made as a result of intensive studies to solve the conventional problems.
It has been found that the use of amorphous silica fine particles of up to 65 nm improves the fluidity of the sealing material and provides an epoxy resin-based sealing material that can reduce burrs and the like.

【0005】[0005]

【課題を解決するための手段】すなわち本発明は、エポ
キシ樹脂系封止材料に使用されるシリカ系充填材におい
て、(A)平均粒径8〜65nmの非晶質シリカ微粒子
を使用したことを特徴とするエポキシ樹脂系封止材料用
シリカ系充填材である。
That is, the present invention provides (A) an amorphous silica fine particle having an average particle size of 8 to 65 nm in a silica filler used for an epoxy resin sealing material. Characteristic silica filler for epoxy resin-based sealing materials.

【0006】さらに本発明は、エポキシ樹脂系封止材料
に使用されるシリカ系充填材において、(A)平均粒径
8〜65nmの非晶質シリカ微粒子および(B)平均粒
径0.5〜40μmのシリカ粒子を使用したことを特徴
とするエポキシ樹脂系封止材料用シリカ系充填材であ
る。
Further, the present invention relates to a silica-based filler used for an epoxy resin-based sealing material, wherein (A) amorphous silica fine particles having an average particle size of 8 to 65 nm and (B) average particle size of 0.5 to 65 nm. A silica-based filler for an epoxy resin-based sealing material, characterized by using silica particles of 40 μm.

【0007】上記の(A)平均粒径8〜65nmの非晶
質シリカ微粒子は、直流アークプラズマ法によって製造
されたもので、プラズマ状態の珪素を酸化、冷却するこ
とによって製造された真球状非晶質微粒子で、比表面積
(BET法)が45〜300m2 /gの範囲のものであ
る。
The above-mentioned (A) amorphous silica fine particles having an average particle diameter of 8 to 65 nm are produced by a DC arc plasma method, and are spheric non-spherical particles produced by oxidizing and cooling silicon in a plasma state. A crystalline fine particle having a specific surface area (BET method) of 45 to 300 m 2 / g.

【0008】上記の直流アークプラズマ法は、珪素原料
を消費アノード電極とし、カソード電極からアルゴンガ
スのプラズマフレームを発生させ、前記珪素原料を加
熱、蒸発させ、そのプラズマ状態の珪素を酸化、冷却し
て製造する方法であり、平均粒子径が8〜65nmの範
囲である球状非晶質シリカ微粒子を製造することができ
る。平均粒子径が8nm未満のものは製造の効率が悪く
なり、平均粒子径が65nmを超えるものは粗大粒子が
生成する可能性が大きくなるので好ましくない。この製
法による球状非晶質シリカ微粒子は、極めて緩く凝集し
ているので分散処理が容易であるという特徴を有してい
る。なお、平均粒子径の測定は、比表面積法によって算
出した。
In the DC arc plasma method described above, a silicon material is used as a consumed anode electrode, a plasma flame of argon gas is generated from a cathode electrode, the silicon material is heated and evaporated, and silicon in the plasma state is oxidized and cooled. In this method, spherical amorphous silica fine particles having an average particle diameter in the range of 8 to 65 nm can be manufactured. If the average particle diameter is less than 8 nm, the production efficiency is deteriorated, and if the average particle diameter is more than 65 nm, the possibility of forming coarse particles is increased, which is not preferable. The spherical amorphous silica fine particles produced by this method have a feature that dispersion treatment is easy because they are extremely loosely aggregated. The measurement of the average particle diameter was calculated by a specific surface area method.

【0009】上記の(B)平均粒径0.5〜40μmの
シリカ粒子は、従来より用いられている溶融シリカ、結
晶シリカ、球状シリカ、粉砕シリカなどの充填材であ
り、特に天然珪石や合成シリカをボールミル等で粉砕し
た後、酸素および可燃性ガスによる火炎溶融炉内で溶融
球状化することにより得られる球状溶融シリカ粒子や爆
燃法で得られた球状シリカ粒子が流動性に優れているの
で好ましい。
The (B) silica particles having an average particle size of 0.5 to 40 μm are fillers such as fused silica, crystalline silica, spherical silica, and pulverized silica which have been conventionally used. Spherical silica particles obtained by pulverizing silica with a ball mill or the like and then melting and spheroidizing in a flame melting furnace with oxygen and flammable gas, and spherical silica particles obtained by the deflagration method have excellent fluidity. preferable.

【0010】エポキシ樹脂系封止材料の組成物全体中の
上記のシリカ系充填材の配合割合が、60〜95重量%
であることが好ましく、(A)成分の球状非晶質シリカ
微粒子と(B)成分のシリカ粒子の配合割合が重量比
で、(A)/〔(A)+(B)〕=0.01〜0.5の
範囲が好ましい。この配合割合が0.01未満である
と、流動性の改善効果が小さく、また0.5を超えても
高価な(A)成分の球状非晶質シリカ微粒子の配合割合
に比べてその改善効果が小さくなる傾向となる。
The mixing ratio of the above-mentioned silica-based filler in the entire composition of the epoxy resin-based sealing material is 60 to 95% by weight.
It is preferable that the blending ratio of the spherical amorphous silica fine particles of the component (A) and the silica particles of the component (B) is (A) / [(A) + (B)] = 0.01 by weight ratio. The range of 0.5 to 0.5 is preferable. When the compounding ratio is less than 0.01, the effect of improving the fluidity is small, and even when the compounding ratio exceeds 0.5, the effect of improving the spherical amorphous silica fine particles of the component (A) is expensive. Tend to be smaller.

【0011】また本発明に使用されるエポキシ系樹脂と
しては、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S型エポキシ樹
脂、ビフェニル型エポキシ樹脂、レゾルシノールグリシ
ジルエーテル型エポキシ樹脂等を挙げることができる。
さらに、硬化剤としてはフェノールノボラック樹脂、フ
ェノールアラルキル樹脂などのフェノール系化合物、無
水ピロメリット酸、無水ベンゾフェノンなどの酸無水
物、アミン系化合物等を挙げることができる。
The epoxy resin used in the present invention includes bisphenol A epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin, biphenyl epoxy resin, resorcinol glycidyl ether epoxy resin and the like. it can.
Further, examples of the curing agent include phenolic compounds such as phenol novolak resins and phenol aralkyl resins, acid anhydrides such as pyromellitic anhydride and benzophenone anhydride, and amine compounds.

【0012】さらに、エポキシ樹脂系封止材料には必要
に応じて、難燃剤、着色剤、離型剤、低応力添加剤、硬
化促進剤、カップリング剤などの公知慣用の各種添加剤
を適宜配合することもできる。
Further, various known and commonly used additives such as a flame retardant, a coloring agent, a release agent, a low stress additive, a curing accelerator, and a coupling agent may be appropriately added to the epoxy resin-based sealing material as needed. It can also be blended.

【0013】次に、上述した各成分から封止材料を調整
するには、エポキシ樹脂、硬化剤、(A)球状非晶質シ
リカ微粒子、(B)シリカ粒子、更に必要に応じて、硬
化促進剤、添加剤などを十分混合した後、溶融混練し、
冷却粉砕後、さらに成形機でタブレット状に成形され
る。
Next, in order to adjust the sealing material from the above-described components, an epoxy resin, a curing agent, (A) spherical amorphous silica fine particles, (B) silica particles, and, if necessary, curing acceleration After thoroughly mixing the ingredients, additives, etc., melt kneading,
After being cooled and pulverized, it is further molded into a tablet by a molding machine.

【0014】[0014]

【発明の効果】本発明によれば、エポキシ樹脂系封止材
料に使用する(A)平均粒径8〜65nmの球状非晶質
シリカ微粒子は、エポキシ樹脂系封止材料にチキソトロ
ピー性を付与し、流動性を向上させると共に、バリの低
減等を実現できるという効果を有する。
According to the present invention, the (A) spherical amorphous silica fine particles having an average particle diameter of 8 to 65 nm used for the epoxy resin-based sealing material impart thixotropic properties to the epoxy resin-based sealing material. This has the effect of improving the fluidity and realizing the reduction of burrs and the like.

【0015】[0015]

【実施例】以下、実施例と比較例を示して、本発明を具
体的に説明するが、本発明は下記の実施例に制限される
ものではない。
EXAMPLES Hereinafter, the present invention will be described specifically with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples.

【0016】実施例1〜4、比較例1〜2 エポキシ樹脂(日本化薬社製、「EOCN−102」)
67重量部、硬化剤(大日本インキ化学工業社製、「T
D−2131」)33重量部および表1に示す量(重量
部)のシリカ系充填材に加え、シラン系カップリング剤
2重量部、ワックス0.5重量部、カーボンブラック
0.5重量部、硬化促進剤1重量部を配合した組成物を
二本ロールで均一に溶融混練し、冷却、粉砕して6種類
の熱硬化性樹脂組成物を得た。これらの組成物をスパイ
ラルフローEMM規格に準じた金型を使用し、圧力70
kg/cm2 、温度175℃、120秒の条件でスパイ
ラルフロー値を測定した。
Examples 1-4, Comparative Examples 1-2 Epoxy resin ("EOCN-102", manufactured by Nippon Kayaku Co., Ltd.)
67 parts by weight, curing agent (manufactured by Dainippon Ink and Chemicals, "T
D-2131 ") 33 parts by weight and a silica-based filler in the amount (parts by weight) shown in Table 1, 2 parts by weight of a silane-based coupling agent, 0.5 parts by weight of wax, 0.5 parts by weight of carbon black, The composition containing 1 part by weight of a curing accelerator was uniformly melt-kneaded with two rolls, cooled and pulverized to obtain six types of thermosetting resin compositions. These compositions were used in a mold conforming to the Spiral Flow EMM standard,
The spiral flow value was measured under the conditions of kg / cm 2 , a temperature of 175 ° C. and 120 seconds.

【0017】[0017]

【表1】 [Table 1]

───────────────────────────────────────────────────── 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 23/29 H01L 23/30 R 23/31 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) H01L 23/29 H01L 23/30 R 23/31

Claims (6)

【特許請求の範囲】[Claims] 【請求項1】 エポキシ樹脂系封止材料に使用されるシ
リカ系充填材として、(A)平均粒径8〜65nmの球
状非晶質シリカ微粒子を使用したことを特徴とするエポ
キシ樹脂系封止材料用シリカ系充填材。
1. An epoxy resin-based encapsulation, wherein (A) spherical amorphous silica fine particles having an average particle diameter of 8 to 65 nm are used as a silica-based filler used in an epoxy resin-based encapsulation material. Silica-based filler for materials.
【請求項2】 エポキシ樹脂系封止材料に使用されるシ
リカ系充填材として、(A)平均粒径8〜65nmの球
状非晶質シリカ微粒子および(B)平均粒径0.5〜4
0μmのシリカ粒子を使用したことを特徴とするエポキ
シ樹脂系封止材料用シリカ系充填材。
2. A silica-based filler used in an epoxy resin-based encapsulant, wherein (A) spherical amorphous silica fine particles having an average particle size of 8 to 65 nm and (B) average particle size of 0.5 to 4
A silica-based filler for an epoxy resin-based sealing material, characterized by using silica particles of 0 μm.
【請求項3】 エポキシ樹脂系封止材料組成物全体中の
シリカ系充填材の配合割合が60〜95重量%であるこ
とを特徴とする請求項1または請求項2記載のエポキシ
樹脂系封止材料用シリカ系充填材。
3. The epoxy resin-based encapsulation according to claim 1, wherein the mixing ratio of the silica-based filler in the entire epoxy resin-based encapsulation material composition is 60 to 95% by weight. Silica-based filler for materials.
【請求項4】 (A)成分の球状非晶質シリカ微粒子と
(B)成分のシリカ粒子の配合割合が重量比で、(A)
/〔(A)+(B)〕=0.01〜0.5であることを
特徴とする請求項2または請求項3記載のエポキシ樹脂
系封止材料用シリカ系充填材。
4. A mixing ratio of the spherical amorphous silica fine particles of the component (A) and the silica particles of the component (B) in a weight ratio of (A)
The silica-based filler for an epoxy resin-based sealing material according to claim 2 or 3, wherein /[(A)+(B)]=0.01 to 0.5.
【請求項5】 (A)成分の球状非晶質シリカ微粒子
が、直流アークプラズマ法によって製造されたものであ
ることを特徴とする請求項1ないし請求項4記載のエポ
キシ樹脂系封止材料用シリカ系充填材。
5. The epoxy resin sealing material according to claim 1, wherein the spherical amorphous silica fine particles of the component (A) are produced by a DC arc plasma method. Silica-based filler.
【請求項6】 上記請求項1ないし請求項5に記載され
たエポキシ樹脂系封止材料用シリカ系充填材を使用した
エポキシ樹脂系封止材料。
6. An epoxy resin-based sealing material using the silica-based filler for an epoxy resin-based sealing material according to any one of claims 1 to 5.
JP13121999A 1999-05-12 1999-05-12 Silica filter for epoxy resin sealing material Pending JP2000319633A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP13121999A JP2000319633A (en) 1999-05-12 1999-05-12 Silica filter for epoxy resin sealing material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP13121999A JP2000319633A (en) 1999-05-12 1999-05-12 Silica filter for epoxy resin sealing material

Publications (1)

Publication Number Publication Date
JP2000319633A true JP2000319633A (en) 2000-11-21

Family

ID=15052828

Family Applications (1)

Application Number Title Priority Date Filing Date
JP13121999A Pending JP2000319633A (en) 1999-05-12 1999-05-12 Silica filter for epoxy resin sealing material

Country Status (1)

Country Link
JP (1) JP2000319633A (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002284858A (en) * 2001-03-27 2002-10-03 Sumitomo Bakelite Co Ltd Epoxy resin composition and semiconductor device
JP2002294029A (en) * 2001-03-29 2002-10-09 Sumitomo Bakelite Co Ltd Epoxy resin composition and semiconductor device
JP2002368236A (en) * 2001-06-04 2002-12-20 Nippon Kayaku Co Ltd Sealing agent
US7723407B2 (en) 2004-08-06 2010-05-25 Nippon Shokubai Co., Ltd. Resin composition, method of its composition, and cured formulation
JP2014085638A (en) * 2012-10-26 2014-05-12 Fujicopian Co Ltd Hard coat film
WO2015174141A1 (en) * 2014-05-16 2015-11-19 ナミックス株式会社 Liquid sealing material, and electronic component using same
JP2017005260A (en) * 2006-11-15 2017-01-05 日立化成株式会社 Thermosetting resin composition for light reflection and method for producing the same
US10381533B2 (en) 2006-11-15 2019-08-13 Hitachi Chemical Company, Ltd. Optical semiconductor element mounting substrate and optical semiconductor device using thermosetting resin composition for light reflection

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002284858A (en) * 2001-03-27 2002-10-03 Sumitomo Bakelite Co Ltd Epoxy resin composition and semiconductor device
JP2002294029A (en) * 2001-03-29 2002-10-09 Sumitomo Bakelite Co Ltd Epoxy resin composition and semiconductor device
JP2002368236A (en) * 2001-06-04 2002-12-20 Nippon Kayaku Co Ltd Sealing agent
US7723407B2 (en) 2004-08-06 2010-05-25 Nippon Shokubai Co., Ltd. Resin composition, method of its composition, and cured formulation
JP2017020036A (en) * 2006-11-15 2017-01-26 日立化成株式会社 Thermosetting resin composition for light reflection and manufacturing method therefor
JP2017005260A (en) * 2006-11-15 2017-01-05 日立化成株式会社 Thermosetting resin composition for light reflection and method for producing the same
US10381533B2 (en) 2006-11-15 2019-08-13 Hitachi Chemical Company, Ltd. Optical semiconductor element mounting substrate and optical semiconductor device using thermosetting resin composition for light reflection
JP2014085638A (en) * 2012-10-26 2014-05-12 Fujicopian Co Ltd Hard coat film
WO2015174141A1 (en) * 2014-05-16 2015-11-19 ナミックス株式会社 Liquid sealing material, and electronic component using same
JP2015218229A (en) * 2014-05-16 2015-12-07 ナミックス株式会社 Liquid encapsulant and electronic part
CN106232763A (en) * 2014-05-16 2016-12-14 纳美仕有限公司 Aqueous encapsulation material and use the electronic unit of this aqueous encapsulation material
CN106232763B (en) * 2014-05-16 2018-05-11 纳美仕有限公司 Liquid package material and the electronic unit using the liquid package material
US9994729B2 (en) 2014-05-16 2018-06-12 Namics Corporation Liquid sealing material, and electronic component using same
TWI667267B (en) * 2014-05-16 2019-08-01 日商納美仕有限公司 Liquid encapsulation material, and electronic component using the same

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