JPH0531721A - Preparation of filler material for semiconductor sealing resin - Google Patents
Preparation of filler material for semiconductor sealing resinInfo
- Publication number
- JPH0531721A JPH0531721A JP19431391A JP19431391A JPH0531721A JP H0531721 A JPH0531721 A JP H0531721A JP 19431391 A JP19431391 A JP 19431391A JP 19431391 A JP19431391 A JP 19431391A JP H0531721 A JPH0531721 A JP H0531721A
- Authority
- JP
- Japan
- Prior art keywords
- filler material
- silica
- resin
- foam
- foil
- 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
Links
Landscapes
- Reinforced Plastic Materials (AREA)
Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は半導体封止樹脂などに用
いられるフィラー材の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a filler material used for semiconductor encapsulating resin or the like.
【0002】[0002]
【従来の技術】ICなどの半導体素子は、通常、プラス
チックのパッケージに封入されて使用されている。この
際に用いられる封止用樹脂は、基本的には、エポキシ系
やアクリル系などの有機高分子とシリカ粉などの無機の
フィラー材とから構成されている。フィラー材として使
用される粉体は化学的に安定で電気絶縁性が高く、アル
カリなどの導電性イオンを含まないことが必要である。
このため、フィラー材としては石英ガラスなどのシリカ
系の材料が最も適しており、よく使用されている。2. Description of the Related Art Semiconductor devices such as ICs are usually used by being enclosed in a plastic package. The sealing resin used at this time is basically composed of an organic polymer such as an epoxy-based or acrylic-based polymer and an inorganic filler material such as silica powder. It is necessary that the powder used as the filler material is chemically stable, has high electric insulation, and does not contain conductive ions such as alkali.
Therefore, a silica-based material such as quartz glass is most suitable as the filler material and is often used.
【0003】このフィラー材は、機械的強度の向上、熱
膨張率の低下、熱伝導性の向上、寸法精度の向上など、
封止樹脂の特性向上に寄与している。一般に、フィラー
材の含有率が高いほど、これらの特性を向上できる。This filler material has improved mechanical strength, reduced coefficient of thermal expansion, improved thermal conductivity, and improved dimensional accuracy.
It contributes to the improvement of the characteristics of the sealing resin. Generally, the higher the content of the filler material, the more these properties can be improved.
【0004】一方、封止用樹脂はペレットをモールドす
る際に十分な流動性を持つ必要がある。しかし、フィラ
ー材の含有率が高いほど、良好な流動性を保つことが困
難になるという問題が生じる。On the other hand, the encapsulating resin must have sufficient fluidity when molding the pellets. However, the higher the content of the filler material, the more difficult it becomes to maintain good fluidity.
【0005】近年になって、素子の高集積化、ペレット
の大型化が進むとともに、パッケージの小型化、薄型化
が要請されるようになった。その結果、機械的強度など
の特性を低下させないで、いままで以上の流動性が要求
されるようになってきている。[0005] In recent years, with higher integration of elements and larger pellets, there has been a demand for smaller and thinner packages. As a result, more fluidity than ever has been required without deteriorating properties such as mechanical strength.
【0006】[0006]
【発明が解決しようとする課題】樹脂の流動性を向上さ
せる手段として、フィラー材粒子の形状を制御する方法
が知られている。例えば、シリカ破砕粉の代わりに、丸
く角の少ない球状シリカなどのフィラー材を用いれば、
その目的を達成できる。しかし、このようにフィラー材
の形状を制御すると、どうしても樹脂の強度が低下して
しまい、目的の強度を得ることは非常に困難であった。As a means for improving the fluidity of resin, a method of controlling the shape of filler material particles is known. For example, if instead of crushed silica powder, a filler material such as spherical silica with a small number of rounded corners is used,
You can achieve that purpose. However, when the shape of the filler material is controlled in this way, the strength of the resin is inevitably lowered, and it is very difficult to obtain the desired strength.
【0007】樹脂の強度を損なわずに流動性を向上させ
る手段として、繊維状又は箔片状のフィラー材を使用す
る方法が知られている。これらの形状のフィラー材は、
樹脂が流動するときに流線の方向に配向するので、流動
時の抵抗が小さくなる。特に、箔片状のフィラー材では
この効果が顕著であり、しかも強度の増加も期待でき
る。As a means for improving the fluidity without impairing the strength of the resin, a method of using a fibrous or foil piece filler material is known. These shaped filler materials
Since the resin is oriented in the streamline direction when flowing, the resistance when flowing decreases. In particular, this effect is remarkable in the case of a foil-shaped filler material, and an increase in strength can be expected.
【0008】しかし、従来、このような箔片状シリカ
は、例えば石英ガラスの融液に空気などを吹き込んで極
薄の球をつくり、それを破砕するなど極めて非能率な方
法でしか入手できず、実用上大きな障害となっていた。
本発明は、シリカ質の箔片状のフィラー材を簡便で安価
に製造できる方法を提供することを目的とする。However, conventionally, such a piece of foil-like silica can be obtained only by an extremely inefficient method, for example, by blowing air or the like into a melt of quartz glass to form an extremely thin sphere and crushing it. , Was a big obstacle in practical use.
It is an object of the present invention to provide a method for easily and inexpensively producing a filler material in the form of a siliceous foil.
【0009】[0009]
【課題を解決するための手段と作用】本発明の半導体封
止樹脂用フィラー材の製造方法は、シリカ質の発泡体を
形成した後、この発泡体を破砕することを特徴とするも
のである。本発明において、シリカ質の発泡体とは、多
量の泡を内部に含む無定型シリカを意味する。このよう
な発泡体を得るには、以下のような方法が用いられる。The method for producing a filler material for a semiconductor encapsulating resin of the present invention is characterized by forming a siliceous foam and then crushing the foam. .. In the present invention, the siliceous foam means an amorphous silica containing a large amount of bubbles therein. To obtain such a foam, the following method is used.
【0010】1)水、空気など、加熱するとガスとなっ
て揮散する成分を多量に含むシリカ原料を急速に加熱し
て、軟化溶融させる。2)シリカゾルに発泡剤などを添
加し、加熱してゲル化させるとともに発泡させ、これを
焼成してシリカ発泡体とする。3)発泡剤を含む水など
の溶剤中にシリカ粉末を分散させて発泡体とし、これを
焼成する。これらの方法は、単独で用いてもよいし、組
み合わせて用いてもよい。1) A silica raw material containing a large amount of components that volatilize into a gas when heated, such as water and air, is rapidly heated to soften and melt. 2) A foaming agent or the like is added to silica sol, heated to cause gelation and foaming, and this is fired to obtain a silica foam. 3) Silica powder is dispersed in a solvent such as water containing a foaming agent to form a foam, which is then fired. These methods may be used alone or in combination.
【0011】以上のような方法で作製されたシリカ発泡
体を、ボールミルなどの通常の手段で粉砕することによ
り、目的とする箔片状のフィラー材が得られる。破砕粉
の中の箔片状シリカは、当初の発泡体において泡と泡と
が接した界面の隔壁に由来する。したがって、泡の密度
が高いほど、箔片状シリカの含量も多くなる。逆に、泡
どうしが接触しない程度に泡の密度が低い場合には、目
的とする箔片状シリカは得られない。By crushing the silica foam produced by the above method by a usual means such as a ball mill, a desired foil-shaped filler material can be obtained. The foil-like silica in the crushed powder originates from the partition walls at the interface where bubbles are in contact with each other in the original foam. Therefore, the higher the density of the foam, the higher the content of the flaky silica. On the contrary, if the density of bubbles is low enough that the bubbles do not come into contact with each other, the desired foil-like silica cannot be obtained.
【0012】なお、破砕粉の中には箔片状でない形状の
ものも混在する。したがって、特に樹脂の流動性を向上
させたい場合など、例えば浮遊法などの手段を用いて、
このような破砕粉の中から箔片状のものだけを選別して
もよい。ただし、通常の破砕型の形状の粉末粒子の中に
箔片状シリカが混在するものをフィラー材として用いて
も、樹脂の流動性を向上できる。実験によれば、フィラ
ー材中の箔片状シリカの割合が20%以上であれば、樹
脂の流動性を向上させる効果が得られることが判明して
いる。It should be noted that the crushed powder also contains a non-foil-like shape. Therefore, especially when it is desired to improve the fluidity of the resin, for example, by using a method such as a floating method,
Only the pieces in the form of foil may be selected from such crushed powder. However, the fluidity of the resin can be improved by using, as the filler material, the one in which the foil-shaped silica is mixed in the powder particles of the usual crush type. Experiments have revealed that the effect of improving the fluidity of the resin can be obtained when the proportion of the flake-like silica in the filler material is 20% or more.
【0013】また、フィラー材として樹脂の流動性を向
上させる効果がある箔片状シリカの形状は、厚さ0.1
〜10μm、最大幅100μm以下である。前述した種
々の方法で作製したシリカ質の発泡体の段階で、泡の平
均径が0.05〜0.5mmの範囲であれば、これを破
砕した粉末中にこのような形状の箔片状シリカが多く含
まれることが判明している。Further, the shape of the flake-like silica which has the effect of improving the fluidity of the resin as a filler material has a thickness of 0.1.
10 μm and maximum width of 100 μm or less. At the stage of the siliceous foam produced by the various methods described above, if the average diameter of the foam is in the range of 0.05 to 0.5 mm, the crushed powder will have the shape of a foil piece having such a shape. It has been found to be high in silica.
【0014】このようにして得られた箔片状シリカを含
むシリカ粉末をフィラー材として樹脂に混練して封止用
樹脂コンパウンドを調製する。この工程は公知の技術を
適用できる。また、得られた樹脂コンパウンドの特性も
公知の手法で評価できる。The silica powder containing the flaky silica thus obtained is kneaded with a resin as a filler material to prepare a sealing resin compound. A known technique can be applied to this step. The properties of the obtained resin compound can also be evaluated by a known method.
【0015】[0015]
【実施例】以下、本発明の実施例を説明する。 実施例1EXAMPLES Examples of the present invention will be described below. Example 1
【0016】エタノールで2倍に希釈したエチルシリケ
ートに、塩酸でpH1に調整した等量の水をエタノール
で2倍に希釈して添加し、シリカゾルを調製した。これ
を80℃に保持してゲル化させ、さらに150℃で乾燥
させて多孔質の乾燥ゲルを調製した。これを酸化雰囲気
中で1000℃までゆっくり加熱して有機物を除去し、
ついで1400℃まで1時間で昇温し、そのまま1時間
保持した後に炉から取り出して冷却した。得られたシリ
カ発泡体は0.1〜3mm径の泡からなっていた。これ
を石英ガラス製のボールミルで粉砕し、平均粒径25μ
mの粉末とした。この粉末を走査電子顕微鏡で調べたと
ころ、約20%が偏平な形状を有し、その厚さは0.1
〜10μmであった。A silica sol was prepared by adding an equal amount of water adjusted to pH 1 with hydrochloric acid to ethyl silicate diluted 2-fold with ethanol, diluted 2-fold with ethanol. This was kept at 80 ° C. for gelation and further dried at 150 ° C. to prepare a porous dry gel. This is slowly heated to 1000 ° C. in an oxidizing atmosphere to remove organic matter,
Then, the temperature was raised to 1400 ° C. in 1 hour, kept for 1 hour, taken out of the furnace and cooled. The silica foam obtained consisted of bubbles having a diameter of 0.1 to 3 mm. This is crushed with a ball mill made of quartz glass, and the average particle size is 25μ.
m powder. When the powder was examined with a scanning electron microscope, about 20% had a flat shape and its thickness was 0.1.
It was -10 μm.
【0017】この粉末をフィラー材として70重量%と
なるように、クレゾール−ノボラック型エポキシ樹脂に
配合し、ホットローラを用いて混練した後、タブレット
状及び棒状に加工した。得られたコンパウンドについて
フローテスタで流動性を測定した。また、棒状試料につ
いて曲げ強度を測定し、機械的強度を評価した。This powder was mixed as a filler material in a cresol-novolak type epoxy resin so as to be 70% by weight, kneaded using a hot roller, and processed into tablets and rods. The fluidity of the obtained compound was measured with a flow tester. Moreover, the bending strength of the rod-shaped sample was measured to evaluate the mechanical strength.
【0018】比較のために、レーザ回折法による粒度分
布測定機による評価で、同じ平均粒径を示し、粒度分布
が非常によく一致した破砕粉シリカを用意した。これを
フィラー材として用い、前記と同じ方法で樹脂と混練し
てコンパウンドを調製し、流動性及び強度を測定した。For comparison, crushed silica powder was prepared which showed the same average particle size as evaluated by a particle size distribution analyzer by a laser diffraction method and had a very good particle size distribution. This was used as a filler material and kneaded with a resin in the same manner as above to prepare a compound, and its fluidity and strength were measured.
【0019】データの比較を容易にするために、破砕粉
の場合の特性を1として、本実施例のフィラー材の特性
の比を求めた結果、流動性は1.5〜2、強度は1.5
となっった。このことから、本実施例のフィラー材は樹
脂の流動性と機械的強度を向上させる効果があることが
わかる。 実施例2In order to facilitate the comparison of the data, the property of the crushed powder was set to 1, and the ratio of the properties of the filler material of this example was determined. As a result, the fluidity was 1.5 to 2 and the strength was 1. .5
Became. From this, it is understood that the filler material of this example has an effect of improving the fluidity and mechanical strength of the resin. Example 2
【0020】エチルシリケートを60℃に加熱しなが
ら、等量の水をアルコールで2倍に希釈して酢酸酸性下
で添加した後、過剰のアルコールを蒸発させて体積で1
/3に濃縮した。冷却後、1%の濃度になるようにテト
ラデシルアルコールとテトラデシルアミンを溶解させ
た。この溶液1に対して1/2の水を加え、強く撹拌し
て均質な発泡体とし、アンモニアガスでこの発泡体を固
化させた。この発泡体を酸素雰囲気中で1000℃まで
6時間で昇温し、更に4時間かけて1300℃まで加熱
し、1時間保持した。得られた発泡体は、約1mmのよ
く径の揃った泡からなっていた。これを石英ガラスボー
ルミルで軽く粉砕した。この破砕粉を水中に投入して沈
降速度の違いを利用して箔片状のものを選別した。得ら
れた箔片状シリカを走査型電子顕微鏡により観察したと
ころ、厚さが0.1〜5μm、最大幅が0.1mm以下
であった。While heating the ethyl silicate to 60 ° C., an equal amount of water was diluted 2-fold with alcohol and added under acidity of acetic acid, and then excess alcohol was evaporated to reach 1 vol.
Concentrated to / 3. After cooling, tetradecyl alcohol and tetradecylamine were dissolved to have a concentration of 1%. 1/2 of water was added to this solution 1 and stirred vigorously to form a homogeneous foam, and the foam was solidified with ammonia gas. This foam was heated to 1000 ° C. in an oxygen atmosphere for 6 hours, further heated to 1300 ° C. over 4 hours, and held for 1 hour. The resulting foam consisted of well-sized bubbles of about 1 mm. This was lightly crushed with a quartz glass ball mill. The crushed powder was put into water and foil pieces were selected using the difference in sedimentation speed. When the obtained flaky silica was observed with a scanning electron microscope, the thickness was 0.1 to 5 μm and the maximum width was 0.1 mm or less.
【0021】得られた箔片状シリカと実施例1で比較の
ために用いた破砕粉シリカとを表1に示す種々の割合で
混合し、実施例1と同様な方法で樹脂と混練してコンパ
ウンドを調製し、実施例1と同様に流動性及び強度を評
価した。この結果を表1に示す。表1から、箔片状シリ
カが樹脂の流動性と機械的強度の向上に効果的であるこ
とがわかる。The foil-like silica obtained and the crushed powder silica used for comparison in Example 1 were mixed at various ratios shown in Table 1, and kneaded with the resin in the same manner as in Example 1. A compound was prepared and the fluidity and strength were evaluated in the same manner as in Example 1. The results are shown in Table 1. It can be seen from Table 1 that the foil-like silica is effective in improving the fluidity and mechanical strength of the resin.
【0022】[0022]
【表1】 実施例3[Table 1] Example 3
【0023】平均粒径0.1μm以下のシリカ粉(商品
名エアロジル130)を水に分散させて25%の溶液を
調製し、この溶液に1%のステアリン酸アンモニウム及
び0.5%の塩化アンモニウムと重炭酸アンモニウムを
加えた。この溶液を撹拌しながら加熱して発泡、固化さ
せた。得られた発泡体を乾燥した後、実施例2と同様な
方法で加熱、焼成した、更に粉砕した。この粉末の平均
粒径は40μmであり、厚さ1〜10μmの箔片状シリ
カが約60%含まれていた。これを実施例1と同様な方
法で樹脂に添加してその特性を評価したところ、同様な
粒度分布を持つ破砕粉をフィラー材に用いた場合と比較
して、流動性で約3倍、強度で約2倍の特性向上が認め
られた。A 25% solution was prepared by dispersing silica powder (trade name Aerosil 130) having an average particle size of 0.1 μm or less in water, and 1% ammonium stearate and 0.5% ammonium chloride were added to this solution. And ammonium bicarbonate were added. This solution was heated with stirring to foam and solidify. The obtained foam was dried, then heated and baked in the same manner as in Example 2, and further pulverized. This powder had an average particle size of 40 μm, and contained about 60% of foil flaky silica having a thickness of 1 to 10 μm. When this was added to the resin in the same manner as in Example 1 and the characteristics thereof were evaluated, the flowability was about three times that of the case where crushed powder having the same particle size distribution was used as the filler material, and the strength was increased. It was confirmed that the characteristics were improved about twice.
【0024】[0024]
【発明の効果】以上詳述したように本発明の方法を用い
れば、樹脂の流動性及び機械的強度の向上に効果がある
箔片状シリカからなる半導体封止樹脂用フィラー材を簡
便で安価に製造できる。As described in detail above, by using the method of the present invention, a filler material for semiconductor encapsulating resin, which is made of foil-like silica and is effective in improving the fluidity and mechanical strength of the resin, is simple and inexpensive. Can be manufactured.
Claims (1)
泡体を破砕することを特徴とする半導体封止樹脂用フィ
ラー材の製造方法。Claim: What is claimed is: 1. A method for producing a filler material for a semiconductor encapsulating resin, comprising forming a siliceous foam and then crushing the foam.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP19431391A JPH0531721A (en) | 1991-08-02 | 1991-08-02 | Preparation of filler material for semiconductor sealing resin |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP19431391A JPH0531721A (en) | 1991-08-02 | 1991-08-02 | Preparation of filler material for semiconductor sealing resin |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH0531721A true JPH0531721A (en) | 1993-02-09 |
Family
ID=16322531
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP19431391A Pending JPH0531721A (en) | 1991-08-02 | 1991-08-02 | Preparation of filler material for semiconductor sealing resin |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH0531721A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5727329A (en) * | 1995-07-03 | 1998-03-17 | Ushikata Mfg. Co., Ltd. | Device for measuring a figure |
US5748502A (en) * | 1994-03-07 | 1998-05-05 | Ushikata Mfg. Co., Ltd. | Apparatus for measuring a figure having a calibration mode and method for calibrating a measuring apparatus |
US5875556A (en) * | 1995-12-07 | 1999-03-02 | Akio Kubo | Apparatus and method for measuring a figure |
-
1991
- 1991-08-02 JP JP19431391A patent/JPH0531721A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5748502A (en) * | 1994-03-07 | 1998-05-05 | Ushikata Mfg. Co., Ltd. | Apparatus for measuring a figure having a calibration mode and method for calibrating a measuring apparatus |
US5727329A (en) * | 1995-07-03 | 1998-03-17 | Ushikata Mfg. Co., Ltd. | Device for measuring a figure |
US5875556A (en) * | 1995-12-07 | 1999-03-02 | Akio Kubo | Apparatus and method for measuring a figure |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP3299340B1 (en) | Method for preparing spherical silica aerogel granules and spherical silica aerogel granules prepared thereby | |
KR102210029B1 (en) | Method preparing silicon carbide particle and the silicon carbide particle prepared the same | |
CN114539809A (en) | Surface-modified silicon micropowder and preparation method thereof | |
JP3413873B2 (en) | Synthetic quartz glass powder | |
Masuda et al. | Particle size distribution of spherical silica gel produced by sol-gel method | |
CN112358674A (en) | Core-shell nano silicon oxide @ zirconium oxide particle-polypropylene maleic anhydride grafted polypropylene composite material and preparation method thereof | |
JPH0531721A (en) | Preparation of filler material for semiconductor sealing resin | |
JP2003201111A (en) | Low thickening fumed silica and its slurry | |
RU2141928C1 (en) | Method of preparing monolithic quartz glass using sol-gel process | |
CA1317696C (en) | Encapsulating compositions containing ultra-pure, fused-silica fillers | |
CN115417415B (en) | Silicon dioxide for high-transparency silicon rubber and preparation method and application thereof | |
JP2007211252A (en) | Semiconductor encapsulating epoxy resin composition using fly ash powder and semiconductor device using the same | |
JPS6296567A (en) | Semiconductor sealing resin composition | |
JP6129216B2 (en) | Method for producing and processing pasty SiO2 material and use thereof | |
KR102282500B1 (en) | Nanocomposite insulation materials with enhanced thermal conductivity by dispersion of inorganic nanoparticles and their manufacturing method | |
CN115818654B (en) | Thick wall SiO2Preparation method of hollow microspheres | |
JPH0959014A (en) | Hygroscopic silica particle and its production | |
JP2000160205A (en) | Rare earth-base magnetic powder and its surface treatment | |
CN110465671B (en) | Preparation method of flaky silver powder | |
JP2018203601A (en) | Method for producing phenyl alkoxysilane-treated silica | |
JP4040715B2 (en) | Filler and semiconductor sealing resin composition | |
JP2915224B2 (en) | Method for producing inorganic oxide particles | |
JP2649054B2 (en) | Particulate inorganic composite and method for producing the same | |
CN108102137B (en) | Nanopal composition, method of preparing the same, and resin composition comprising the same | |
CN115959912A (en) | Preparation process of micro-nano cross-scale ceramic slurry |