JPH11269302A - Filler for improving thermal conductivity of resin product and its production - Google Patents

Filler for improving thermal conductivity of resin product and its production

Info

Publication number
JPH11269302A
JPH11269302A JP10095269A JP9526998A JPH11269302A JP H11269302 A JPH11269302 A JP H11269302A JP 10095269 A JP10095269 A JP 10095269A JP 9526998 A JP9526998 A JP 9526998A JP H11269302 A JPH11269302 A JP H11269302A
Authority
JP
Japan
Prior art keywords
filler
thermal conductivity
aln
resin product
improving thermal
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
JP10095269A
Other languages
Japanese (ja)
Inventor
Takeo Nishimura
西村威夫
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.)
NISHIMURA TOGYO KK
Original Assignee
NISHIMURA TOGYO KK
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 NISHIMURA TOGYO KK filed Critical NISHIMURA TOGYO KK
Priority to JP10095269A priority Critical patent/JPH11269302A/en
Publication of JPH11269302A publication Critical patent/JPH11269302A/en
Pending legal-status Critical Current

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  • Ceramic Products (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

PROBLEM TO BE SOLVED: To obtain a filler useful for improving thermal conductivity of a resin product such as a semiconductor sealing resin. SOLUTION: This filler for improving thermal conductivity of a resin product comprises AlN spherical sintered body having 10-200 μm average particle diameter. The filler is obtained by blending AlN powder with a molding adjuvant, wet-blending the obtained mixture, granulating the wet-blended materials by a spray drier to provide granules, mixing BN powder with the obtained granules and firing the obtained mixture in nitrogen stream at >=1,500 deg.C.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、半導体封止樹脂
用、放熱シートの放熱性接着用及び放熱基板用等の樹脂
製品の熱伝導性向上用充填剤に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a filler for improving the thermal conductivity of a resin product such as a resin for a semiconductor encapsulation resin, a heat radiation sheet for heat radiation bonding, and a heat radiation substrate.

【0002】[0002]

【従来の技術】従来の半導体封止樹脂用の充填剤(フィ
ラー)としては、主に溶融シリカが用いられてきたが、
これは熱伝導性に劣るため、所望の効果を得ることがで
きなかった。しかし、近年発熱性電子部品の高密度化に
より、これら部品の放熱性に関する要求が高まりを見せ
てきた。
2. Description of the Related Art Fused silica has been mainly used as a conventional filler for semiconductor encapsulation resins.
This was inferior in thermal conductivity, and could not achieve the desired effect. However, in recent years, due to the increase in the density of heat-generating electronic components, demands for heat radiation of these components have been increasing.

【0003】[0003]

【発明が解決しようとする課題】本発明は、かかる要求
に対応し、半導体封止樹脂等の樹脂製品の熱伝導性を向
上するのに有用な充填剤を提供することを課題とする。
SUMMARY OF THE INVENTION It is an object of the present invention to provide a filler which meets such a demand and which is useful for improving the thermal conductivity of a resin product such as a semiconductor sealing resin.

【0004】[0004]

【課題を解決するための手段】本発明では、AlN(窒
化アルミニウム)の具備する諸特性、特に熱伝導率に着
目し、これを球状焼結体とすることによって、上記課題
を解決する方法を見いだした。
The present invention focuses on the characteristics of AlN (aluminum nitride), particularly on the thermal conductivity, and provides a method for solving the above-mentioned problem by forming it into a spherical sintered body. I found it.

【0005】即ち、本発明では、平均粒径が10〜20
0μmであるAlN球状焼結体を、樹脂製品の充填剤と
する。
That is, in the present invention, the average particle size is 10 to 20.
The AlN spherical sintered body of 0 μm is used as a filler for resin products.

【0006】放熱性を要求される各電子部品の基材、例
えば放熱シートは、充填剤の熱伝導率が高い程、また充
填剤の添加量が多い程、熱伝導性が大きくなることか
ら、充填剤として要求される性質は、高熱伝導率を有す
ること、流動性がよく、樹脂等に多量に含有せしめるこ
とができることが挙げられるが、本発明のAlNの焼結
体は、高熱伝導率を有し、かつ球状であることから、流
動性に富み、他の樹脂へ大量に添加することが可能とな
り、その結果、前述の如き要求をいずれも満たすものと
なる。なお、AlN球状焼結体の平均粒径は10〜20
0μm程度であればよいが、充填密度を向上するために
は、50〜150μm程度であるのが特に好ましい。こ
の粒径が大きくなり過ぎると流動性が低下して、樹脂に
高い含有率で分散し難くなる。
[0006] The base material of each electronic component that requires heat dissipation, for example, a heat dissipation sheet, has a higher thermal conductivity as the thermal conductivity of the filler is higher and the amount of the filler added is greater. The properties required as a filler include high thermal conductivity, good fluidity, and the ability to be contained in a large amount in a resin or the like.AlN sintered bodies of the present invention have high thermal conductivity. Since it has and is spherical, it is rich in fluidity and can be added to other resins in a large amount. As a result, all of the above requirements are satisfied. The average particle size of the AlN spherical sintered body is 10 to 20.
It may be about 0 μm, but in order to improve the packing density, it is particularly preferably about 50 to 150 μm. If the particle size is too large, the fluidity is reduced, and it is difficult to disperse the resin at a high content.

【0007】かかるAlN球状焼結体は、AlN粉末に
成形助剤を配合し、湿式混合の後、スプレードライヤー
を用いて造粒して得た顆粒にBN粉末を混合し、該混合
物を窒素気流中、1500℃以上の高温で焼成すること
によって製造できる。
[0007] Such an AlN spherical sintered body is obtained by mixing a molding aid with AlN powder, wet-mixing, granulating using a spray drier, and mixing BN powder with the obtained granule, and subjecting the mixture to a nitrogen stream. And by firing at a high temperature of 1500 ° C. or more.

【0008】例えば、AlN粉末単独又はこれに焼結助
剤(Y2 3 ,CaO他)を添加したものに、成形助剤
を添加し、湿式混合した後、該混合物をスプレードライ
ヤーにて造粒し、得られた造粒粉末100重量部にBN
(窒化硼素)粉末1〜30重量部を混合し、窒素気流中
で1700℃以上1950℃未満で焼成すればよい。な
お、成形助剤としては、メチルセルロース系樹脂やポリ
ビニルブチラール等の樹脂類をAlN粉末に対して1〜
10重量%程度添加するのが好ましい。
For example, a molding aid is added to AlN powder alone or a mixture of a sintering aid (Y 2 O 3 , CaO, etc.) and wet-mixed, and the mixture is formed by a spray drier. BN is added to 100 parts by weight of the obtained granulated powder.
(Boron nitride) 1 to 30 parts by weight of powder may be mixed and fired at 1700 ° C. or higher and lower than 1950 ° C. in a nitrogen stream. As a molding aid, a resin such as a methylcellulose-based resin or polyvinyl butyral is added to the AlN powder in an amount of 1 to 10.
It is preferable to add about 10% by weight.

【0009】BNの添加の理由は、AlN造粒粉末が焼
成時に互いに焼付いてしまうことを防止するためであ
る。BNは高温で安定で、しかもAlNと反応性がない
ため、有用である。なお、造粒の条件を変えることによ
り造粒粉末の粒径粒度分布を制御することができる。
[0009] The reason for adding BN is to prevent the AlN granulated powder from burning together during firing. BN is useful because it is stable at high temperatures and has no reactivity with AlN. The particle size distribution of the granulated powder can be controlled by changing the granulation conditions.

【0010】[0010]

【発明の実施の形態】次に、本発明を実施例に従って更
に詳しく説明するが、実施例において部及び%とあるの
は、特に断らない限り、重量部及び重量%を示す。 〔実施例1〕平均粒径0.8μm、酸素含有量0.6
%、純度98%のAlN粉末97部に平均粒径1.0μ
mのY2 3 粉末3部を添加した。この混合粉末100
部にエタノール55部、分散剤1部及びポリビニールブ
チラール1.5部を添加し、24時間ポットミルで混合
した。次いで、このようにした作成したスラリーを、回
転円盤型のスプレードライヤーで造粒乾燥した。その
後、このAlN造粒物100部にBN10部を混合し
て、AlN坩堝に充填し、常圧下、窒素気流中1800
℃で4時間焼成した。この焼成物をエタノール中で超音
波分散後、濾過してBNを分離除去した後、乾燥して、
AlN球状焼結体を得た。このAlN球状焼結体の平均
粒径は103μmであり、熱伝導率は170〜220W
/mkであった。この球状焼結体をノボラックエポキシ
樹脂に充填剤として配合した例を、従来例(充填剤とし
て溶融シリカを使用したもの)と比較して、次表に示
す。
BEST MODE FOR CARRYING OUT THE INVENTION Next, the present invention will be described in more detail with reference to Examples. In the Examples, "parts" and "%" indicate "parts by weight" and "% by weight" unless otherwise specified. Example 1 Average particle size 0.8 μm, oxygen content 0.6
%, 97 parts of 98% pure AlN powder, average particle size 1.0μ
m 2 of Y 2 O 3 powder were added. This mixed powder 100
55 parts of ethanol, 1 part of a dispersant and 1.5 parts of polyvinyl butyral were added to the mixture, and mixed with a pot mill for 24 hours. Next, the slurry thus prepared was granulated and dried with a rotating disk type spray drier. Thereafter, 100 parts of the AlN granules are mixed with 10 parts of BN, and the mixture is filled in an AlN crucible, and is placed in a nitrogen stream at normal pressure for 1800 minutes.
Calcination was performed at 4 ° C. for 4 hours. This baked product is ultrasonically dispersed in ethanol, and then filtered to separate and remove BN, and then dried,
An AlN spherical sintered body was obtained. This AlN spherical sintered body has an average particle size of 103 μm and a thermal conductivity of 170 to 220 W.
/ Mk. An example in which this spherical sintered body is blended as a filler with a novolak epoxy resin is shown in the following table in comparison with a conventional example (using fused silica as a filler).

【0011】[0011]

【表1】 [Table 1]

【0012】〔実施例2〕平均粒径0.8μm酸素含有
量0.6%、純度98%のAlN粉末100部にエタノ
ール50部、分散剤1部、ポリビニルブチラール1.5
部を添加し、24時間ポットミルで混合した。
Example 2 100 parts of AlN powder having an average particle diameter of 0.8 μm, an oxygen content of 0.6% and a purity of 98% were mixed with 50 parts of ethanol, 1 part of a dispersant, and 1.5 parts of polyvinyl butyral.
Was added and mixed on a pot mill for 24 hours.

【0013】混合後、このスラリーを回転円盤型のスプ
レードライヤーで造粒し、乾燥し、得られたAlN造粒
物100部をBN10倍と混合して、AlN坩堝に充填
し、常圧下、窒素気流中1800℃で4時間焼成した。
この焼成物をエタノール中で超音波分散させた後、濾過
してBNを分散除去した後、乾燥して、AlN球状焼結
体を得た。このAlN球状焼結体の平均粒径は88μm
であり、熱伝導率は50〜100W/mkであった。こ
の球状焼結体をビフェニルエポキシ樹脂に充填剤として
配合した例を、従来例(充填剤として溶融シリカを使用
したもの)と比較して、次表に示す。
After mixing, the slurry is granulated with a rotary disk type spray drier, dried, and 100 parts of the obtained AlN granules are mixed with 10 times of BN, filled into an AlN crucible, and filled with nitrogen under normal pressure. It was baked at 1800 ° C. for 4 hours in an air stream.
The fired product was ultrasonically dispersed in ethanol, filtered to remove BN, and dried to obtain an AlN spherical sintered body. The average particle size of this AlN spherical sintered body is 88 μm
And the thermal conductivity was 50 to 100 W / mk. An example in which this spherical sintered body is blended as a filler with biphenyl epoxy resin is shown in the following table in comparison with a conventional example (using fused silica as a filler).

【0014】[0014]

【表2】 [Table 2]

【0015】[0015]

【発明の効果】本発明の充填剤は、球状焼結体であるた
め、高密度で樹脂製品に充填でき、しかも熱伝導率に非
常に優れるため、樹脂製品の熱伝導性を著しく向上する
ことができ、また放熱性をも著しく改善する。
The filler of the present invention, which is a spherical sintered body, can be filled in a resin product at a high density and has a very high thermal conductivity, so that the thermal conductivity of the resin product can be significantly improved. And also significantly improves the heat dissipation.

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】 平均粒径が10〜200μmであるAl
N球状焼結体からなることを特徴とする樹脂製品の熱伝
導性向上用充填剤。
1. Al having an average particle size of 10 to 200 μm.
A filler for improving thermal conductivity of a resin product, comprising a N-sphere sintered body.
【請求項2】 AlN粉末に成形助剤を配合し、湿式混
合の後、スプレードライヤーを用いて造粒して得た顆粒
にBN粉末を混合し、該混合物を窒素気流中、1500
℃以上の高温で焼成することを特徴とする樹脂製品の熱
伝導性向上用充填剤の製造方法。
2. An AlN powder is mixed with a molding aid, and after wet mixing, BN powder is mixed with granules obtained by granulation using a spray drier, and the mixture is mixed in a nitrogen stream at 1500
A method for producing a filler for improving thermal conductivity of a resin product, wherein the filler is fired at a high temperature of not less than ° C.
JP10095269A 1998-03-23 1998-03-23 Filler for improving thermal conductivity of resin product and its production Pending JPH11269302A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP10095269A JPH11269302A (en) 1998-03-23 1998-03-23 Filler for improving thermal conductivity of resin product and its production

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP10095269A JPH11269302A (en) 1998-03-23 1998-03-23 Filler for improving thermal conductivity of resin product and its production

Publications (1)

Publication Number Publication Date
JPH11269302A true JPH11269302A (en) 1999-10-05

Family

ID=14133061

Family Applications (1)

Application Number Title Priority Date Filing Date
JP10095269A Pending JPH11269302A (en) 1998-03-23 1998-03-23 Filler for improving thermal conductivity of resin product and its production

Country Status (1)

Country Link
JP (1) JPH11269302A (en)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006206393A (en) * 2005-01-28 2006-08-10 Mitsui Chemicals Inc Spherical aluminum nitride sintered powder, its manufacturing method, and its use
JP2006273948A (en) * 2005-03-28 2006-10-12 Mitsui Chemicals Inc Thermally-conductive resin composition and use of the same
JP2006273969A (en) * 2005-03-29 2006-10-12 Mitsui Chemicals Inc Curable resin composition and its use
JP2010059055A (en) * 2001-08-07 2010-03-18 Saint-Gobain Ceramics & Plastics Inc HIGH-SOLID hBN SLURRY, hBN PASTE, SPHERICAL hBN POWDER, AND METHODS OF MAKING AND USING THEM
US9073755B2 (en) 2010-09-03 2015-07-07 Tokuyama Corporation Spherical aluminum nitride powder
US9090469B2 (en) 2010-09-28 2015-07-28 Tokuyama Corporation Method of producing a spherical aluminum nitride powder
US9199848B2 (en) 2010-01-29 2015-12-01 Tokuyama Corporation Process for producing spherical aluminum nitride powder and spherical aluminum nitride powder produced by the same process
US10427939B2 (en) 2017-08-11 2019-10-01 Lg Chem, Ltd. Method for producing spherical aluminum nitride power
WO2019189182A1 (en) * 2018-03-29 2019-10-03 Jnc株式会社 Thermally conductive composite filler, heat-dissipating resin composition containing same, and heat-dissipating grease and heat-dissipating member comprising heat-dissipating resin composition
EP3730455A4 (en) * 2017-12-21 2021-08-04 Showa Denko K.K. Glass-coated aluminum nitride particles, method for producing same, and heat dissipating resin composition containing same

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010059055A (en) * 2001-08-07 2010-03-18 Saint-Gobain Ceramics & Plastics Inc HIGH-SOLID hBN SLURRY, hBN PASTE, SPHERICAL hBN POWDER, AND METHODS OF MAKING AND USING THEM
JP2006206393A (en) * 2005-01-28 2006-08-10 Mitsui Chemicals Inc Spherical aluminum nitride sintered powder, its manufacturing method, and its use
JP2006273948A (en) * 2005-03-28 2006-10-12 Mitsui Chemicals Inc Thermally-conductive resin composition and use of the same
JP2006273969A (en) * 2005-03-29 2006-10-12 Mitsui Chemicals Inc Curable resin composition and its use
US9199848B2 (en) 2010-01-29 2015-12-01 Tokuyama Corporation Process for producing spherical aluminum nitride powder and spherical aluminum nitride powder produced by the same process
US9073755B2 (en) 2010-09-03 2015-07-07 Tokuyama Corporation Spherical aluminum nitride powder
US9090469B2 (en) 2010-09-28 2015-07-28 Tokuyama Corporation Method of producing a spherical aluminum nitride powder
US10427939B2 (en) 2017-08-11 2019-10-01 Lg Chem, Ltd. Method for producing spherical aluminum nitride power
EP3730455A4 (en) * 2017-12-21 2021-08-04 Showa Denko K.K. Glass-coated aluminum nitride particles, method for producing same, and heat dissipating resin composition containing same
US11254572B2 (en) 2017-12-21 2022-02-22 Showa Denko K.K. Glass-coated aluminum nitride particles, method for producing same, and heat dissipating resin composition containing same
WO2019189182A1 (en) * 2018-03-29 2019-10-03 Jnc株式会社 Thermally conductive composite filler, heat-dissipating resin composition containing same, and heat-dissipating grease and heat-dissipating member comprising heat-dissipating resin composition

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