JPS60186479A - Manufacture of high heat conductivity aluminum nitride sintered body - Google Patents

Manufacture of high heat conductivity aluminum nitride sintered body

Info

Publication number
JPS60186479A
JPS60186479A JP59041908A JP4190884A JPS60186479A JP S60186479 A JPS60186479 A JP S60186479A JP 59041908 A JP59041908 A JP 59041908A JP 4190884 A JP4190884 A JP 4190884A JP S60186479 A JPS60186479 A JP S60186479A
Authority
JP
Japan
Prior art keywords
aluminum nitride
sintered body
carbon
nitride sintered
manufacture
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.)
Granted
Application number
JP59041908A
Other languages
Japanese (ja)
Other versions
JPH0567593B2 (en
Inventor
安斎 和雄
加曽利 光男
高野 武士
和夫 篠崎
柘植 章彦
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.)
Toshiba Corp
Original Assignee
Toshiba Corp
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 Toshiba Corp filed Critical Toshiba Corp
Priority to JP59041908A priority Critical patent/JPS60186479A/en
Publication of JPS60186479A publication Critical patent/JPS60186479A/en
Publication of JPH0567593B2 publication Critical patent/JPH0567593B2/ja
Granted legal-status Critical Current

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Abstract

(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。
(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

【発明の詳細な説明】 し発明の技術分野〕 本発明は高熱伝導性を具備した窒化アルミニウム焼結体
の製造方法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION Technical Field of the Invention The present invention relates to a method for manufacturing an aluminum nitride sintered body having high thermal conductivity.

〔発明の技術的背景とその問題点〕[Technical background of the invention and its problems]

窒化アルミニウムは絶縁性でありかつ熱伝導性に優れた
セラミックスとして知られている。
Aluminum nitride is known as a ceramic that is insulating and has excellent thermal conductivity.

しかしながら窒化アルミニウム焼結体の原料の窒化アル
ミニウム粉末には通常は不純物として酸素をはじめとす
る不純物が含まれている。このため原料粉末をできるだ
け不純物の混入を防いだ工程で焼結、例えば1600℃
〜1900℃における加圧焼結で行なっても得られた焼
結体の熱伝導率は40〜45 w/Im−K程度の値に
止まってしまう問題があり、さらに高熱伝導化の要求が
あった。
However, aluminum nitride powder, which is a raw material for aluminum nitride sintered bodies, usually contains impurities such as oxygen. For this reason, the raw material powder is sintered in a process that prevents the contamination of impurities as much as possible, for example at 1600℃.
Even if pressure sintering is performed at ~1900°C, there is a problem that the thermal conductivity of the obtained sintered body remains at a value of about 40 to 45 w/Im-K, and there is a demand for higher thermal conductivity. Ta.

〔発明の目的〕[Purpose of the invention]

本発明は上述の問題を改善し、熱伝導性に優れた窒化ア
ルミニウム焼結体の製造方法を提供することを目的とし
ている。
The present invention aims to improve the above-mentioned problems and provide a method for producing an aluminum nitride sintered body with excellent thermal conductivity.

〔発明の概要〕[Summary of the invention]

本発明者は上述の目的を達成するためには平均粒径3岬
以下の窒化アルミニウム原料粉末に0.05〜2重量%
の炭素ないしは分解して同量の炭素を形成する化合物を
添加混合した粉末を加圧焼結することが極めて有効であ
ることを見い出した。
In order to achieve the above-mentioned object, the present inventors added 0.05 to 2% by weight of aluminum nitride raw material powder with an average particle size of 3 or less.
It has been found that it is extremely effective to pressure sinter powder mixed with carbon or a compound that decomposes to form the same amount of carbon.

焼結時の圧力は高い方が焼結体の緻密化、熱伝導率改善
及び焼結時に用いられる容器の強度を瑚慮して実際上5
0〜600ψ−の範囲が好ましい。
In practice, the higher the pressure during sintering, the higher the densification of the sintered body, the improvement of thermal conductivity, and the strength of the container used during sintering.
The range of 0 to 600 ψ- is preferable.

焼結時の温度は1700℃未満では焼結体が緻密化せず
、逆に2100℃を超えると高温では窒化アルミニウム
の蒸発が顕著となり良好な焼結体が得られないので、1
700℃−2100℃の範囲とする。添加される炭素の
量が過剰であると焼結体中に残存して熱伝導度き下げる
原因ともなるので0.05〜2*量チの範囲とする必要
がある。又A/N粉末は3μmを超えると緻密性、熱伝
導性が低下する為3μm以下とする。
If the temperature during sintering is less than 1,700°C, the sintered body will not become dense, and if it exceeds 2,100°C, the evaporation of aluminum nitride will be noticeable and a good sintered body will not be obtained.
The temperature range is 700°C to 2100°C. If the amount of carbon added is excessive, it may remain in the sintered body and cause a decrease in thermal conductivity, so it is necessary to keep the amount in the range of 0.05 to 2*. Further, if the A/N powder exceeds 3 μm, the density and thermal conductivity will decrease, so the thickness should be 3 μm or less.

〔発明の効果〕〔Effect of the invention〕

本発明になる窒化アルミニウム焼結体は窒化アルミニウ
ム粉末に所定量の炭素ないしは分解して炭素となる化合
物を添加混合した粉末を焼結することによる簡単な操作
で焼結体の熱伝導性を改善することができる。また添加
物が炭素のみであり、かつ添加された炭素が窒化アルミ
ニウム粉末に含せれる酸素を除去するだめに焼結後の焼
結体は非常Iこ高純度となり高純度であることを要求さ
れるアルミ溶融用ルツボなどへの利用も可能であるなど
の効果が期待できる。
The aluminum nitride sintered body of the present invention improves the thermal conductivity of the sintered body through a simple operation by sintering aluminum nitride powder with a predetermined amount of carbon or a compound that decomposes into carbon. can do. In addition, since the only additive is carbon, and the added carbon removes oxygen contained in the aluminum nitride powder, the sintered body after sintering has extremely high purity, which is required. It can also be used in aluminum melting crucibles, etc., and other effects can be expected.

し発明の実施例〕 以下実施例によって詳細に説明する。Examples of the invention] This will be explained in detail below using examples.

実施例1 平均粒径3μm以下の窒化アルミニウム粉末100y1
こ無定形炭素(粒径1μm以下) 0.IPを添加しボ
ールミルで湿式混合を4時間行ない乾燥後金型プレスを
用い3QQKy’m’の加圧成形を行ない約3Q7WX
30mX12Mの圧粉体を得た。
Example 1 Aluminum nitride powder 100y1 with an average particle size of 3 μm or less
This amorphous carbon (particle size 1 μm or less) 0. Add IP and wet mix in a ball mill for 4 hours. After drying, use a mold press to pressure mold 3QQKy'm' to approximately 3Q7WX.
A green compact of 30m×12M was obtained.

圧粉体をカーボン製モールド1こ入れ窒素ガス雰囲気下
で300に61,4’−1800℃−1時間の加圧焼結
を行なった。得られた焼結体から直径10調、厚さ4w
Rの円板を切り出しレーザーフラッシュ法にて熱伝導率
を測定したところ55w/m−にの値が得られた。
The green compact was placed in a carbon mold and subjected to pressure sintering at 300° C. and 1800° C. for 1 hour in a nitrogen gas atmosphere. The obtained sintered body has a diameter of 10 mm and a thickness of 4 mm.
When a circular plate of R was cut out and its thermal conductivity was measured by the laser flash method, a value of 55 w/m was obtained.

焼結体の密度は3.26V(ldであった。The density of the sintered body was 3.26V (ld).

実施例2−9 実施例1と同じ窒化アルミニウム粉末と炭素を用いて炭
素濃度、焼結温度−圧力を変えて得られた窒化アルミニ
ウム焼結体の熱伝導率測定結果を第1表fこ示した。
Example 2-9 Table 1 shows the thermal conductivity measurement results of aluminum nitride sintered bodies obtained using the same aluminum nitride powder and carbon as in Example 1 but varying the carbon concentration and sintering temperature and pressure. Ta.

第1表 実施例工1 平均粒径2μmの以下へ窒化アルミニウム粉末100)
に炭素源として砂糖1ノを添加しボールミルで乾式混合
を24時間行なった。この混合粉末を金型プレスを用い
て3QQvdの加圧成形を行ない約30m x 3Qm
 x 12mの圧粉体を得た。圧粉体をカーボン製モー
ルドに入れ窒素ガス雰囲気化で300に9/ad−18
00℃−30分間の加圧焼結を行なった。得られた焼結
体から直径IQm、厚さ4mの円板を切り出しレーザー
フラッシュ法lこて熱伝導率を測定したところ55 w
/mKの値が得られた。焼結体の密度は3.26Pβで
あった。
Table 1 Example Work 1 Aluminum nitride powder with an average particle size of 2 μm or less 100)
One portion of sugar was added as a carbon source, and dry mixing was carried out in a ball mill for 24 hours. This mixed powder was pressure-molded to a size of 3QQvd using a mold press, approximately 30m x 3Qm.
A green compact of x 12 m was obtained. The green compact was placed in a carbon mold and heated to 300 in a nitrogen gas atmosphere on 9/ad-18.
Pressure sintering was performed at 00°C for 30 minutes. A disk with a diameter of IQm and a thickness of 4m was cut out from the obtained sintered body and its thermal conductivity was measured using a laser flash method.It was 55w.
/mK values were obtained. The density of the sintered body was 3.26Pβ.

比較例1〜5 実施例1−9と同じ窒化アルミニウム粉末と炭素を用い
て炭素濃度、焼結温度−圧力を変えて得られた窒化アル
ミニウム焼結体の熱伝導率測定結果を第2表fこ示しだ
Comparative Examples 1 to 5 Thermal conductivity measurement results of aluminum nitride sintered bodies obtained by using the same aluminum nitride powder and carbon as in Examples 1-9 and changing the carbon concentration and sintering temperature and pressure are shown in Table 2 f. This is the proof.

代理人 弁理士 則 近 憲 佑 (ほか1名)第1頁
の続き 0発 明 者 柘 植 章 彦 川崎市幸区4所内 1向東芝町1 東京芝浦電気株式会社総合研究A^^
Agent: Kensuke Chika (and 1 other person) Continued from page 1 0 Inventor: Akihiko Tsuge Tokyo Shibaura Electric Co., Ltd. General Research A^^

Claims (2)

【特許請求の範囲】[Claims] (1) 平均粒径3IJrn以下のA/N粉末に炭素案
は分解して炭素になる化合物を炭素に換算して0.05
重量%以上2重量%以下添加した混合粉末を焼結して得
られることを特徴とする高熱伝導性窒化アルミニウム焼
結体の製造方法。
(1) The carbon plan is made into A/N powder with an average particle size of 3 IJrn or less, and the compound that decomposes to become carbon is 0.05 in terms of carbon.
A method for producing a highly thermally conductive aluminum nitride sintered body, characterized in that it is obtained by sintering a mixed powder containing 2% by weight or more and 2% by weight or less.
(2)焼結が1700℃〜2100℃の温度範囲でかつ
50険−以上の加圧焼結であることを特徴とする特許請
求の範囲第1項記載の高熱伝導性窒化アルミニウム焼結
体の製造方法。
(2) The highly thermally conductive aluminum nitride sintered body according to claim 1, wherein the sintering is performed at a temperature range of 1,700°C to 2,100°C and a pressure of 50°C or more. Production method.
JP59041908A 1984-03-07 1984-03-07 Manufacture of high heat conductivity aluminum nitride sintered body Granted JPS60186479A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP59041908A JPS60186479A (en) 1984-03-07 1984-03-07 Manufacture of high heat conductivity aluminum nitride sintered body

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59041908A JPS60186479A (en) 1984-03-07 1984-03-07 Manufacture of high heat conductivity aluminum nitride sintered body

Publications (2)

Publication Number Publication Date
JPS60186479A true JPS60186479A (en) 1985-09-21
JPH0567593B2 JPH0567593B2 (en) 1993-09-27

Family

ID=12621376

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59041908A Granted JPS60186479A (en) 1984-03-07 1984-03-07 Manufacture of high heat conductivity aluminum nitride sintered body

Country Status (1)

Country Link
JP (1) JPS60186479A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01242468A (en) * 1988-03-23 1989-09-27 Japan Steel Works Ltd:The Production of sintered body of aluminum nitride
JPH042663A (en) * 1990-04-17 1992-01-07 Sumitomo Electric Ind Ltd Colored aluminum nitride sintered material having high thermal conductivity and production thereof
WO2001047831A1 (en) * 1999-12-28 2001-07-05 Ibiden Co., Ltd. Carbon-containing aluminum nitride sintered compact, and ceramic substrate for use in apparatus for manufacturing and inspecting semiconductor
US6719931B2 (en) 2000-01-10 2004-04-13 Basf Aktiengesellschaft Low-viscosity, melamine-formaldehyde resin microcapsule dispersions with reduced formaldehyde content
US6900149B1 (en) 1999-09-06 2005-05-31 Ibiden Co., Ltd. Carbon-containing aluminum nitride sintered compact and ceramic substrate for use in equipment for manufacturing or inspecting semiconductor

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01242468A (en) * 1988-03-23 1989-09-27 Japan Steel Works Ltd:The Production of sintered body of aluminum nitride
JPH042663A (en) * 1990-04-17 1992-01-07 Sumitomo Electric Ind Ltd Colored aluminum nitride sintered material having high thermal conductivity and production thereof
US6900149B1 (en) 1999-09-06 2005-05-31 Ibiden Co., Ltd. Carbon-containing aluminum nitride sintered compact and ceramic substrate for use in equipment for manufacturing or inspecting semiconductor
US6964812B2 (en) 1999-09-06 2005-11-15 Ibiden Co., Ltd. Carbon-containing aluminum nitride sintered compact and ceramic substrate for use in equipment for manufacturing or inspecting semiconductor
US7015166B2 (en) 1999-09-06 2006-03-21 Ibiden Co., Ltd. Carbon-containing aluminum nitride sintered compact and ceramic substrate for use in equipment for manufacturing or inspecting semiconductor
WO2001047831A1 (en) * 1999-12-28 2001-07-05 Ibiden Co., Ltd. Carbon-containing aluminum nitride sintered compact, and ceramic substrate for use in apparatus for manufacturing and inspecting semiconductor
US6719931B2 (en) 2000-01-10 2004-04-13 Basf Aktiengesellschaft Low-viscosity, melamine-formaldehyde resin microcapsule dispersions with reduced formaldehyde content

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Publication number Publication date
JPH0567593B2 (en) 1993-09-27

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