JPH0637286B2 - Manufacturing method of aluminum nitride - Google Patents
Manufacturing method of aluminum nitrideInfo
- Publication number
- JPH0637286B2 JPH0637286B2 JP62301301A JP30130187A JPH0637286B2 JP H0637286 B2 JPH0637286 B2 JP H0637286B2 JP 62301301 A JP62301301 A JP 62301301A JP 30130187 A JP30130187 A JP 30130187A JP H0637286 B2 JPH0637286 B2 JP H0637286B2
- Authority
- JP
- Japan
- Prior art keywords
- aluminum nitride
- aqueous solution
- nitrogen
- containing compound
- mixed aqueous
- 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.)
- Expired - Lifetime
Links
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- Ceramic Products (AREA)
Description
【発明の詳細な説明】 〔技術分野〕 この発明は、たとえば高熱伝導率のセラミックス基板を
製造するために使用されるような窒化アルミニウム粉末
の製造技術の分野に属する。Description: TECHNICAL FIELD The present invention belongs to the field of manufacturing technology of aluminum nitride powder such as used for manufacturing a ceramic substrate having high thermal conductivity.
ＩＣ等に代表されるような半導体素子の高集積化や大電
力化が進み、これに伴って放熱性の良い電気絶縁材料が
要求されるようになった。With higher integration and higher power consumption of semiconductor elements represented by ICs and the like, along with this, electric insulating materials having good heat dissipation have been required.
これに応えて、各種の高熱伝導率セラミックス基板が提
案されている。In response to this, various types of high thermal conductivity ceramic substrates have been proposed.
その中でも、特に窒化アルミニウムセラミックス基板が
熱伝導性、熱膨張性、電気絶縁性等の点で優れていると
言うことから、実用化が進んでいる。Among them, in particular, aluminum nitride ceramics substrates are being put to practical use because they are excellent in terms of thermal conductivity, thermal expansion property, electrical insulating property, and the like.
ところが、この窒化アルミニウムセラミックス基板は、
価格が高いという欠点がある。この高価格の原因として
は、特に、原料となる窒化アルミニウム粉末が高価格で
あること、焼結に高温を要することなどが挙げられる。However, this aluminum nitride ceramic substrate is
It has the drawback of being expensive. The reason for this high price is that aluminum nitride powder as a raw material is expensive and that sintering requires high temperature.
従来から窒化アルミニウム粉末は、アルミニウムの直接
窒化や、アルミナの炭素還元等の方法によって製造され
ているが、たとえば、アルミニウムの直接窒化法におい
ては、高純度で粒径の小さい窒化アルミニウム粉末を得
ることが困難であり、アルミナの炭素還元法において
は、反応に高温を要する、原料価格が高い等の問題があ
った。Conventionally, aluminum nitride powder has been produced by methods such as direct nitriding of aluminum and carbon reduction of alumina. For example, in the direct nitriding method of aluminum, it is possible to obtain aluminum nitride powder with high purity and small particle size. However, in the carbon reduction method of alumina, there are problems that the reaction requires a high temperature and the raw material cost is high.
アルミナの炭素還元法の改良として、アルミニウム源を
液中で混合する方法などが提案さされているが、けん濁
状態での混合であり、分子オーダーでの混合がなされな
いため、均一な反応を行わせるためには、反応を高温で
行う必要がある等により、製造価格が高くなるなどの問
題が残っている（特公昭６１−２６４８５号公報）。As a method for improving the carbon reduction method of alumina, a method of mixing an aluminum source in a liquid has been proposed, but since it is mixing in a suspended state and mixing on a molecular order is not performed, a uniform reaction is achieved. In order to carry out the reaction, it is necessary to carry out the reaction at a high temperature, so that there remains a problem that the manufacturing cost becomes high (Japanese Patent Publication No. 61-26585).
この発明は、以上のような事情に鑑みてなされたもので
あり、純度が高くかつ微粒子の粉末を安価に得ることが
できる窒化アルミニウム粉末の製法を提供することを目
的としている。The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a method for producing an aluminum nitride powder, which has a high purity and can obtain a fine particle powder at a low cost.
この発明は、以上のような目的を達成するために、塩基
性硝酸アルミニウム、炭素含有化合物および／または窒
素含有化合物を含む混合水溶液を得た後、この混合水溶
液から水分を除去すると共に窒素を含む非酸化性雰囲気
中で焼成することを特徴とする窒化アルミニウムの製法
を提供するものである。In order to achieve the above object, the present invention obtains a mixed aqueous solution containing basic aluminum nitrate, a carbon-containing compound and / or a nitrogen-containing compound, removes water from the mixed aqueous solution and contains nitrogen. The present invention provides a method for producing aluminum nitride, which is characterized by firing in a non-oxidizing atmosphere.
以下、この発明を工程に従って順次詳しく説明する。も
っとも、以下の工程は例示的趣旨のものであり、これに
より本発明の範囲が限定されるものではない。Hereinafter, the present invention will be described in detail step by step. However, the following steps are for illustrative purposes only, and the scope of the present invention is not limited thereby.
塩基性硝酸アルミニウム、炭素含有化合物および／ま
たは窒素含有化合物を水溶液として混合する。Basic aluminum nitrate, carbon-containing compound and / or nitrogen-containing compound are mixed as an aqueous solution.
なお、各成分原料を別々に水に溶かし、これを混合して
混合水溶液を得てもよく、原料混合物を先ず作り、これ
を水に溶かして混合水溶液としてもよい。The raw materials for each component may be separately dissolved in water and mixed to obtain a mixed aqueous solution, or a raw material mixture may be first prepared and then dissolved in water to form a mixed aqueous solution.
この水溶液では、各成分が分子オーダーで均質に混合さ
れている。In this aqueous solution, the components are homogeneously mixed on the molecular order.
炭素含有化合物としては、各種糖類、メチルセルロー
ス、ポリエチレンオキサイド、ポリビニルアルコールな
ど水溶性のものが挙げられる。Examples of the carbon-containing compound include water-soluble compounds such as various sugars, methyl cellulose, polyethylene oxide, and polyvinyl alcohol.
窒素含有化合物としては、尿素、グリシンなどの水溶性
のものが挙げられる。Examples of the nitrogen-containing compound include water-soluble compounds such as urea and glycine.
前記混合水溶液から、蒸発乾燥により塩基性硝酸アル
ミニウム、炭素含有化合物および／または窒素含有化合
物が分子オーダーで均質に混合された混合物粉末を得
る。乾燥温度としては、１００〜２００℃が適当であ
る。From the mixed aqueous solution, a mixture powder in which basic aluminum nitrate, a carbon-containing compound and / or a nitrogen-containing compound are homogeneously mixed in a molecular order is obtained by evaporative drying. A suitable drying temperature is 100 to 200 ° C.
この混合粉末を窒素を含む非酸化性雰囲気中で焼成し
て窒化アルミニウム粉末を得る。混合物粉末は、混合物
中に窒素源を有している場合は、混合物内部から窒化反
応が促進され、窒化アルミニウムが迅速に形成される。This mixed powder is fired in a non-oxidizing atmosphere containing nitrogen to obtain an aluminum nitride powder. When the mixture powder has a nitrogen source in the mixture, the nitriding reaction is promoted from the inside of the mixture, and aluminum nitride is rapidly formed.
非酸化性雰囲気としては、窒素さらに好ましくはアンモ
ニアなどが使用される。As the non-oxidizing atmosphere, nitrogen, more preferably ammonia or the like is used.
焼成温度は、９００℃以上、好ましくは１２００〜１８
００℃である。The firing temperature is 900 ° C. or higher, preferably 1200 to 18
It is 00 ° C.
なお、残留炭素は窒化アルミニウム形成後、６００〜７
５０℃の酸化性雰囲気中で加熱処理するようにすれば除
去できる。Residual carbon is 600 to 7 after aluminum nitride is formed.
It can be removed by heat treatment in an oxidizing atmosphere at 50 ° C.
この発明の製造によれば、塩基性硝酸アルミニウム、炭
素含有化合および／または窒素含有化合物を含む混合水
溶液を得た後、この混合水溶液から水分を除去すると共
に、窒素を含む非酸化性雰囲気中で焼成することを特徴
とするので、微細で均質な窒化アルミニウム粉末を迅速
に、かつ安価に得ることができる。According to the production of the present invention, after a mixed aqueous solution containing basic aluminum nitrate, a carbon-containing compound and / or a nitrogen-containing compound is obtained, water is removed from the mixed aqueous solution, and the mixed aqueous solution is removed in a non-oxidizing atmosphere containing nitrogen. Since it is characterized by firing, a fine and uniform aluminum nitride powder can be obtained quickly and at low cost.
なお、このものは微細粉末であるので、焼結性がよいと
いう効果もある。Since this is a fine powder, it also has the effect of good sinterability.
以下、実施例に基づきさらに詳しく説明する。Hereinafter, further details will be described based on examples.
実施例 塩基性硝酸アルミニウムとして、 ［Ａｌ13O4(OH)２５(H2O)11］(NO3)３（純度８０重％）
のものを使用し、これとブドウ糖をＣ／Ａｌ2O3＝０．
８の重量比率となるように水溶液を調整し、１５０℃で
乾燥して混合粉末を得た。Example As basic aluminum nitrate, [Al 13 O 4 (OH) 25 (H 2 O) 11 ] (NO 3 ) 3 (purity 80 weight%)
Of C / Al 2 O 3 = 0.
The aqueous solution was adjusted to have a weight ratio of 8 and dried at 150 ° C. to obtain a mixed powder.
つぎに、前記混合粉末を窒素ガス雰囲気中で、１５００
℃で５時間焼成して窒化アルミニウム粉末を得た。Next, the mixed powder was subjected to 1500 gas in a nitrogen gas atmosphere.
It baked at 5 degreeC for 5 hours, and the aluminum nitride powder was obtained.
なお、得られた窒化アルミニウム粉末は、純度が９８．
５重量％以上、平均粒径０．３μｍであった。The obtained aluminum nitride powder had a purity of 98.
The content was 5% by weight or more and the average particle size was 0.3 μm.
この発明は、塩基性硝酸アルミニウム、炭素含有化合物
および／または窒素含有化合物を含む混合水溶液を得た
後、この混合水溶液から水分を除去すると共に窒素を含
む非酸化性雰囲気中で焼成することを特徴とするので、
微粒子で純度の高い窒化アルミニウム粉末を安価に得る
ことができる効果がある。This invention is characterized in that after a mixed aqueous solution containing basic aluminum nitrate, a carbon-containing compound and / or a nitrogen-containing compound is obtained, water is removed from the mixed aqueous solution and the mixture is baked in a non-oxidizing atmosphere containing nitrogen. Since,
The effect is that fine particles of high-purity aluminum nitride powder can be obtained at low cost.
Claims (1)
および／または窒素含有化合物を含む混合水溶液を得た
後、この混合水溶液から水分を除去すると共に、窒素を
含む非酸化性雰囲気中で焼成することを特徴とする窒化
アルミニウムの製法。1. After obtaining a mixed aqueous solution containing basic aluminum nitrate, a carbon-containing compound and / or a nitrogen-containing compound, removing water from the mixed aqueous solution and baking in a non-oxidizing atmosphere containing nitrogen. A method for manufacturing aluminum nitride, which is characterized by:
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62301301A JPH0637286B2 (en) | 1987-11-28 | 1987-11-28 | Manufacturing method of aluminum nitride |
| US07/273,761 US4985225A (en) | 1987-10-26 | 1988-08-22 | Process for producing aluminum nitride powders |
| KR1019880010683A KR950005761B1 (en) | 1987-10-26 | 1988-08-23 | Process for producing aluminum nitride powders |
| DE3828598A DE3828598C2 (en) | 1987-10-26 | 1988-08-23 | Process for the production of aluminum nitride powders |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62301301A JPH0637286B2 (en) | 1987-11-28 | 1987-11-28 | Manufacturing method of aluminum nitride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01141810A JPH01141810A (en) | 1989-06-02 |
| JPH0637286B2 true JPH0637286B2 (en) | 1994-05-18 |
Family
ID=17895191
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62301301A Expired - Lifetime JPH0637286B2 (en) | 1987-10-26 | 1987-11-28 | Manufacturing method of aluminum nitride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0637286B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116062714A (en) * | 2023-01-18 | 2023-05-05 | 大连海事大学 | Pure-phase nanometer AlN powder and preparation method and application thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63210003A (en) * | 1987-02-24 | 1988-08-31 | Matsushita Electric Works Ltd | Production of aluminum nitride powder |
| JPS63210002A (en) * | 1987-02-24 | 1988-08-31 | Matsushita Electric Works Ltd | Production of aluminum nitride powder |
| JPS6456309A (en) * | 1987-08-26 | 1989-03-03 | Matsushita Electric Works Ltd | Production of aluminum nitride powder |
-
1987
- 1987-11-28 JP JP62301301A patent/JPH0637286B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01141810A (en) | 1989-06-02 |
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