JPS6256309A - Production of fine aluminum nitride powder - Google Patents
Production of fine aluminum nitride powderInfo
- Publication number
- JPS6256309A JPS6256309A JP19387285A JP19387285A JPS6256309A JP S6256309 A JPS6256309 A JP S6256309A JP 19387285 A JP19387285 A JP 19387285A JP 19387285 A JP19387285 A JP 19387285A JP S6256309 A JPS6256309 A JP S6256309A
- Authority
- JP
- Japan
- Prior art keywords
- aluminum nitride
- nitride powder
- powder
- halogenated hydrocarbon
- fine aluminum
- 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
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、微粉末窒化アルミニウムの製造方法：に関す
る。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing fine powder aluminum nitride.
セラミック粉末を製造する際には水あるいはエタノール
、インブタノール等の溶媒の存在下湿式粉砕して製造す
ることが知られている。しかし、これらの方法において
、前者の方法ではサブミクロンオーダの粉末窒化アルミ
ニウムを得ることが難しいばかりでなく窒化アルミニウ
ムの加水分解を伴いＮＨ３ガスを発生し、工業的に使用
できない欠点がある。また後者の有機溶媒を用いる方法
では、微粉末化はできるが、エタノール、インブタノー
ルなどによる酸化により窒化アルミニウム中の一部がア
ルミナ及びアルミナ水和物となり、組成式ＡＩＮ以外は
すべて不純物とみなすため製品の純度が低下する欠点が
ある。It is known that ceramic powder is produced by wet grinding in the presence of water or a solvent such as ethanol or inbutanol. However, in the former method, it is not only difficult to obtain powdered aluminum nitride on the order of submicrons, but also NH3 gas is generated due to hydrolysis of aluminum nitride, making it unsuitable for industrial use. In addition, in the latter method using an organic solvent, fine powder can be obtained, but part of the aluminum nitride becomes alumina and alumina hydrate due to oxidation with ethanol, inbutanol, etc., and everything other than the composition formula AIN is considered to be an impurity. The disadvantage is that the purity of the product is reduced.
本発明の目的は、加水分解や酸化を起すことなく高純度
でしかも平均粒子径が１μｍ程変Ｑ９化アルミニウム粉
末を製造することができる方法を提供するところにある
。An object of the present invention is to provide a method for producing aluminum Q9 powder of high purity and having an average particle diameter of about 1 μm without causing hydrolysis or oxidation.
本発明は、５（化アルミニウム粉末を、その窒化アルミ
ニウム粉末のｔａに対して等廿以上の）・ロデン化炭化
水素溶媒中で粉砕することを特徴とする微粉末窒化アル
ミニウムの製造方法である。The present invention is a method for producing finely powdered aluminum nitride, which is characterized by pulverizing aluminum nitride powder in a lodenated hydrocarbon solvent having a ta of at least equal to the ta of the aluminum nitride powder.
以下、さらに詳しく本発明を説明する。The present invention will be explained in more detail below.
原料である窒化アルミニウム粉末の粒度は７４μｍ以下
であることが好ましい。７４μｎ〕を超えると粉砕効果
が悪くなり粗粒が多（残る欠点がある。The particle size of the raw material aluminum nitride powder is preferably 74 μm or less. If it exceeds 74 μn, the pulverizing effect will be poor and there will be a large number of coarse particles (some remaining defects).
原料窒化アルミニウムの粉末とハロケ”ン比炭化水素と
を所定の割合に混合し粉砕機へ装入する。ハロケ０ン化
炭化水素としてはｉ 、 ｉ 、 ｉ ＋−リクロール
エタン、クロロホルム等があげられるカ１，１゜１−ト
リクロールエタンは粉砕助剤効果の大きいこともあるが
特に窒化アルミニウムを加水分解させずに微粉化でき得
る利点を有している。、溶媒の量は、原料窒化アルミニ
ウムの重ψに対し等せ以上とすることが好ましい。等址
倍未満では、粉砕熱により溶媒が連敗して粉砕効果が低
下する。上限についズは特に限定はないが、スラリー濃
度の減少による粘性の低下により粉砕効果が悪（なるの
で、５重量倍以下とするのが望ましい。好ましくは２重
量倍を超え４重量倍以下である。粉砕機としては、めの
うやコランダム質又は炭化水素におかされない材質の内
張をしたボールミル、（辰動ミル、アトライターミルな
どを用いる。以上の方法で粉砕して得たスラリーを、次
に遠心分離機、フィルタープ１７ス、ヌツチェ等で分離
しケーク状としてこれを乾燥し溶媒を除去することによ
り微粉末窒化アルミニウムとすることができる。Raw material aluminum nitride powder and halokene ratio hydrocarbons are mixed at a predetermined ratio and charged into a pulverizer. Examples of halokene hydrocarbons include i, i, i + -lichloroethane, chloroform, etc. 1,1゜1-trichloroethane has a great effect as a grinding aid, but it also has the advantage of being able to pulverize aluminum nitride without hydrolyzing it. It is preferable that the weight be equal to or more than the weight ψ of aluminum.If it is less than the same weight, the solvent will continuously lose due to the heat of grinding and the grinding effect will decrease.There is no particular limit to the upper limit, but due to the decrease in slurry concentration The pulverizing effect will be poor due to the decrease in viscosity, so it is desirable that the crushing effect be less than 5 times the weight. Preferably it is more than 2 times the weight and less than 4 times the weight. Use a ball mill lined with a material that is not contaminated with water (such as a radial mill or an attritor mill.) The slurry obtained by grinding in the above manner is then separated using a centrifuge, a filter, a nutsche, etc., and a cake is formed. Fine powder aluminum nitride can be obtained by drying this as a solid state and removing the solvent.
次に本発明を実施例および比イ・文例をあげて説すＪＪ
する。窒化アルミニウム粉末（ｄｔ気化学工業（印−叫
）囚と１ 、１ 、１１リクロールエタン（商品名「ク
ロロセン」旭ダウ社□）（Ｂ）とを表に示す割合で混合
し、この混合物をポリエチレンライニングのボールミル
（容ｆ１０１）に装入して１０時間粉砕した。次に、こ
の粉砕物をヌツチェで分離１゜ケーク状窒化アルミニウ
ムとｌ−た後、真空ｔｆ、燥機（東洋製作所■製商品名
「ＶＴＪＣＵＭ ＤＲＹＩ：ＮＧ ０ＶＥＮＪ ）に装
入し一７００ｍｍＨｇ、 １００℃で１昼夜乾燥して
クロロセンを除去した。この様にして得た製品の平均粒
子径、窒素及び酸素含有量、並びにＸ線回折の測定結果
を表に示す。Next, JJ will explain the present invention by giving examples, comparisons, and examples.
do. Aluminum nitride powder (dt Kagaku Kogyo Co., Ltd.) and 1, 1, 11 chlorethane (trade name "Chlorocene" Asahi Dow Co., Ltd.) (B) were mixed in the proportions shown in the table, and this mixture was It was charged into a polyethylene-lined ball mill (capacity F101) and pulverized for 10 hours.Then, this pulverized product was separated with a Nutsche and mixed with a 1° cake-like aluminum nitride, and then placed in a vacuum TF and dryer (manufactured by Toyo Seisakusho). The product was charged into a container (trade name: VTJCUM DRYI: NG 0VENJ) and dried at 1700 mmHg and 100°C for one day and night to remove chlorocene.The average particle size, nitrogen and oxygen content, and X-ray The results of diffraction measurements are shown in the table.
米実験番号４はクロロセンの代わりに水を使用し′−Ａ
＞２番号５はイソシタノールを用いた。Rice experiment number 4 used water instead of chlorocene'-A
>2 No. 5 used isositanol.
なお表に示す物性値は次の方法に準じた。The physical property values shown in the table were determined according to the following method.
（１）平均粒子径・・・・・・・・・”ｐ’ｓｓｓによ
る（フィッシャー社製）
（２） ’４素含有量・・・・・・・・・化学分析によ
る（ケルゾール法）
（３）酸素含有量・・・・・・・・・Ｏ／Ｎ同時分析計
商品名ｒＴｃ−１３６Ｊ
（ｒ＝ｇｃｏ 、１＋ ＃ ）
（４）Ｘ線回折・・・・・・・・・・・・ガイが一フレ
ックス２０１６型（ＪｊＪ学電機展）
〔発明の効果〕
本発明によれば加水分解や酸化を起すことｉｃ ＜サブ
ミクロンオーダの窒化アルミニウム粉末を製造すること
ができる。(1) Average particle diameter...... by p'sss (manufactured by Fischer) (2) Quaternary content...... by chemical analysis (Kelsol method) ( 3) Oxygen content...... O/N simultaneous analyzer product name rTc-136J (r=gco, 1+ #) (4) X-ray diffraction... - Gai Ichiflex 2016 type (JJJ Gakudenki Exhibition) [Effects of the Invention] According to the present invention, it is possible to produce aluminum nitride powder on the order of submicrons without causing hydrolysis or oxidation.
Claims (1)
末の重量に対して等量以上のハロゲン化炭化水素溶媒中
で粉砕することを特徴とする微粉末窒化アルミニウムの
製造方法。 ２、ハロゲン化炭化水素が１，１，１トリクロールエタ
ンであることを特徴とする特許請求の範囲第１項記載の
微粉末窒化アルミニウムの製造方法。[Claims] 1. A method for producing fine powder aluminum nitride, which comprises pulverizing aluminum nitride powder in a halogenated hydrocarbon solvent in an amount equal to or more than the weight of the aluminum nitride powder. 2. The method for producing fine powder aluminum nitride according to claim 1, wherein the halogenated hydrocarbon is 1,1,1 trichloroethane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19387285A JPS6256309A (en) | 1985-09-04 | 1985-09-04 | Production of fine aluminum nitride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19387285A JPS6256309A (en) | 1985-09-04 | 1985-09-04 | Production of fine aluminum nitride powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6256309A true JPS6256309A (en) | 1987-03-12 |
Family
ID=16315152
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19387285A Pending JPS6256309A (en) | 1985-09-04 | 1985-09-04 | Production of fine aluminum nitride powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6256309A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0647538U (en) * | 1992-10-12 | 1994-06-28 | 立山アルミニウム工業株式会社 | Door handle |
| JPH07159A (en) * | 1991-08-30 | 1995-01-06 | Noritake Co Ltd | Roasting mechanism in sieving operation type roaster |
| AU718494B2 (en) * | 1997-01-11 | 2000-04-13 | Ecc International Limited | Processing of ceramic materials |
| US20130059522A1 (en) * | 2011-09-03 | 2013-03-07 | Denso Corporation | Air conditioner for vehicle |
-
1985
- 1985-09-04 JP JP19387285A patent/JPS6256309A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07159A (en) * | 1991-08-30 | 1995-01-06 | Noritake Co Ltd | Roasting mechanism in sieving operation type roaster |
| JPH0647538U (en) * | 1992-10-12 | 1994-06-28 | 立山アルミニウム工業株式会社 | Door handle |
| AU718494B2 (en) * | 1997-01-11 | 2000-04-13 | Ecc International Limited | Processing of ceramic materials |
| US20130059522A1 (en) * | 2011-09-03 | 2013-03-07 | Denso Corporation | Air conditioner for vehicle |
| US9290078B2 (en) | 2011-09-03 | 2016-03-22 | Denso Corporation | Air conditioner for vehicle |
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