JPS58135112A - Production of aluminum oxynitride - Google Patents

Production of aluminum oxynitride

Info

Publication number
JPS58135112A
JPS58135112A JP57014992A JP1499282A JPS58135112A JP S58135112 A JPS58135112 A JP S58135112A JP 57014992 A JP57014992 A JP 57014992A JP 1499282 A JP1499282 A JP 1499282A JP S58135112 A JPS58135112 A JP S58135112A
Authority
JP
Japan
Prior art keywords
powder
aluminum
producing
mixed powder
weight
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
JP57014992A
Other languages
Japanese (ja)
Inventor
Katsutoshi Yoneya
勝利 米屋
Akihiko Tsuge
柘植 章彦
Hiroshi Inoue
寛 井上
Hiroyasu Ota
博康 大田
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
Tokyo Shibaura Electric Co Ltd
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, Tokyo Shibaura Electric Co Ltd filed Critical Toshiba Corp
Priority to JP57014992A priority Critical patent/JPS58135112A/en
Publication of JPS58135112A publication Critical patent/JPS58135112A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:An Al powder and an Al2O3 powder are combined at a specific ratio and the mixed powder is calcined in a specific temperature range in an atmosphere mainly containing N2 gas to enable the calcination at a low temperature. CONSTITUTION:15-50wt% of A powder and 50-85wt% of Al2O3 powder are mixed to prepare a mixed powder. The Al powder is preferably scaly and the Al2O3 powder has less than 1 micron particle sizes. The mixed powder is calcined at 600-1,200 deg.C, particularly 650-900 deg.C in an atmosphere mainly consisting of N2 gas into aluminum oxynitride. A part of Al2O3 may be replaced with AlN of less than 2 micron particle sizes so that the total amount of Al and AlN does not exceed 50wt% based on the total amount of the powder mixture.

Description

【発明の詳細な説明】 〔発明O技術分野〕 本発明はアルミニウム酸窒化物の製造方法に関、シ、更
に詳しくは、省エネルギーを可能としたアルミニウム酸
窒化物の製造方法に関する。
DETAILED DESCRIPTION OF THE INVENTION [Technical Field of the Invention] The present invention relates to a method for producing aluminum oxynitride, and more particularly, to a method for producing aluminum oxynitride that enables energy saving.

〔発明の技術的背景〕[Technical background of the invention]

非酸化性材料の1種であるアルミニウム酸窒化物は、耐
熱性、電気絶縁性、耐食性に優れ、その緻密な焼結体は
透光性を備えているので注目を集めていゐ。
Aluminum oxynitride, a type of non-oxidizing material, is attracting attention because it has excellent heat resistance, electrical insulation, and corrosion resistance, and its dense sintered body is transparent.

このアルミニウム酸窒化物は、一般式=(ムα)・(ム
tshs)ア(!、yはそれぞれモル数を表わす、)で
示されるメビネル麿化合物である。
This aluminum oxynitride is a mebinel compound represented by the general formula=(α)·(mutshs)a (!, y each represents the number of moles).

これは通常、窒化アルミニウム(hni )と酸化アル
ミニウム(At寓Os )を原料とし、これらの原料を
それぞれ目的とするアル(% ニクム駿窪化I#I。
It usually uses aluminum nitride (hni) and aluminum oxide (Ategos) as raw materials, and uses these raw materials as aluminum (% nicum), respectively.

化学組成に対応させて配合し、得られた混合粉末t15
00℃以上の温度域で焼成して製造されている。
Mixed powder t15 obtained by blending according to the chemical composition
It is manufactured by firing at a temperature range of 00°C or higher.

〔背景技術の問題点〕[Problems with background technology]

上記した製造方法は、1500℃以上の高温域における
同相反応を適用するものであるため、その反応工sK必
要とする熱エネルギーは大きく、それを供給するために
、煩雑かつ高価の設備を必要とするという工業上の難点
があった。
Since the above manufacturing method applies an in-phase reaction in a high temperature range of 1500°C or higher, the reaction process requires a large amount of thermal energy and requires complicated and expensive equipment to supply it. There was an industrial difficulty in doing so.

〔発明の目的〕[Purpose of the invention]

本発明は、従来適用されていた焼成温度よシもはるかに
低い温度でアルミニウム酸窒化物を製造することができ
、したが9て、熱エネルギー的に優れ友製造方法の提供
を目的とする。
The present invention is capable of producing aluminum oxynitride at a much lower temperature than conventionally applied firing temperatures, and therefore aims to provide a method for producing aluminum which is superior in terms of thermal energy.

〔発明の概要〕[Summary of the invention]

本発明は、アルミニウム(At)の窒化反応が次式で示
すような発熱反応であることに着目してなされ九もので
ある。
The present invention was made by focusing on the fact that the nitriding reaction of aluminum (At) is an exothermic reaction as shown by the following formula.

2 ムL + Nm  →2  ムIN  −152,
8K@alすなわち、ム10粉末をN、雰囲気中で60
0℃以上の温度に加熱すると、上に示し九反応が起生し
てムαを生成すると同時に、この反応系は発熱して自ら
昇温する。
2 MU L + Nm → 2 MU IN -152,
8K@al, i.e. 60% of Mu10 powder in N atmosphere
When heated to a temperature of 0° C. or higher, the nine reactions shown above occur to produce mu α, and at the same time, this reaction system generates heat and raises its temperature by itself.

本発明方法は、この反応系に発生し良熱量をアルミニウ
ム酸窒化物の生成に必要な熱量の一部として利用するも
のである。
The method of the present invention utilizes the good amount of heat generated in this reaction system as part of the amount of heat required to produce aluminum oxynitride.

本発明方法は、Atとムt、OSとの各粉末を所定量配
合し、得られ九混合粉末t N mガスを主成分とする
雰囲気下、600〜1200℃の温度で焼成することを
特徴とするものである。
The method of the present invention is characterized in that a predetermined amount of each powder of At, Mut, and OS is blended, and the resulting mixed powder is fired at a temperature of 600 to 1200°C in an atmosphere containing tNm gas as the main component. That is.

本発明方法にありては、まず、ムt、ムt303の各粉
末を所定量配合して成る混合粉末を出発原料とする。
In the method of the present invention, first, a mixed powder obtained by blending predetermined amounts of Mut and Mut303 powders is used as a starting material.

このとき、ムtとムt!01の配合量は、At:151
0重量−、ムL@OH: 85〜50重量−の範Hに設
定されることが好ましく、ムtの配合量が15重量−未
満の場合には後述する窒化反応時に発生する熱量が小さ
く、アルミニウム酸窒化物の生成に必  □要な熱量を
充分に補完するととKならない。逆に、ムtが50重量
参を超えると、ムtとムtが混合粉末中で互いに隣接し
て存在するようKな〉、それは窒化反応の結果による発
熱でムを相互が融着(ムtの融点:660℃)してムL
全体がLα化することなく凝集するという事態を招く。
At this time, Mut and Mut! The blending amount of 01 is At:151
0 weight -, Mu L@OH: It is preferable to set it in the range H of 85 to 50 weight -, and when the amount of Mut is less than 15 weight -, the amount of heat generated during the nitriding reaction described later is small, □If the amount of heat required to generate aluminum oxynitride is sufficiently supplemented, it will not reach K. On the other hand, when Mt exceeds 50% by weight, Mt and Mt exist adjacent to each other in the mixed powder. Melting point of t: 660℃)
This results in a situation in which the entire product aggregates without being converted into Lα.

その意味では、混合粉末のAj*Osの一部を予めムα
で置換して混在せしめると、このムαが一種のムL希釈
剤oathsをして上記した不都合を解消するので有効
である。友だし、その場合、ムαの配合量は、ムtとム
αの総量がムを重量に換算して全混合粉末重量の50重
量−を超えない量で参ることが好ましく、鋏総量が50
重量−を超えると、ムαが必要以上に残存するといった
不都合を派生する。
In that sense, a part of Aj*Os of the mixed powder is
It is effective to replace and mix with Muα, since this Muα acts as a kind of MuL diluent oaths and eliminates the above-mentioned inconvenience. In that case, it is preferable that the amount of Mu α is such that the total amount of Mu t and Mu α does not exceed 50% by weight of the total mixed powder weight when Mu is converted to weight, and the total amount of Mu α is 50% by weight.
If the weight exceeds -, a problem arises in that more mu α remains than necessary.

このようKして配合されえ出発原料の混合粉末は、総重
量が20p以上であることが好ましく、該重量が201
1未満の場合には、ムtの窒化反応による発生熱量が小
さく全体の系の反応が円滑に進行しない。
It is preferable that the mixed powder of starting materials that can be blended in this way has a total weight of 20p or more, and the weight is 201p or more.
When it is less than 1, the amount of heat generated by the nitriding reaction of Mut is small and the reaction of the entire system does not proceed smoothly.

、まえ、ム1.0.粉末は粒径1μ鯛以下、必要に応じ
て配合するムα粉末の粒径は2#調以下、ムtKついて
は後述する窒化反応に伴う熱量を有効に発生させる丸め
に5μ講以下のリン片状の粉末を用いることが好ましい
、肯発熱を利用することから、充てん時の多孔度に対応
する相対密度は4〇−以下であることが好ましい。
, Mae, Mu 1.0. The particle size of the powder is 1μ or less, the particle size of the Muα powder blended as necessary is 2# or less, and the MutK is a scale-shaped powder with a round size of 5μ or less that effectively generates the amount of heat associated with the nitriding reaction described later. Since positive heat generation is utilized, the relative density corresponding to the porosity at the time of filling is preferably 40 or less.

さて、この出発原料は次に、N5t−主成分とする雰囲
気中で焼成される。この段階でムtの窒化反応とアルi
 +ラム酸窒化物生成反応とが進行する。
Next, this starting material is fired in an atmosphere containing N5t as the main component. At this stage, the nitriding reaction of Mut and the Al i
+Rum oxynitride production reaction progresses.

焼成社SOO〜1200℃、好ましくは650〜900
℃oiit域で行われる。焼成温度が600℃未満の場
合には、上記し九ムtの窒化反応は進行せず、また、1
200℃を超えるといたずらに無駄な熱量を供給すゐの
みであ〉、熱経済的には何んらOメリットも与えまい。
Baking company SOO~1200℃, preferably 650~900℃
It is carried out in the ℃oiit region. If the firing temperature is less than 600°C, the nitriding reaction described above will not proceed, and the nitriding reaction will not proceed.
If the temperature exceeds 200°C, it will only provide unnecessary heat and will not provide any thermoeconomic benefits.

この焼成段階においては、ム10@面に供給されるN3
によりてムLはムαへと窒化し、そのとき発熱する。そ
O結果、反応系は全体としてよシ高い温度に昇温して1
500℃以上、しばしば1800℃以上Keる。
In this firing stage, N3 is supplied to the mu 10@ surface.
As a result, MU L is nitrided to MU α, and heat is generated at this time. As a result, the reaction system as a whole is heated to a much higher temperature.
Ke of 500°C or more, often 1800°C or more.

反応系から自生する発熱は、配合したムシ粉末011面
積に規制されるので、本発明方法にありては、このムを
粉末の表面積を大きくすることが有利である。その丸め
、ムL粉末としては、シん片状の粉末でその粒WkSs
講以下のものを用いることが好ましい、を九、本発明方
法にあっては、反応系で発生する熱量を系外に無駄に放
散させない丸めに、例えば、反応系を収納する容器とし
て断熱性の良い材料を用いるとか、全体を断熱材で被包
するなどの手段を講じることが有効である。
Since the heat generated spontaneously from the reaction system is regulated by the area of the mixed powder 011, in the method of the present invention, it is advantageous to increase the surface area of the powder. The rounded, muL powder is a flaky powder whose grains WkSs
9. In the method of the present invention, it is preferable to use a container that contains the reaction system in a round shape that does not wastefully dissipate the amount of heat generated in the reaction system outside the system. It is effective to take measures such as using good materials or covering the entire structure with heat insulating material.

〔発明の実施例〕[Embodiments of the invention]

実施例1 粒径3μ常のリン片状At粉末30jlと粒径0.3μ
mのAt、O,粉末7(lとをボールミルで乾式混合し
友。
Example 1 30jl of scale-like At powder with a particle size of 3μ and a particle size of 0.3μ
Dry mix At, O, and powder 7 (l) in a ball mill.

得られた混合粉末のうち40.Fを内容積40■×40
箇×180■の黒鉛製ボートの中に入れ、etm種状を
気rを用い、3001/br (D Nsガスを流入し
ながら700℃で1時間焼成した。
Of the obtained mixed powder, 40. F has an internal volume of 40×40
The mixture was placed in a 180 mm graphite boat and fired at 700° C. for 1 hour using 3001/br (D Ns gas) using air.

混合粉末の温度は!100℃まで上昇し、ムtの窒化反
応が急激に進行していることが確認された。
What is the temperature of the mixed powder? The temperature rose to 100°C, and it was confirmed that the nitriding reaction of Mut was rapidly progressing.

得られえインゴットを粉砕し、その組成を分析し九とヒ
ろ、ムtは単独では存在せず、大略スピネル相であるこ
とが確認されえ。
The obtained ingot was crushed and its composition was analyzed, and it was confirmed that the ingot did not exist alone and that it was roughly in the spinel phase.

実施例2〜7 実施例1に準じて表に示した組成め混合粉末を調製し、
表に示し九条件で焼成した。実施例1と同様に反応時の
温度を測定し、得られたインゴットを粉砕してその組成
を分析した。結果を一括して表に示した。
Examples 2 to 7 Mixed powders with the composition shown in the table were prepared according to Example 1,
Firing was performed under the nine conditions shown in the table. The temperature during the reaction was measured in the same manner as in Example 1, and the resulting ingot was crushed and its composition analyzed. The results are summarized in the table.

実施例8 実施例1と同一仕様のムL粉末1sIi、ム1.0゜2
0IIの外に粒110.2 setのムz(oH)、の
粉末459を用、いたととを除いては実施例1と同様に
して、これら混合粉末を焼成し丸。組成(ムAN )x
(Ak Os )yのxYは決めがたいがX線的にこの
化合物であることを示すスピネル減のアルミニウム酸窒
化物が得られえ。
Example 8 MuL powder 1sIi, Mu 1.0゜2 with the same specifications as Example 1
These mixed powders were fired in the same manner as in Example 1, except that powder 459 of Muz (oH) of 110.2 sets of grains was used in addition to 0II. Composition (MUAN) x
Although it is difficult to determine xY of (Ak Os )y, an aluminum oxynitride with reduced spinel can be obtained, which is shown to be this compound by X-rays.

〔発明の効果〕〔Effect of the invention〕

以上の説明で明らかなように、本発明方法はムtの窒化
反応に伴って自生する熱量を有効に利用するので、従来
方法のように外部から大きな熱エネルギーを投入するこ
とが不要となりその工業的な価値は大である。
As is clear from the above explanation, the method of the present invention effectively utilizes the amount of heat generated naturally during the nitriding reaction of Mut, so it is not necessary to input a large amount of thermal energy from the outside as in the conventional method, and the method can be used in various industries. The value is great.

Claims (1)

【特許請求の範囲】 1、 アルミニウムと酸化アルミニウムとの各粉末を所
定量配合し、得られた混合粉末を窒素ガスを主成分とす
る雰囲気下、600〜1200℃の温度で焼成すること
を特徴とするアルミニウム酸窒化物の製造方法。 2、該混合粉末において、皺酸化アルミニウムの配合量
が50〜85重量−である特許請求の範囲第1項記載の
アルミニウム酸窒化物の製造方法。 3、該酸化アルミニウムの一部を粒径2μm以下の窒化
アルミニウムで置換し、かつ、該アルミニウムと該窒化
アルミニウムの総量がアル叱ニウム重量に換算して誼混
合粉末全体に対し50重量−を超え危い特許請求の範囲
第1項記載のアルミニウム酸窒化物の製造方法。 4、咳アルミニウム粉末がリン片状の粉末である特許請
求の範囲第1〜第3項のいずれかに記載のアルミニウム
酸窒化物の製造方法。 S、諌酸化アルミニウム粉末O粒径が1声慣以下である
特許請求の範囲第1〜第3項のいずれかに記載のアルミ
−ラム酸窒化物の製造方法。
[Claims] 1. The method is characterized in that predetermined amounts of each powder of aluminum and aluminum oxide are blended, and the resulting mixed powder is fired at a temperature of 600 to 1200°C in an atmosphere containing nitrogen gas as the main component. A method for producing aluminum oxynitride. 2. The method for producing aluminum oxynitride according to claim 1, wherein the mixed powder contains wrinkled aluminum oxide in an amount of 50 to 85% by weight. 3. A part of the aluminum oxide is replaced with aluminum nitride having a particle size of 2 μm or less, and the total amount of the aluminum and the aluminum nitride exceeds 50% by weight based on the entire mixed powder in terms of aluminum weight. A method for producing aluminum oxynitride according to claim 1. 4. The method for producing aluminum oxynitride according to any one of claims 1 to 3, wherein the cough aluminum powder is flaky powder. 4. The method for producing an aluminum-ram oxynitride according to any one of claims 1 to 3, wherein the particle size of the aluminum sulfur oxide powder O is less than one tone diameter.
JP57014992A 1982-02-03 1982-02-03 Production of aluminum oxynitride Pending JPS58135112A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP57014992A JPS58135112A (en) 1982-02-03 1982-02-03 Production of aluminum oxynitride

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP57014992A JPS58135112A (en) 1982-02-03 1982-02-03 Production of aluminum oxynitride

Publications (1)

Publication Number Publication Date
JPS58135112A true JPS58135112A (en) 1983-08-11

Family

ID=11876431

Family Applications (1)

Application Number Title Priority Date Filing Date
JP57014992A Pending JPS58135112A (en) 1982-02-03 1982-02-03 Production of aluminum oxynitride

Country Status (1)

Country Link
JP (1) JPS58135112A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3538044A1 (en) * 1984-10-26 1986-04-30 Nikkei Kako K.K., Tokio/Tokyo Process for the manufacture of refractory aluminium oxynitride
US6955798B2 (en) * 2002-05-01 2005-10-18 Nanomat, Inc. Method for manufacturing aluminum oxynitride (AlON) powder and other nitrogen-containing powders
US7262145B2 (en) 2004-04-23 2007-08-28 Kennametal Inc. Whisker-reinforced ceramic containing aluminum oxynitride and method of making the same

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3538044A1 (en) * 1984-10-26 1986-04-30 Nikkei Kako K.K., Tokio/Tokyo Process for the manufacture of refractory aluminium oxynitride
FR2572393A1 (en) * 1984-10-26 1986-05-02 Nikkei Kako Kk Refractory aluminium oxy:nitride prodn.
US6955798B2 (en) * 2002-05-01 2005-10-18 Nanomat, Inc. Method for manufacturing aluminum oxynitride (AlON) powder and other nitrogen-containing powders
US7262145B2 (en) 2004-04-23 2007-08-28 Kennametal Inc. Whisker-reinforced ceramic containing aluminum oxynitride and method of making the same
US7309475B2 (en) * 2004-04-23 2007-12-18 Kennametal Inc. Whisker-reinforced ceramic containing aluminum oxynitride and method of making the same
US7368406B2 (en) 2004-04-23 2008-05-06 Kennametal Inc. Whisker-reinforced ceramic containing aluminum oxynitride and method of making the same

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