JPH01100007A - Production of aluminum nitride with cubic system - Google Patents
Production of aluminum nitride with cubic systemInfo
- Publication number
- JPH01100007A JPH01100007A JP25464987A JP25464987A JPH01100007A JP H01100007 A JPH01100007 A JP H01100007A JP 25464987 A JP25464987 A JP 25464987A JP 25464987 A JP25464987 A JP 25464987A JP H01100007 A JPH01100007 A JP H01100007A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- gas
- aluminum nitride
- aluminum
- mixture
- 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
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000007789 gas Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000011812 mixed powder Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 abstract description 5
- 239000011261 inert gas Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000008020 evaporation Effects 0.000 abstract description 2
- 238000001704 evaporation Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 229910052782 aluminium Inorganic materials 0.000 description 9
- 239000013078 crystal Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 238000010891 electric arc Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- -1 aluminum halide Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
- C01B21/0722—Preparation by direct nitridation of aluminium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は立方晶窒化アルミニウムの製造方法に関し、詳
しくはアルミニウム粉末等を原料として、これをアンモ
ニアガス雰囲気中あるいは窒素ガスとアンモニアガスと
の混合ガス雰囲気中で加熱処理することによって、熱伝
導率および硬度等のすぐれた立方晶窒化アルミニウムを
製造する方法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing cubic aluminum nitride, and more specifically, the present invention relates to a method for producing cubic aluminum nitride, and more specifically, using aluminum powder as a raw material, it is produced in an ammonia gas atmosphere or in a mixture of nitrogen gas and ammonia gas. The present invention relates to a method for producing cubic aluminum nitride with excellent thermal conductivity, hardness, etc. by heat treatment in a gas atmosphere.
〔従来の技術及び発明が解決しようとする問題点〕従来
から、窒化アルミニウム（ＡｆＮ）を製造する方法とし
ては、アルミニウムの直接窒化法、酸化アルミニウムの
炭素還元窒化法、ハロゲン化アルミニウムとアンモニア
の気相反応による方法、窒素ガス雰囲気下での直流アー
クプラズマ法などが知られている。[Prior art and problems to be solved by the invention] Conventionally, methods for producing aluminum nitride (AfN) include direct nitriding of aluminum, carbon reduction nitriding of aluminum oxide, and oxidation of aluminum halide and ammonia. A method using a phase reaction, a direct current arc plasma method under a nitrogen gas atmosphere, etc. are known.
しかしながら、これらの方法によって得られる窒化アル
ミニウムは、いずれも六方晶系のものであり、立方晶窒
化アルミニウムは製造することができなかった。However, the aluminum nitride obtained by these methods is all hexagonal, and cubic aluminum nitride could not be produced.
そこで本発明者らは、熱伝導率や硬度等のすぐれた立方
晶窒化アルミニウムを効率よく製造することのできる方
法を開発すべく鋭意研究を重ねた。Therefore, the present inventors have conducted extensive research in order to develop a method that can efficiently produce cubic aluminum nitride with excellent thermal conductivity and hardness.
その結果、アルミニウム粉末等を、アンモニアガス雰囲
気中あるいは窒素ガスにアンモニアガスを混合した混合
ガス雰囲気中で加熱処理することにより、目的を達成し
うることを見出し、本発明を完成するに至った。As a result, the inventors discovered that the object could be achieved by heat-treating aluminum powder or the like in an ammonia gas atmosphere or a mixed gas atmosphere of nitrogen gas and ammonia gas, thereby completing the present invention.
すなわち本発明は、アルミニウム粉末、六方晶窒化アル
ミニウム粉末あるいはこれらの混合粉末を、アンモニア
ガス雰囲気中あるいは窒素ガスとアンモニアガスとの混
合ガス雰囲気中で加熱処理することを特徴とする立方晶
窒化アルミニウムの製造方法を提供するものである。That is, the present invention provides a method for producing cubic aluminum nitride, which is characterized in that aluminum powder, hexagonal aluminum nitride powder, or a mixed powder thereof is heat-treated in an ammonia gas atmosphere or a mixed gas atmosphere of nitrogen gas and ammonia gas. A manufacturing method is provided.
本発明では、アルミニウム粉末、窒化アルミニウム粉末
（六方晶）あるいはこれらの混合粉末を原料として用い
る。これら原料粉末は、各種公知の方法によって得られ
るものを使用することができ、特に制限はないが、その
粒子径が１．０μｍ以下、とりわけ０．４μｍ以下のも
のが好ましい。In the present invention, aluminum powder, aluminum nitride powder (hexagonal crystal), or a mixed powder thereof is used as a raw material. These raw material powders can be obtained by various known methods, and are not particularly limited, but preferably have a particle size of 1.0 μm or less, particularly 0.4 μm or less.
このような粒子径が１．０μｍ以下の原料粉末は、直流
アークプラズマ法によって効率よく得ることができる。Such raw material powder having a particle size of 1.0 μm or less can be efficiently obtained by a DC arc plasma method.
ここで直流アークプラズマ法は、従来から知られている
手法であり、基本的には塊状のアルミニウムを陽極であ
る銅板上にのせ、タングステンなどの陰極との間にアー
クプラズマを発生させ、アルミニウムを溶融、強制蒸発
させることによってアルミニウムーの粉末（微粒子）を
得るものである。このアーク放電を、窒素ガス雰囲気下
あるいは窒素ガスとアンモニアガスとの混合ガス雰囲気
下で行えば、アルミニウム微粒子と窒素プラズマ等との
反応により窒化アルミニウム（六方晶）が生成し、窒化
アルミニウム粉末あるいはこれとアルミニウム粉末との
混合粉末が得られる。The DC arc plasma method is a conventionally known method. Basically, a lump of aluminum is placed on a copper plate as an anode, and an arc plasma is generated between it and a cathode made of tungsten, etc. Aluminum powder (fine particles) is obtained by melting and forced evaporation. If this arc discharge is performed in a nitrogen gas atmosphere or a mixed gas atmosphere of nitrogen gas and ammonia gas, aluminum nitride (hexagonal crystal) is generated by the reaction between aluminum fine particles and nitrogen plasma, etc., and aluminum nitride powder or this A mixed powder of aluminum powder and aluminum powder is obtained.
なお、このアーク放電は、このほか不活性ガス。In addition, this arc discharge also uses inert gas.
水素ガスあるいはこれらの混合ガスの雰囲気下で行うこ
ともできる。また、雰囲気ガス圧はアーク放電が可能な
圧力であれば特に制限はない。It can also be carried out in an atmosphere of hydrogen gas or a mixture of these gases. Further, there is no particular restriction on the atmospheric gas pressure as long as it is a pressure that allows arc discharge.
本発明の方法では、このようにして得られたアルミニウ
ム粉末、窒化アルミニウム（但し、六方晶構造）粉末あ
るいはこれらの混合粉末を用い、これをアンモニアガス
雰囲気中あるいは窒素ガスとアンモニアガスの混合ガス
雰囲気中で加熱処理する。なお、雰囲気中にアンモニア
ガスが存在しないと、加熱処理しても立方晶構造の窒化
アルミニウムを得ることはできない。In the method of the present invention, the thus obtained aluminum powder, aluminum nitride (hexagonal crystal structure) powder, or a mixed powder thereof is used, and is heated in an ammonia gas atmosphere or a mixed gas atmosphere of nitrogen gas and ammonia gas. heat-treated inside. Note that unless ammonia gas is present in the atmosphere, aluminum nitride having a cubic crystal structure cannot be obtained even by heat treatment.
また、本発明の方法では、上記雰囲気中で加熱処理する
が、この際の加熱温度は各種状況により異なるが、一般
には５００〜９００℃、好ましくは７５０〜８５０℃で
ある。Further, in the method of the present invention, heat treatment is performed in the above atmosphere, and the heating temperature at this time varies depending on various circumstances, but is generally 500 to 900°C, preferably 750 to 850°C.
本発明の方法では、他の条件は特に制限はな（適宜型め
ればよい０例えば加熱処理時間は、温度等によっても異
なるが、−殻内には３〜３０時間である。また、雰囲気
ガス全圧は通常は１００〜１０００ Ｔｏｒｒであり、
必要に応じて不活性ガス等を希釈ガスとして加えること
もできる。In the method of the present invention, other conditions are not particularly limited (they may be set as appropriate).For example, the heat treatment time varies depending on the temperature, etc. The total gas pressure is usually 100 to 1000 Torr,
An inert gas or the like can also be added as a diluent gas, if necessary.
次に、本発明を実施例および比較例により更に詳しく説
明する。Next, the present invention will be explained in more detail with reference to Examples and Comparative Examples.
実施例１〜７および比較例１．２
（１）窒化アルミニウム（六方晶）粉末とアルミニウム
粉末の混合粉末の調製
第２図に示す装置を用い、純度９９．９９％のアルミニ
ウム塊１と電極２との間に直流アークプラズマを発生さ
せて、このアルミニウム塊１を溶融させて蒸気化し、窒
化アルミニウム（六方晶）粉末とアルミニウム粉末の混
合粉末（平均粒径０．２ａｍ）（窒化アルミニウム：ア
ルミニウムー３ニア（重量比））を得た。なお、上述の
直流アークプラズマを発生させるにあたっては、アーク
電流を１３ＯＡとし、また窒素ガスボンベ３から導入す
る窒素ガス流量は３０Ｅ／分であった。Examples 1 to 7 and Comparative Example 1.2 (1) Preparation of mixed powder of aluminum nitride (hexagonal crystal) powder and aluminum powder Using the apparatus shown in FIG. 2, aluminum ingot 1 with a purity of 99.99% and electrode 2 were prepared. A direct current arc plasma is generated between the aluminum ingot 1 and the aluminum ingot 1 to be melted and vaporized to form a mixed powder (average particle size 0.2 am) of aluminum nitride (hexagonal crystal) powder and aluminum powder (aluminum nitride: aluminum). 3 (weight ratio)) was obtained. In generating the above-mentioned DC arc plasma, the arc current was 13 OA, and the flow rate of nitrogen gas introduced from the nitrogen gas cylinder 3 was 30 E/min.
（２）立方晶窒化アルミニウムの製造
上記（１）で得られた窒化アルミニウム（六方晶）粉末
とアルミニウム粉末の混合粉末を原料として、これを第
１表に示す条件で加熱処理して、立方晶窒化アルミニウ
ムの製造を行った。結果を第１表に示す。なお、実施例
５で得られた立方晶窒化アルミニウムのＸ線回折パター
ンを第１図に示す。(2) Production of cubic aluminum nitride The mixed powder of the aluminum nitride (hexagonal) powder and aluminum powder obtained in (1) above was used as a raw material and was heat-treated under the conditions shown in Table 1 to form a cubic aluminum nitride. Manufactured aluminum nitride. The results are shown in Table 1. The X-ray diffraction pattern of the cubic aluminum nitride obtained in Example 5 is shown in FIG.
叙上の如（、本発明の方法によれば、簡単な操作でしか
も効率よく立方晶窒化アルミニウムを製造することがで
きる。また、この方法で製造された立方晶窒化アルミニ
ウムは、従来の六方晶のものに比べて熱伝導率や硬度等
の物理的９機械的特性がすぐれており、集積回路（ＩＣ
）用基板等の電子工学材料、さらには構造材料などに幅
広く、かつ有効に利用される。As mentioned above, according to the method of the present invention, cubic aluminum nitride can be produced efficiently with simple operations.Also, the cubic aluminum nitride produced by this method is different from the conventional hexagonal aluminum nitride. It has superior physical and mechanical properties such as thermal conductivity and hardness compared to those of integrated circuits (ICs).
) It is widely and effectively used in electronic engineering materials such as substrates, as well as structural materials.
第１図は実施例５で得られた立方晶窒化アルミニウムの
Ｘ線回折パターンを示し、第２図は実施例で用いた直流
アークプラズマの発生装置の説明図である。
第１図中、θはブラッグ角を示す。また第２図中、１は
アルミニウム塊、２は電極、３は窒素ボンベ、４はアル
ゴンボンベ、５は電源、６はハース、７はグローブボッ
クス、８はサイクロン、９はフィルター、１０は循環ポ
ンプをそれぞれ示す。FIG. 1 shows the X-ray diffraction pattern of the cubic aluminum nitride obtained in Example 5, and FIG. 2 is an explanatory diagram of the DC arc plasma generator used in the example. In FIG. 1, θ indicates the Bragg angle. In Figure 2, 1 is an aluminum block, 2 is an electrode, 3 is a nitrogen cylinder, 4 is an argon cylinder, 5 is a power source, 6 is a hearth, 7 is a glove box, 8 is a cyclone, 9 is a filter, and 10 is a circulation pump. are shown respectively.
Claims (4)
あるいはこれらの混合粉末を、アンモニアガス雰囲気中
あるいは窒素ガスとアンモニアガスとの混合ガス雰囲気
中で加熱処理することを特徴とする立方晶窒化アルミニ
ウムの製造方法。(1) A method for producing cubic aluminum nitride, which comprises heat-treating aluminum powder, hexagonal aluminum nitride powder, or a mixed powder thereof in an ammonia gas atmosphere or a mixed gas atmosphere of nitrogen gas and ammonia gas. .
あるいはこれらの混合粉末が、粒子径１．０μｍ以下の
ものである特許請求の範囲第１項記載の製造方法。(2) The manufacturing method according to claim 1, wherein the aluminum powder, hexagonal aluminum nitride powder, or a mixed powder thereof has a particle size of 1.0 μm or less.
あるいはこれらの混合粉末が、直流アークプラズマ法に
よって得られたものである特許請求の範囲第１項記載の
製造方法。(3) The manufacturing method according to claim 1, wherein the aluminum powder, hexagonal aluminum nitride powder, or a mixed powder thereof is obtained by a direct current arc plasma method.
範囲第１項記載の製造方法。(4) The manufacturing method according to claim 1, wherein the heat treatment is performed at 500 to 900°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25464987A JPH01100007A (en) | 1987-10-12 | 1987-10-12 | Production of aluminum nitride with cubic system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25464987A JPH01100007A (en) | 1987-10-12 | 1987-10-12 | Production of aluminum nitride with cubic system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01100007A true JPH01100007A (en) | 1989-04-18 |
Family
ID=17267950
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25464987A Pending JPH01100007A (en) | 1987-10-12 | 1987-10-12 | Production of aluminum nitride with cubic system |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01100007A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211025A (en) * | 2014-08-29 | 2014-12-17 | 中国计量学院 | Preparation method of cubic phase aluminum nitride fiber |
| JP2015151307A (en) * | 2014-02-14 | 2015-08-24 | 株式会社アテクト | Alumina sintered compact and method for producing the same |
-
1987
- 1987-10-12 JP JP25464987A patent/JPH01100007A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015151307A (en) * | 2014-02-14 | 2015-08-24 | 株式会社アテクト | Alumina sintered compact and method for producing the same |
| US9464221B2 (en) * | 2014-02-14 | 2016-10-11 | Atect Corporation | Alumina sintered body and method for producing same |
| CN104211025A (en) * | 2014-08-29 | 2014-12-17 | 中国计量学院 | Preparation method of cubic phase aluminum nitride fiber |
| CN104211025B (en) * | 2014-08-29 | 2016-01-20 | 中国计量学院 | A kind of preparation method of Emission in Cubic aluminium nitride fibres |
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