JPH04321505A - Production of aluminum nitride - Google Patents
Production of aluminum nitrideInfo
- Publication number
- JPH04321505A JPH04321505A JP9079291A JP9079291A JPH04321505A JP H04321505 A JPH04321505 A JP H04321505A JP 9079291 A JP9079291 A JP 9079291A JP 9079291 A JP9079291 A JP 9079291A JP H04321505 A JPH04321505 A JP H04321505A
- Authority
- JP
- Japan
- Prior art keywords
- aluminum
- metal
- aluminum nitride
- alloy
- aluminum metal
- 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 28
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 238000005121 nitriding Methods 0.000 claims abstract description 19
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 17
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 14
- 150000003624 transition metals Chemical class 0.000 claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 13
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 16
- 239000001301 oxygen Substances 0.000 abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 abstract description 16
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 36
- 229910045601 alloy Inorganic materials 0.000 description 13
- 239000000956 alloy Substances 0.000 description 13
- 239000002994 raw material Substances 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 8
- 229910001873 dinitrogen Inorganic materials 0.000 description 7
- 229910052727 yttrium Inorganic materials 0.000 description 6
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 6
- 239000012495 reaction gas Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- 229910052720 vanadium Inorganic materials 0.000 description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
- Ceramic Products (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は窒化アルミニウムの製造
方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing aluminum nitride.
【０００２】0002
【従来の技術】窒化アルミニウムは通常、電気炉内でア
ルミニウム金属を窒素を含む非酸化性雰囲気中で窒化し
て製造される。窒化率は、反応温度が高いほど、また反
応時間が長いほど向上するが、アルミニウム金属の融点
等を考慮して、最適な窒化条件は ６００〜１６００℃
、３０〜３００ 分間である。BACKGROUND OF THE INVENTION Aluminum nitride is usually produced by nitriding aluminum metal in a non-oxidizing atmosphere containing nitrogen in an electric furnace. The higher the reaction temperature and the longer the reaction time, the higher the nitriding rate, but considering the melting point of aluminum metal, etc., the optimal nitriding condition is 600 to 1600°C.
, 30 to 300 minutes.
【０００３】窒化アルミニウムの製造における重大な課
題は、前記した窒化条件を用いたとしても原料のアルミ
ニウム金属が完全に窒化されず、製造された窒化アルミ
ニウム中にアルミニウム金属が残留することである。製
造された窒化アルミニウム中にアルミニウム金属が残留
すると、反応ガス中の酸素と反応して形成された酸化物
が残留して、酸素含量の高い窒化アルミニウムが製造さ
れるという問題が生ずる。酸素含量の高い窒化アルミニ
ウムを焼結させても熱伝導率の低い焼結体しか得られな
いことは周知の通りである。A serious problem in the production of aluminum nitride is that even if the above-mentioned nitriding conditions are used, the raw aluminum metal is not completely nitrided, and the aluminum metal remains in the produced aluminum nitride. If aluminum metal remains in the produced aluminum nitride, an oxide formed by reacting with oxygen in the reaction gas remains, resulting in a problem that aluminum nitride with a high oxygen content is produced. It is well known that even if aluminum nitride with a high oxygen content is sintered, only a sintered body with low thermal conductivity can be obtained.
【０００４】原料のアルミニウム金属が完全に窒化され
ない原因は、アルミニウム金属の窒化反応は主にアルミ
ニウム金属の表面で起るため、金属表面に窒化アルミニ
ウムが生成されるとアルミニウム金属の内部にまで反応
ガスが浸透せず、アルミニウム金属の窒化反応が停止し
てしまうからである。このために、アルミニウム金属と
反応ガスとの接触面積をできるだけ大きくすべく、原料
として、アルミニウム金属を約１０〜５０μｍに粉砕し
て得た粉砕物または予め約１０〜５０μｍのサイズの粒
状に製造したアルミニウム金属粉が用いられている。し
かしながら、原料として上記したアルミニウム金属の粉
砕物またはアルミニウム金属粉を用いても、窒化アルミ
ニウム中に数重量％のアルミニウム金属が残留している
。The reason why the raw material aluminum metal is not completely nitrided is that the nitriding reaction of aluminum metal mainly occurs on the surface of the aluminum metal, so when aluminum nitride is formed on the metal surface, the reaction gas reaches the inside of the aluminum metal. This is because the aluminum metal does not penetrate and the nitriding reaction of aluminum metal stops. For this purpose, in order to increase the contact area between the aluminum metal and the reaction gas as much as possible, aluminum metal was used as a raw material by pulverizing it to about 10 to 50 μm, or a pulverized product obtained by grinding it to about 10 to 50 μm, or prepared in advance into granules with a size of about 10 to 50 μm. Aluminum metal powder is used. However, even if the above-mentioned pulverized aluminum metal or aluminum metal powder is used as a raw material, several weight percent of aluminum metal remains in aluminum nitride.
【０００５】また、原料としてアルミニウム金属の粉砕
物またはアルミニウム金属粉を用いた場合、粉砕時また
は貯蔵中にアルミニウム金属が酸化を受けて、生じた酸
化物が後の窒化反応を阻害する。また、前記酸化物が製
造された窒化アルミニウム中に残留物として存在し、そ
のため窒化アルミニウム中の酸素含量が高くなる問題も
生ずる。[0005] Furthermore, when pulverized aluminum metal or aluminum metal powder is used as a raw material, the aluminum metal is oxidized during pulverization or storage, and the resulting oxide inhibits the subsequent nitriding reaction. Furthermore, the problem arises that the oxide is present as a residue in the aluminum nitride produced, resulting in a high oxygen content in the aluminum nitride.
【０００６】窒化アルミニウムは、上記したアルミニウ
ム金属を非酸化性雰囲気中で窒化させる方法以外、プラ
ズマジェット法やアーク放電法によっても製造されるが
、いずれの方法においても製造された窒化アルミニウム
中にアルミニウム金属が残留する課題は解決され得ない
。Aluminum nitride can be produced by a plasma jet method or an arc discharge method, in addition to the above-mentioned method of nitriding aluminum metal in a non-oxidizing atmosphere. The problem of residual metal cannot be solved.
【０００７】[0007]
【発明が解決しようする課題】本発明の目的は、アルミ
ニウム金属の残留量の少なくかつ酸素含量も少ない窒化
アルミニウムを製造する方法を提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide a method for producing aluminum nitride with a small amount of residual aluminum metal and a low oxygen content.
【０００８】[0008]
【課題を解決するための手段および作用】上記した課題
を解決するために、本発明においては原料として遷移金
属を含むアルミニウム合金を使用することを特徴とする
。Means and Effects for Solving the Problems In order to solve the above problems, the present invention is characterized in that an aluminum alloy containing a transition metal is used as a raw material.
【０００９】本発明の窒化アルミニウム製造方法は、遷
移金属を含むアルミニウム合金を窒素ガスを含む非酸化
性雰囲気中で窒化することからなる。The method for producing aluminum nitride of the present invention comprises nitriding an aluminum alloy containing a transition metal in a non-oxidizing atmosphere containing nitrogen gas.
【００１０】本発明において原料として遷移金属を含む
アルミニウム合金を使用すると、アルミニウム合金中に
含まれる遷移金属によって反応ガスがアルミニウム金属
の内部にまで浸透し、窒化反応が金属表面で停止するこ
となく順次速やかに進行し、窒化率の高い窒化アルミニ
ウムが得られる。本発明によって製造された窒化アルミ
ニウム中のアルミニウム金属の残留量は数十ｐｐｍ以下
である。本発明において原料として使用されるアルミニ
ウム合金中の遷移金属としては、ニッケル、イットリウ
ム、タングステン、チタン、バナジウムが好ましく、よ
り好ましくはイットリウムである。遷移金属を２種類以
上添加した合金でも同様に窒化アルミニウム粉末が得ら
れる。本発明において原料として使用されるアルミニウ
ム合金中の遷移金属の量は、好ましくは ０．１〜３０
重量％、より好ましくは１〜１０重量％である。遷移金
属の量が ０．１重量％未満では所期の添加効果が達成
されず、１０重量％を越えると添加元素の酸化物を多量
に含む窒化アルミニウムが製造される。In the present invention, when an aluminum alloy containing a transition metal is used as a raw material, the transition metal contained in the aluminum alloy allows the reaction gas to penetrate into the interior of the aluminum metal, and the nitriding reaction occurs sequentially without stopping at the metal surface. The process progresses quickly and aluminum nitride with a high nitriding rate can be obtained. The amount of aluminum metal remaining in the aluminum nitride produced by the present invention is several tens of ppm or less. The transition metal in the aluminum alloy used as a raw material in the present invention is preferably nickel, yttrium, tungsten, titanium, or vanadium, and more preferably yttrium. Aluminum nitride powder can be obtained in the same way with an alloy containing two or more types of transition metals. The amount of transition metal in the aluminum alloy used as a raw material in the present invention is preferably 0.1 to 30
% by weight, more preferably 1 to 10% by weight. If the amount of transition metal is less than 0.1% by weight, the desired effect of addition cannot be achieved, and if it exceeds 10% by weight, aluminum nitride containing a large amount of oxide of the added element will be produced.
【００１１】本発明において原料として遷移金属を含む
アルミニウム合金を使用した場合、遷移金属は窒化反応
時に原料中の酸素と反応して酸化物を形成すると共に、
反応ガス中に微量の酸素が含まれている場合でもその酸
素と反応して酸化物を形成するが、形成された遷移金属
の酸化物は反応時に系外に排出されるので、窒化アルミ
ニウムの酸素含量が高くなることはない。遷移金属の酸
化物は、その種類によっては（例えば、Ｙ２ Ｏ３ 、
Ｖ２ Ｏ５ 、Ｎ：Ｏ）窒化アルミニウム中に残留する
が、この酸化物は窒化アルミニウムの焼結時に焼結助剤
として作用するので、焼結時に別の焼結助剤を全くもし
くは少量しか添加しなくてすむ。酸化物は窒化アルミニ
ウムに均一に分散存在しているので、より均質な焼結体
が得られる。In the present invention, when an aluminum alloy containing a transition metal is used as a raw material, the transition metal reacts with oxygen in the raw material during a nitriding reaction to form an oxide,
Even if the reaction gas contains a trace amount of oxygen, it will react with that oxygen to form an oxide, but the formed transition metal oxide will be discharged from the system during the reaction, so the oxygen in aluminum nitride will react with the oxygen and form an oxide. The content will not be high. Depending on the type of transition metal oxide (for example, Y2 O3,
V2 O5, N:O) remains in aluminum nitride, but since this oxide acts as a sintering aid during sintering of aluminum nitride, no or only a small amount of another sintering aid is added during sintering. I don't need it. Since the oxide is uniformly dispersed in the aluminum nitride, a more homogeneous sintered body can be obtained.
【００１２】本発明においては遷移金属によって窒化反
応が速やかに進行するので、原料としてのアルミニウム
合金は微細な形状を有していなくてもよく、数ｍｍ程度
の塊状のアルミニウム合金を原料として使用することも
できる。しかしながら、原料として微細な形状を有する
アルミニウム合金を使用する方が窒化反応がより速かに
進行する。[0012] In the present invention, since the nitriding reaction proceeds rapidly with the transition metal, the aluminum alloy as a raw material does not need to have a fine shape, and a lumpy aluminum alloy of about several mm in size is used as a raw material. You can also do that. However, the nitriding reaction proceeds more quickly when an aluminum alloy having a fine shape is used as a raw material.
【００１３】本発明における窒化反応の条件は従来と同
様である。窒化反応は窒素を含む非酸化性雰囲気中で実
施され、主に窒素ガスが使用されるが、窒素ガスに他の
ガス、例えばアンモニアガス、アルゴンガスを組合せて
もよい。また、非酸化性雰囲気中に０．０３％程度の微
量ならば酸素が含まれていてもよい。反応温度は通常、
６００〜１６００℃である。反応時間は窒化反応が速
やかに進行するので、１０〜１００ 分位短縮すること
もできる。The conditions for the nitriding reaction in the present invention are the same as those in the prior art. The nitriding reaction is carried out in a non-oxidizing atmosphere containing nitrogen, and nitrogen gas is mainly used, but nitrogen gas may be combined with other gases such as ammonia gas and argon gas. Further, oxygen may be contained in a trace amount of about 0.03% in the non-oxidizing atmosphere. The reaction temperature is usually
The temperature is 600-1600°C. Since the nitriding reaction proceeds rapidly, the reaction time can be shortened by about 10 to 100 minutes.
【００１４】[0014]
【実施例】以下、本発明の非限定的実施例を示す。EXAMPLES Non-limiting examples of the present invention are shown below.
【００１５】実施例１
純度９９．９９ ％のアルミニウム金属にニッケル、イ
ットリウム、タングステン、バナジウムの各金属を ３
重量％添加したアルミニウム合金を用いて、直径１０ｍ
ｍ、高さ ５ｍｍの円柱状の合金サンプルを作成した。
この合金サンプルを純度９９．９％のアルミナ製のボー
トに載置し、カーボン製の電気炉内に配置し、電気炉内
に窒素ガスを流しながら１１００℃で４時間反応させて
窒化生成物を得た。また、合金サンプルの代りに純度９
９．９９ ％のアルミニウム金属を用い、該金属に同一
条件下で反応させて得た窒化生成物を対照とした。Example 1 Three metals of nickel, yttrium, tungsten, and vanadium were added to aluminum metal with a purity of 99.99%.
Diameter 10m using aluminum alloy with wt% addition
A cylindrical alloy sample with a height of 5 mm and a height of 5 mm was prepared. This alloy sample was placed on a 99.9% pure alumina boat, placed in a carbon electric furnace, and reacted at 1100°C for 4 hours while flowing nitrogen gas into the electric furnace to remove nitrided products. Obtained. Also, instead of the alloy sample, purity 9
A nitrided product obtained by reacting 9.99% aluminum metal under the same conditions was used as a control.
【００１６】得られた生成物をＸ線分析したところ、い
ずれも窒化アルミニウムとして確認された。生成物中の
アルミニウム金属の残留量を化学分析した結果および酸
素含量を機器分析（堀場製作所製ＥＭＧＡ−２８００）
した結果を表１に示す。結果はすべて試料３個の平均値
である。When the obtained products were subjected to X-ray analysis, they were all confirmed to be aluminum nitride. Results of chemical analysis of residual amount of aluminum metal in the product and instrumental analysis of oxygen content (EMGA-2800 manufactured by Horiba, Ltd.)
The results are shown in Table 1. All results are average values of three samples.
【００１７】[0017]
【表１】[Table 1]
【００１８】実施例２
純度９９．９９ ％のアルミニウム金属にイットリウム
金属を３０，２０，１５， ５， １，０．１ 重量％
添加したアルミニウム合金を用いて、直径１０ｍｍ、高
さ ５ｍｍの円柱状の合金サンプルを作成した。この合
金サンプルを純度９９．９％のアルミナ製のボートに載
置し、カーボン製の電気炉内に配置し、電気炉内に窒素
ガスを流しながら１２００℃で３時間反応させて窒化生
成物を得た。また、合金サンプルの代りに純度９９．９
９ ％のアルミニウム金属を用い、該金属に同一条件下
で反応させて得た窒化生成物を対照とした。Example 2 30, 20, 15, 5, 1, and 0.1% by weight of yttrium metal in aluminum metal with a purity of 99.99%
A cylindrical alloy sample with a diameter of 10 mm and a height of 5 mm was created using the added aluminum alloy. This alloy sample was placed on a boat made of 99.9% pure alumina, placed in a carbon electric furnace, and reacted at 1200°C for 3 hours while flowing nitrogen gas into the electric furnace to remove nitrided products. Obtained. Also, instead of alloy samples, purity 99.9
The control was a nitrided product obtained by reacting 9% aluminum metal under the same conditions.
【００１９】得られた生成物をＸ線分析したところ、い
ずれも窒化アルミニウムとして確認された。生成物中の
アルミニウム金属の残留量を化学分析した結果および酸
素含量を機器分析（堀場製作所製ＥＭＧＡ−２８００）
した結果を表２に示す。結果はすべて試料３個の平均値
である。When the obtained products were subjected to X-ray analysis, they were all confirmed to be aluminum nitride. Results of chemical analysis of residual amount of aluminum metal in the product and instrumental analysis of oxygen content (EMGA-2800 manufactured by Horiba, Ltd.)
The results are shown in Table 2. All results are average values of three samples.
【００２０】[0020]
【表２】[Table 2]
【００２１】実施例３
純度９９．９９ ％のアルミニウム金属にニッケル、イ
ットリウム、タングステン、バナジウムの各金属を ３
重量％添加したアルミニウム合金を用いて、粒子サイズ
が １ｍｍ以下の粉末状の合金サンプルを作成した。こ
の合金サンプル１０ｇを純度９９．９％のアルミナ製の
ボートに載置し、カーボン製の電気炉内に配置し、電気
炉内に窒素ガスを流しながら１０００℃で２時間反応さ
せて窒化生成物を得た。
また、合金サンプルの代りに純度９９．９９ ％のアル
ミニウム金属を用い、該金属に同一条件下で反応させて
得た窒化生成物を対照とした。Example 3 Three metals of nickel, yttrium, tungsten, and vanadium were added to aluminum metal with a purity of 99.99%.
Powdered alloy samples with a particle size of 1 mm or less were prepared using the aluminum alloy to which % by weight was added. 10 g of this alloy sample was placed on a 99.9% pure alumina boat, placed in a carbon electric furnace, and reacted at 1000°C for 2 hours while flowing nitrogen gas into the electric furnace to form a nitrided product. I got it. In addition, aluminum metal with a purity of 99.99% was used instead of the alloy sample, and a nitrided product obtained by reacting the metal under the same conditions was used as a control.
【００２２】得られた生成物をＸ線分析したところ、い
ずれも窒化アルミニウムとして確認された。生成物中の
アルミニウム金属の残留量を化学分析した結果および酸
素含量を機器分析（堀場製作所製ＥＭＧＡ−２８００）
した結果を表３に示す。結果はすべて試料３個の平均値
である。When the obtained products were subjected to X-ray analysis, they were all confirmed to be aluminum nitride. Results of chemical analysis of residual amount of aluminum metal in the product and instrumental analysis of oxygen content (EMGA-2800 manufactured by Horiba, Ltd.)
The results are shown in Table 3. All results are average values of three samples.
【００２３】[0023]
【表３】[Table 3]
【００２４】実施例４
純度 ９９．９９％のアルミニウム金属にニッケル、イ
ットリウム、タングステン、バナジウムの各金属を ２
重量％添加したアルミニウム合金を用いて、直径１０ｍ
ｍ、高さ ５ｍｍの円柱状の合金サンプルを作成した。
この合金サンプルを純度９９．９％のアルミナ製のボー
トに載置し、カーボン製の電気炉内に配置し、電気炉内
に窒素ガスを流しながら ９００℃で ０．５、 １、
２．５、 ５、１０時間反応させて窒化生成物を得た
。また、合金サンプルの代りに純度９９．９９ ％のア
ルミニウム金属を用い、該金属に同一条件下で反応させ
て得た窒化生成物を対照とした。Example 4 Each metal of nickel, yttrium, tungsten, and vanadium was added to aluminum metal with a purity of 99.99%.
Diameter 10m using aluminum alloy with wt% addition
A cylindrical alloy sample with a height of 5 mm and a height of 5 mm was prepared. This alloy sample was placed on a boat made of alumina with a purity of 99.9%, placed in a carbon electric furnace, and heated at 900°C while flowing nitrogen gas into the electric furnace.
The reaction was carried out for 2.5, 5 and 10 hours to obtain nitrided products. In addition, aluminum metal with a purity of 99.99% was used instead of the alloy sample, and a nitrided product obtained by reacting the metal under the same conditions was used as a control.
【００２５】得られた生成物をＸ線分析したところ、い
ずれも窒化アルミニウムとして確認された。生成物中の
アルミニウム金属の残留量を化学分析した結果を表４、
酸素含量を機器分析（堀場製作所製ＥＭＧＡ−２８００
）した結果を表５に示す。結果はすべて試料３個の平均
値である。When the obtained products were subjected to X-ray analysis, they were all confirmed to be aluminum nitride. Table 4 shows the results of chemical analysis of the residual amount of aluminum metal in the product.
Instrumental analysis of oxygen content (EMGA-2800 manufactured by Horiba)
) The results are shown in Table 5. All results are average values of three samples.
【００２６】[0026]
【表４】[Table 4]
【００２７】[0027]
【表５】[Table 5]
Claims (1)
素を含む非酸化性雰囲気中で窒化することを特徴とする
窒化アルミニウムの製造方法。1. A method for producing aluminum nitride, which comprises nitriding an aluminum alloy containing a transition metal in a non-oxidizing atmosphere containing nitrogen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9079291A JPH04321505A (en) | 1991-04-22 | 1991-04-22 | Production of aluminum nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9079291A JPH04321505A (en) | 1991-04-22 | 1991-04-22 | Production of aluminum nitride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04321505A true JPH04321505A (en) | 1992-11-11 |
Family
ID=14008438
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9079291A Pending JPH04321505A (en) | 1991-04-22 | 1991-04-22 | Production of aluminum nitride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04321505A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6159439A (en) * | 1996-12-26 | 2000-12-12 | Toyota Jidosha Kabushiki Kaisha | Process for producing aluminum nitride |
| CN102295276A (en) * | 2011-06-14 | 2011-12-28 | 西安理工大学 | Method for preparing porous aluminium nitride particle or porous gallium nitride particle by two-step nitridation method |
| WO2015182477A1 (en) * | 2014-05-30 | 2015-12-03 | 国立大学法人名古屋大学 | Aln crystal preparation method, aln crystals, and organic compound including aln crystals |
-
1991
- 1991-04-22 JP JP9079291A patent/JPH04321505A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6159439A (en) * | 1996-12-26 | 2000-12-12 | Toyota Jidosha Kabushiki Kaisha | Process for producing aluminum nitride |
| CN102295276A (en) * | 2011-06-14 | 2011-12-28 | 西安理工大学 | Method for preparing porous aluminium nitride particle or porous gallium nitride particle by two-step nitridation method |
| WO2015182477A1 (en) * | 2014-05-30 | 2015-12-03 | 国立大学法人名古屋大学 | Aln crystal preparation method, aln crystals, and organic compound including aln crystals |
| JPWO2015182477A1 (en) * | 2014-05-30 | 2017-04-20 | 国立大学法人名古屋大学 | Method for producing AlN crystal, AlN crystal, and organic compound containing AlN crystal |
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