JPH0466807B2 - - Google Patents
Info
- Publication number
- JPH0466807B2 JPH0466807B2 JP21419987A JP21419987A JPH0466807B2 JP H0466807 B2 JPH0466807 B2 JP H0466807B2 JP 21419987 A JP21419987 A JP 21419987A JP 21419987 A JP21419987 A JP 21419987A JP H0466807 B2 JPH0466807 B2 JP H0466807B2
- Authority
- JP
- Japan
- Prior art keywords
- aluminum nitride
- precursor
- powder
- ammonia
- nitride powder
- 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
Links
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 41
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 27
- 239000002243 precursor Substances 0.000 claims description 26
- 229910021529 ammonia Inorganic materials 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims 1
- 238000000034 method Methods 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 5
- 238000005121 nitriding Methods 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 125000005234 alkyl aluminium group Chemical group 0.000 description 2
- -1 aluminum compound Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- MCULRUJILOGHCJ-UHFFFAOYSA-N triisobutylaluminium Chemical compound CC(C)C[Al](CC(C)C)CC(C)C MCULRUJILOGHCJ-UHFFFAOYSA-N 0.000 description 2
- LQIIEHBULBHJKX-UHFFFAOYSA-N 2-methylpropylalumane Chemical compound CC(C)C[AlH2] LQIIEHBULBHJKX-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- HJXBDPDUCXORKZ-UHFFFAOYSA-N diethylalumane Chemical compound CC[AlH]CC HJXBDPDUCXORKZ-UHFFFAOYSA-N 0.000 description 1
- YNLAOSYQHBDIKW-UHFFFAOYSA-M diethylaluminium chloride Chemical compound CC[Al](Cl)CC YNLAOSYQHBDIKW-UHFFFAOYSA-M 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Description
〔産業上の利用分野〕
本発明は高純度窒化アルミニウム粉の製造法に
関する。窒化アルミニウムは電子機器材料用セラ
ミツクとして注目されているが、本発明は特に球
形に近くかつ酸素および炭素が極めて少なく成形
性に優れた高純度窒化アルミニウム粉を大量に提
供する製造法に関するものである。
〔従来の技術〕
窒化アルミニウム粉の製造法としては、金属ア
ルミニウムに窒素またはアンモニアを直接反応さ
せる直接窒化法と、アルミナとカーボンの混合粉
末を窒素含有雰囲気下で焼成する還元窒化法およ
び有機アルミニウム化合物とアンモニアまたは一
級あるいは二級アミン類と反応させて窒化アルミ
ニウム前駆体を調製した後、該前駆体を不活性ガ
ス、真空下あるいはアンモニア気流下に焼成する
方法（特開昭53−68700号）が知られている。
しかしながら直接窒化法および還元窒化法では
原料に起因する不純物、特に酸素が混在し易いた
めに焼結体の熱伝導率は低下する。また特開昭53
−68700号に開示されている窒化アルミニウム前
駆体を焼成して窒化アルミニウムとする方法にお
いては、生成する前駆体は均一核生成によると推
察される非常に微細な粒子の凝集体であるためそ
の形状にはほど遠く不定形であり、粒度分布が広
く、また粒径は十数ミクロンから数十ミクロンと
大きい。かような前駆体を焼成して得られる窒化
アルミニウム粉の形状は前駆体のレプリカであ
り、それ故窒化アルミニウム粉の成形密度は低
い。このため焼成後に解砕または粉砕工程を不可
欠とするうえに、該処理により活性面が形成され
るため酸素および水と反応し易くなり結果的には
酸素およびカチオン不純物が更に増加するという
致命的欠陥を有している。
〔発明が解決しようとする問題点〕
そこで本発明者らは有機アルミニウム化合物を
出発原料とする方法において酸素および炭素が少
なくしかも成形性の優れた高純度窒化アルミニウ
ム粉の製造法について種々研究の結果、新規な製
造法を見い出し本発明に至つたものである。
〔問題点を解決するための手段〕
そこでさらに鋭意研究を重ねた結果、平均粒径
1μm以下の窒化アルミニウム前駆体およびまたは
窒化アルミニウム粉末を、生成する窒化アルミニ
ウム前駆体に対し0.1〜10重量％含む高純度有機
アルミニウム溶液にアンモニアを130℃以上で反
応させることによつて沈澱した窒化アルミニウム
前駆体は、凝集がなくしかもその形状は球状に近
いという事実を発見した。該前駆体の生成機構に
ついては詳しく分らないが種子表面で核生成が起
り続いて成長するため核同士の合一がないものと
推察される。
この様にして得られた窒化アルミニウム前駆体
をアンモニア気流下400〜1100℃の温度範囲に一
定時間保持し、さらに不活性ガス気流下1100〜
1600℃の温度域で焼成すれば球状に近く解砕を必
要としない。しかも酸素および炭素の極めて少な
い成形性に優れた高純度窒化アルミニウム粉が得
られることを発見し本発明を完成するに至つた。
以下詳しく説明すると、有機アルミニウム化合
物としては、トリアルキルアルミニウム，ジアル
キルアルミニウムハイドライド，ジアルキルアル
ミニウムハライド，アルキルアルミニウムジハラ
イド，アルキルアルミニウムセスキハライドであ
り、具体的にはトリメチルアルミニウム，トリエ
チルアルミニウム，トリイソブチルアルミニウ
ム，ジエチルアルミニウムハイドライド，ジエチ
ルアルミニウムクロライド，イソブチルアルミニ
ウムセスキクロライド等であるが、経済面からト
リエチルアルミニウムあるいはトリイソブチルア
ルミニウムの使用が有利である。
反応にあたつては有機アルミニウム化合物はキ
シレン，ケロシン，デカン，テトラリン等の溶媒
で希釈し20重量％程度の溶液として使用する。
有機アルミニウム化合物溶液に添加する種子と
しては窒化アルミニウム前駆体粉末およびまたは
窒化アルミニウム粉末が使用できるが、粒径はい
ずれも1μm以下が好ましい。窒化アルミニウム前
駆体粉末としては有機アルミニウム化合物とアン
モニアまたは有機アミン類を適当な条件下に反応
させて得られる窒化アルミニウム前駆体をボール
ミルまたは振動ミル等で粉砕したものが、また窒
化アルミニウム粉末としては本発明者らが先に提
案した特願昭61−203463号（特公平４−8364号公
報参照）により容易に得られる気相法窒化アルミ
ニウム粉末および市販窒化アルミニウム粉末が好
適に用いられる。該粉末の添加量であるが、添加
量が多い程、窒化アルミニウム粉の粒径は小さく
なるが、10重量％以上では再凝集し0.1重量％以
下では顕著な効果が認められないために0.1〜10
重量％好ましく１〜５重量％が適当である。また
有機アルミニウム化合物とアンモニアは適当な攪
拌のもとに反応させることが必要である。反応温
度は130℃以下では窒化アルミニウム前駆体の収
率が低下するばかりか過性が悪くなる。130℃
以上であれば特に制限はないが、使用する溶媒の
沸点を考慮すると130〜250℃が適当である。
焼成は非酸化性ガス気流下に実施する。
雰囲気ガスとしては窒素，アルゴン等の不活性
ガス、アンモニア，水素等の還元性ガス単独ある
いはこれらの混合ガスを用いることが可能である
が、窒化アルミニウム粉の炭素量を少なくするた
めにはアンモニアが好ましく400〜1100℃の温度
範囲で0.5〜４時間保持することが望ましい。400
℃以下では有機残基の分解が遅く長時間を要し、
また1100℃以上ではアンモニアの分解が著しいた
め経済的でない。かかる焼成により炭素量の少な
い窒化アルミニウムが得られるが、さらに不活性
ガス気流下1100〜1600℃の温度域で適当な時間保
持することにより空気中で安定な窒化アルミニウ
ム粉となる。1600℃以上では窒化アルミニウムの
焼結が起り硬化するため好ましくない。
〔実施例〕
以下実施例をあげてさらに具体的に説明する。
実施例 １
トリエチルアルミニウムの20重量％ｎ−デカン
溶液を170℃に保ちアンモニアと反応させること
により窒化アルニウム前駆体を合成した。この前
駆体20ｇを350mlのｎ−デカン中に投入し振動ミ
ルで１時間粉砕し平均粒径0.5μmの前駆体スラリ
ーを得た。
次に、トリエチルアルミニウムの15重量％ｎ−
デカン溶液2.1に先に調製したスラリー35mlを
添加した。ついで155℃に加熱し攪拌下反応器気
相部にアンモニアを導入した。アンモニアをトリ
エチルアルミニウムに対して1.2当量導入した時
点で反応器内温度は低下し始め沈澱が析出したこ
とを示した。本実施例では種子として添加した窒
化アルミニウム前駆体の量は生成した当該窒化ア
ルミニウム前駆体に対し1.3重量％に相当する。
反応終了後生成した白色沈澱を別し減圧下に
乾燥して窒化アルミニウム前駆体を得た。
この粉末250ｇをカーボン皿にとりアンモニア
気流下1000℃まで加熱し２時間保持した後、雰囲
気ガスを窒素に代え1500℃で４時間焼成した。得
られた白色粉末の平均粒径は2.5μmであり凝集の
ない球状に近い微粉末でその組成は酸素0.5重量
％，炭素0.02重量％、Fe10ppm，Si200ppmであ
り、Ｘ線回折の結果窒化アルミニウム単相であつ
た。
次にこの粉末約４ｇを450Kg／cm2で一軸成形後、
1.5t／cm2でラバープレスした結果、成形後の密度
は理論密度（3.20ｇ／cm3）に対して60％であつ
た。
次に実施例２〜６、比較例１〜２を第１表に示
す。平均粒径の測定値はマイクロトラツクパーテ
イクルアナライザーによつて求めた。
尚比較例１および２では実施例１および４にお
ける種子としての窒化アルミニウム前駆体を添加
することを除いてその他は実施例１および４と全
く同様にして実施した。
[Industrial Application Field] The present invention relates to a method for producing high purity aluminum nitride powder. Aluminum nitride is attracting attention as a ceramic material for electronic devices, and the present invention particularly relates to a manufacturing method that provides a large amount of high-purity aluminum nitride powder that is nearly spherical, contains very little oxygen and carbon, and has excellent formability. . [Prior art] Aluminum nitride powder can be produced using a direct nitriding method in which metal aluminum is directly reacted with nitrogen or ammonia, a reductive nitriding method in which a mixed powder of alumina and carbon is fired in a nitrogen-containing atmosphere, and an organic aluminum compound. After preparing an aluminum nitride precursor by reacting it with ammonia or primary or secondary amines, there is a method (Japanese Patent Laid-Open No. 68700/1983) in which the precursor is fired in an inert gas, vacuum, or ammonia stream. Are known. However, in the direct nitriding method and the reductive nitriding method, the thermal conductivity of the sintered body decreases because impurities originating from the raw materials, especially oxygen, are likely to be mixed. Also, JP-A-53
In the method disclosed in No. 68700, in which an aluminum nitride precursor is fired to produce aluminum nitride, the precursor produced is an agglomerate of very fine particles, which is presumed to be caused by uniform nucleation. It has an amorphous shape, has a wide particle size distribution, and has a large particle size ranging from a dozen microns to several tens of microns. The shape of the aluminum nitride powder obtained by firing such a precursor is a replica of the precursor, and therefore the compacting density of the aluminum nitride powder is low. For this reason, a crushing or pulverizing process is essential after firing, and this process forms active surfaces that easily react with oxygen and water, resulting in a further increase in oxygen and cationic impurities, which is a fatal flaw. have. [Problems to be Solved by the Invention] Therefore, the present inventors have conducted various studies on a method for producing high-purity aluminum nitride powder that is low in oxygen and carbon and has excellent formability using an organic aluminum compound as a starting material. , discovered a new manufacturing method and led to the present invention. [Means to solve the problem] As a result of further intensive research, the average particle diameter
Aluminum nitride precipitated by reacting ammonia at 130°C or higher with a high-purity organoaluminum solution containing 0.1 to 10% by weight of aluminum nitride precursor and/or aluminum nitride powder with a diameter of 1 μm or less based on the aluminum nitride precursor to be produced. It was discovered that the precursor has no agglomeration and its shape is close to spherical. Although the details of the production mechanism of the precursor are not known, it is presumed that nucleation occurs on the surface of the seed and continues to grow, so that the nuclei do not coalesce. The aluminum nitride precursor obtained in this way was maintained at a temperature range of 400 to 1100°C under a stream of ammonia for a certain period of time, and then kept at a temperature of 1100 to 1100°C under a stream of inert gas.
If fired at a temperature of 1600℃, it will have a nearly spherical shape and will not require crushing. In addition, the inventors discovered that a high-purity aluminum nitride powder with extremely low oxygen and carbon content and excellent moldability could be obtained, leading to the completion of the present invention. To explain in detail below, the organoaluminum compounds include trialkylaluminum, dialkylaluminum hydride, dialkylaluminum halide, alkylaluminum dihalide, and alkylaluminum sesquihalide, and specifically, trimethylaluminum, triethylaluminum, triisobutylaluminum, diethyl Aluminum hydride, diethylaluminum chloride, isobutylaluminum sesquichloride, etc. are used, but triethylaluminum or triisobutylaluminum is advantageous from an economic standpoint. In the reaction, the organoaluminum compound is diluted with a solvent such as xylene, kerosene, decane, tetralin, etc. and used as a solution of about 20% by weight. Aluminum nitride precursor powder and/or aluminum nitride powder can be used as seeds to be added to the organoaluminum compound solution, but the particle size of both is preferably 1 μm or less. The aluminum nitride precursor powder is obtained by reacting an organoaluminum compound with ammonia or organic amines under appropriate conditions, and the aluminum nitride precursor is ground using a ball mill or vibration mill. Vapor phase process aluminum nitride powder and commercially available aluminum nitride powder which can be easily obtained according to Japanese Patent Application No. 61-203463 (see Japanese Patent Publication No. 4-8364) proposed by the inventors are preferably used. Regarding the amount of the powder added, the larger the amount added, the smaller the particle size of the aluminum nitride powder becomes. However, if it is 10% by weight or more, it will re-agglomerate, and if it is 0.1% by weight or less, no significant effect will be observed. Ten
It is preferably 1 to 5% by weight. Further, it is necessary to react the organoaluminum compound and ammonia with appropriate stirring. If the reaction temperature is lower than 130°C, not only will the yield of the aluminum nitride precursor decrease, but also the transitivity will deteriorate. 130℃
There is no particular restriction as long as it is above, but 130 to 250°C is appropriate considering the boiling point of the solvent used. Firing is carried out under a stream of non-oxidizing gas. As the atmospheric gas, it is possible to use an inert gas such as nitrogen or argon, or a reducing gas such as ammonia or hydrogen, or a mixture thereof, but in order to reduce the amount of carbon in the aluminum nitride powder, ammonia is used. It is desirable to hold the temperature preferably in the temperature range of 400 to 1100°C for 0.5 to 4 hours. 400
Below ℃, the decomposition of organic residues is slow and takes a long time.
Moreover, at temperatures above 1100°C, the decomposition of ammonia is significant, making it uneconomical. By such calcination, aluminum nitride with a low carbon content is obtained, and by further holding the powder in a temperature range of 1100 to 1600° C. for an appropriate time under a stream of inert gas, aluminum nitride powder becomes stable in air. A temperature of 1600° C. or higher is not preferable because aluminum nitride will sinter and harden. [Example] A more specific explanation will be given below with reference to Examples. Example 1 An aluminum nitride precursor was synthesized by reacting a 20% by weight n-decane solution of triethylaluminum at 170° C. with ammonia. 20 g of this precursor was poured into 350 ml of n-decane and ground in a vibration mill for 1 hour to obtain a precursor slurry with an average particle size of 0.5 μm. Next, 15% by weight of triethylaluminum
35 ml of the previously prepared slurry was added to decane solution 2.1. The reactor was then heated to 155°C and ammonia was introduced into the gas phase of the reactor while stirring. When 1.2 equivalents of ammonia were introduced relative to triethylaluminum, the temperature inside the reactor began to decrease, indicating that a precipitate was deposited. In this example, the amount of aluminum nitride precursor added as seeds corresponds to 1.3% by weight of the aluminum nitride precursor produced. After the reaction was completed, the white precipitate produced was separated and dried under reduced pressure to obtain an aluminum nitride precursor. 250 g of this powder was placed in a carbon dish and heated to 1000°C under an ammonia stream, held for 2 hours, and then the atmosphere gas was changed to nitrogen and fired at 1500°C for 4 hours. The average particle size of the obtained white powder was 2.5 μm, and it was a nearly spherical fine powder with no agglomeration. Its composition was 0.5% by weight of oxygen, 0.02% by weight of carbon, 10ppm of Fe, and 200ppm of Si. It was a phase. Next, about 4g of this powder was uniaxially molded at 450Kg/ cm2 ,
As a result of rubber pressing at 1.5 t/cm 2 , the density after molding was 60% of the theoretical density (3.20 g/cm 3 ). Next, Examples 2 to 6 and Comparative Examples 1 to 2 are shown in Table 1. Measurements of average particle size were determined using a microtrack particle analyzer. Comparative Examples 1 and 2 were carried out in exactly the same manner as in Examples 1 and 4, except that the aluminum nitride precursor was added as a seed.
以上、詳述した本発明方法によれば、従来法に
比較し、球形に近くしかも凝集がなく成形性に優
れた高純度窒化アルミニウム粉が工業的に得られ
る。
According to the method of the present invention described in detail above, compared to conventional methods, high-purity aluminum nitride powder can be industrially obtained which has a nearly spherical shape, is free from agglomeration, and has excellent formability.
第１図は本発明（実施例１）による窒化アルミ
ニウム粉の粒子を示す顕微鏡写真であり、また第
２図は比較例１で製造した窒化アルミニウムの粒
子を示す顕微鏡写真である。倍率はいずれも1500
倍である。
FIG. 1 is a photomicrograph showing particles of aluminum nitride powder according to the present invention (Example 1), and FIG. 2 is a photomicrograph showing particles of aluminum nitride produced in Comparative Example 1. All magnifications are 1500
It's double.
Claims (1)
およびまたは窒化アルミニウム粉末を、生成する
窒化アルミニウム前駆体に対し0.1〜10重量％含
む高純度有機アルミニウム溶液に、アンモニアを
130℃以上で反応させて窒化アルミニウム前駆体
を沈澱させた後、該前駆体をアンモニア気流下
400〜1100℃の温度範囲に一定時間保持し、さら
に不活性ガス気流下1100〜1600℃の温度域で焼成
することを特徴とする高純度窒化アルミニウム粉
の製造法。1. Ammonia is added to a high-purity organic aluminum solution containing 0.1 to 10% by weight of aluminum nitride precursor and/or aluminum nitride powder with an average particle size of 1 μm or less based on the aluminum nitride precursor to be produced.
After precipitating the aluminum nitride precursor by reacting at 130°C or higher, the precursor is precipitated under an ammonia stream.
A method for producing high-purity aluminum nitride powder, which comprises holding the powder in a temperature range of 400 to 1100°C for a certain period of time, and then firing it in a temperature range of 1100 to 1600°C under an inert gas flow.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21419987A JPS6456308A (en) | 1987-08-28 | 1987-08-28 | Production of aluminum nitride powder having high purity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21419987A JPS6456308A (en) | 1987-08-28 | 1987-08-28 | Production of aluminum nitride powder having high purity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6456308A JPS6456308A (en) | 1989-03-03 |
| JPH0466807B2 true JPH0466807B2 (en) | 1992-10-26 |
Family
ID=16651871
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21419987A Granted JPS6456308A (en) | 1987-08-28 | 1987-08-28 | Production of aluminum nitride powder having high purity |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6456308A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5645559B2 (en) * | 2010-09-03 | 2014-12-24 | 株式会社トクヤマ | Spherical aluminum nitride powder |
| JP5618734B2 (en) | 2010-09-28 | 2014-11-05 | 株式会社トクヤマ | Spherical aluminum nitride powder |
| JP6149668B2 (en) * | 2012-10-11 | 2017-06-21 | 宇部興産株式会社 | Al-N-H compound powder and method for producing the same |
-
1987
- 1987-08-28 JP JP21419987A patent/JPS6456308A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6456308A (en) | 1989-03-03 |
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