JPH03215399A - Method for preparing fibrous aluminum nitride - Google Patents
Method for preparing fibrous aluminum nitrideInfo
- Publication number
- JPH03215399A JPH03215399A JP708590A JP708590A JPH03215399A JP H03215399 A JPH03215399 A JP H03215399A JP 708590 A JP708590 A JP 708590A JP 708590 A JP708590 A JP 708590A JP H03215399 A JPH03215399 A JP H03215399A
- Authority
- JP
- Japan
- Prior art keywords
- mixture
- aluminum nitride
- aluminum
- water
- aluminum oxide
- 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 abstract description 33
- 238000000034 method Methods 0.000 title description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 27
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 16
- 239000012298 atmosphere Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 14
- 239000006229 carbon black Substances 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 229920000620 organic polymer Polymers 0.000 claims description 12
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 8
- 239000008240 homogeneous mixture Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 238000002156 mixing Methods 0.000 abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 5
- 239000004793 Polystyrene Substances 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract description 2
- 239000012299 nitrogen atmosphere Substances 0.000 abstract description 2
- 229920002223 polystyrene Polymers 0.000 abstract description 2
- 239000012779 reinforcing material Substances 0.000 abstract description 2
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 229910002804 graphite Inorganic materials 0.000 description 10
- 239000010439 graphite Substances 0.000 description 10
- 239000002904 solvent Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000000843 powder Substances 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 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229920002239 polyacrylonitrile Polymers 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- NYQDCVLCJXRDSK-UHFFFAOYSA-N Bromofos Chemical compound COP(=S)(OC)OC1=CC(Cl)=C(Br)C=C1Cl NYQDCVLCJXRDSK-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- -1 aluminum compound Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000012461 cellulose resin Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野］
本発明は、新規な繊維状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 novel method for producing fibrous aluminum nitride.
窒化アルミニウムウィスカーの製造方法としては、実験
室的には窒化アルミニウム粉末をルツボに入れ、１８０
０℃以上に加熱し、アルゴンガスで窒素濃度を調整する
ことにより製造することが報告されている。また、工業
的には以下の生成法が知られている。In the laboratory, aluminum nitride whiskers are produced by placing aluminum nitride powder in a crucible and heating it at 180°C.
It has been reported that it can be produced by heating to 0° C. or higher and adjusting the nitrogen concentration with argon gas. In addition, the following production methods are known industrially.
（１）昇華法
窒化アルミニウム粉末を黒鉛ルッポに入れ、加熱炉中で
炉内を窒素ガス雰囲気に保ちながら２０００℃以上の温
度に加熱する。原料となる窒化アルミニウム粉末は１５
００℃〜１７００℃の領域で急速に昇華再結晶し単結晶
ウィスカ一としてルッポ壁に生成付着する。(1) Sublimation method aluminum nitride powder is placed in a graphite Lupo and heated to a temperature of 2000°C or higher in a heating furnace while maintaining a nitrogen gas atmosphere inside the furnace. The raw material aluminum nitride powder is 15
It rapidly sublimes and recrystallizes in the region of 00°C to 1700°C, and forms and adheres to the Lupo wall as a single crystal whisker.
（２）金属アルミニウムと窒素ガスによる反応生成法
金属アルミニウムを黒鉛ルッポに入れ、窒素ガス雰囲気
下で加熱処理することによりルッポ内部に窒化アルミニ
ウムウィスカ一を生成する［Ｐｒｏｔｏｎ：ｅｔａｌ
Ｐｏｒｏｓｈ Ｍｅｔ （ＵＳＳＲ）１０−５． １０
（１９７０）］。(2) Reaction generation method using metal aluminum and nitrogen gas Metal aluminum is placed in a graphite Lupo and heated in a nitrogen gas atmosphere to generate aluminum nitride whiskers inside the Lupo [Proton: etal
Porosh Met (USSR) 10-5. 10
(1970)].
（３）酸化アルミニウム、炭素および窒化ガスによる反
応生成法
酸化アルミニウムと炭素の混合物を黒鉛ルッポに入れ、
窒素ガス雰囲気下の黒鉛抵抗炉中で２１００℃〜２２０
０℃に加熱し、その後空気を導入して黒鉛ルッポを燃焼
させて、窒化アルミニウムウィスカ１を得る ［Ｋｏｈ
ｎｅｔａｌ Ｍｉｎｅｒａｌｏｇｉｓｔ ４１３５５
（１’９６５）］。(3) Reaction production method using aluminum oxide, carbon and nitriding gas A mixture of aluminum oxide and carbon is placed in a graphite Lupo,
2100℃~220℃ in a graphite resistance furnace under nitrogen gas atmosphere
Heating to 0°C, then introducing air to combust graphite Luppo to obtain aluminum nitride whiskers 1 [Koh
netal Mineralologist 41355
(1'965)].
（４）酸化アルミニウム、炭素および遷移金属と窒素ガ
スによる反応生成法
酸化アルミニウムに遷移金属化合物とカーポンブラック
とを均質混合して嵩密度０．０５ ｇ／ｃｃ〜０．１５
ｇ／ｃｃの混合物を調製し、該混合物を窒素ガス雰囲
気下の反応炉中でｌ６５０℃〜１８５０″Ｃに加熱し、
窒化アルミニウムウィスカーを得る［特開昭６２ −
２８３９００号公報］。(4) Reaction production method using aluminum oxide, carbon, and transition metals with nitrogen gas A transition metal compound and carbon black are homogeneously mixed with aluminum oxide, and the bulk density is 0.05 g/cc to 0.15.
g/cc mixture and heating the mixture to 1650°C to 1850″C in a reactor under nitrogen gas atmosphere,
Obtaining aluminum nitride whiskers [JP-A-62-
No. 283900].
（５）アルミナ繊維、炭素および窒素ガスによる反応生
成法
アルミナ金属繊維もしくはアルミナ形成性アルミニウム
化合物と炭素含有物質からなる混合物を繊維化して得た
アルミナ繊維を窒素雰囲気下で加熱し、窒化アルミニウ
ム繊維とする［特開昭６１−１２４６２６号公報、特開
昭６３ − ２７０８６１号公報１。(5) Reaction production method using alumina fiber, carbon and nitrogen gas Alumina fiber obtained by fiberizing alumina metal fiber or a mixture of an alumina-forming aluminum compound and a carbon-containing substance is heated in a nitrogen atmosphere to form aluminum nitride fiber. [JP-A-61-124626, JP-A-63-270861 1.
〔発明が解決しようとする課題］
（１）の方法によれば原料として高価な窒化アルミニウ
ム粉末を用い、さらには２０００℃以上の高温で処理す
る必要があるなど製造コストが非常に高くなる欠点を有
する。[Problems to be Solved by the Invention] The method (1) uses expensive aluminum nitride powder as a raw material and has the drawbacks of extremely high manufacturing costs, such as the need for processing at a high temperature of 2000°C or higher. have
〔２）、（３）および（５）の方法によれば原料は安価
な金属アルミニウムさらには酸化アルミニウムによるが
高温で加熱処理しなければならずさらには粒状の窒化ア
ルミニウムとなりやすく、ウィスカーの生成収率が良く
ない欠点がある。[2), (3), and (5) methods use cheap metal aluminum or aluminum oxide as raw materials, but they must be heat-treated at high temperatures, and furthermore, they tend to become granular aluminum nitride, which leads to problems with whisker formation. There is a drawback that the rate is not good.
（４）の方法によれば、原料として安価な酸化アルミニ
ウムを用い、さらには低温域での加熱処理で窒化アルミ
ニウムウィスカーを生成させ得ることができるが、ウィ
スカーの生成を促進させるための触媒として金属塩を原
料中に混合させるため、生成したウィスカー中に金属元
素が不純物として残存し、窒化アルミニウムウィスカー
の純度が低下する欠点がある。According to method (4), aluminum nitride whiskers can be generated by using inexpensive aluminum oxide as a raw material and further by heat treatment in a low temperature range. Since the salt is mixed into the raw material, metal elements remain as impurities in the generated whiskers, which has the disadvantage of reducing the purity of the aluminum nitride whiskers.
上記の問題点を解決するため、鋭意研究を行った結果、
従来法に比べ、安価な原料をもちいさらには低い温度域
で加熱処理する繊維状窒化アルミニウムの製造方法をみ
いだし、本発明を完成した。In order to solve the above problems, as a result of intensive research,
We have discovered a method for producing fibrous aluminum nitride that uses cheaper raw materials and is heat-treated at a lower temperature range than conventional methods, and have completed the present invention.
すなわち、本発明は、酸化アルミニウム及び水酸化アル
ミニウムの単独またはその混合物とカボンブラックまた
は加熱分解により炭素を生成する有機高分子物質とを混
合して均質な混合物とし、該混合物を水２００ｐｐｍ以
上５０００ ｐｐｍ以下含む窒素ガス雰囲気下の反応炉
中で１３００℃〜１７００℃に加熱することを特徴とす
る繊維状窒化アルミニウムの製造方法である。That is, the present invention mixes aluminum oxide and aluminum hydroxide alone or a mixture thereof with carbon black or an organic polymer substance that generates carbon by thermal decomposition to form a homogeneous mixture, and the mixture is mixed with 200 ppm or more of water and 5000 ppm of water. This is a method for producing fibrous aluminum nitride, which is characterized by heating to 1300° C. to 1700° C. in a reaction furnace under a nitrogen gas atmosphere containing:
本発明に用いる酸化アルミニウム及び水酸化アルミニウ
ムは純度９９重量％以上、好ましくは９９．９重量％以
上である。粒子径は、遠心沈降法による平均粒子径が２
μ一以下、好ましくは１μ翔以下、さらに好ましくは０
．８μｍ以下である。平均粒子径の小さいアルミニウム
をもちいることにより繊維状窒化アルミニウムの生成が
促進され、さらには加熱温度を低い温度とすることがで
きる。The purity of aluminum oxide and aluminum hydroxide used in the present invention is 99% by weight or more, preferably 99.9% by weight or more. The particle size is determined by the centrifugal sedimentation method, with an average particle size of 2.
μ1 or less, preferably 1μ or less, more preferably 0
．． It is 8 μm or less. By using aluminum with a small average particle size, the formation of fibrous aluminum nitride is promoted, and furthermore, the heating temperature can be lowered.
本発明に用いるカーボンブラックとしては灰分が０．２
重量％以下、平均粒子径が１μ−以下である。また、加
熱分解することにより炭素を生成する有機高分子物質と
しては、すべての有機高分子物質をもちいることができ
るが、好ましくはボリアミド、ポリイミド、セルロース
系樹脂、ポリスルホン、ポリアクリロニトリル、ポリス
チレン等である。The carbon black used in the present invention has an ash content of 0.2
% by weight or less, and the average particle diameter is 1 μm or less. Further, as the organic polymer substance that generates carbon by thermal decomposition, any organic polymer substance can be used, but polyamide, polyimide, cellulose resin, polysulfone, polyacrylonitrile, polystyrene, etc. are preferable. be.
本発明の製造方法において、酸化アルミニウムとカーボ
ンブラックを用いる場合、重量比１ ： ０．４〜１：
１．０で溶媒中に混入し、また、水酸化アルミニウムと
カーポンブラックを用いる場合、重量比１ ： ０．３
５〜１ ： ０．８５で溶媒中に混入して攪拌する方法
により均質なスラリー状混合液とし、該混合液をスプレ
ードライヤ等により粒状混合物とする。もちいる溶媒と
しては、酸化アルミニウム、水酸化アルミニウム及びカ
ーボンブラックを溶解しないものであれば特に限定され
ない。例えば水、塩水溶液、界面活性剤の水溶液、エタ
ノール等である。In the production method of the present invention, when aluminum oxide and carbon black are used, the weight ratio is 1:0.4 to 1:
When aluminum hydroxide and carbon black are used, the weight ratio is 1:0.3.
5-1: A homogeneous slurry-like mixture is prepared by mixing in a solvent at a concentration of 0.85 and stirring, and the mixture is made into a granular mixture using a spray dryer or the like. The solvent used is not particularly limited as long as it does not dissolve aluminum oxide, aluminum hydroxide, and carbon black. Examples include water, an aqueous salt solution, an aqueous surfactant solution, and ethanol.
また、酸化アルミニウムと加熱分解により炭素を生成す
る有機高分子物質を用いる場合、酸化アルミニウムと加
熱分解により生成する炭素の重量比Ｌ：０．４〜１ ：
１．０ 、水酸化アルミニウムと加熱分解により炭素
を生成する有機高分子物質を用いる場合、水酸化アルミ
ニウムと加熱分解により生成する炭素の重量比１：０．
３５〜１：０．８５で、有機高分子物質が溶解しうる溶
媒例えば、ジメチルホルムアミド等中で酸化アルミニウ
ムまたは水酸化アルミニウムを有機高分子物質と混合す
る。この混合の方法としては、
■酸化アルミニウムもしくは水酸化アルミニウムを溶媒
中に混入したのち有機高分子物質を加え混合する方法
■有機高分子物質を溶媒中に溶解したのち、酸化アルミ
ニウムもしくは水酸化アルミニウムを加え混合する方法
■酸化アルミニウムもしくは水酸化アルミニウム有機高
分子物質を同時に溶媒中に加え混合する方法
のいずれの方法でもよい。その後、該混合液を有機 高
分子物質を凝固させる溶媒中に入れ酸化アルミニウムも
しくは水酸化アルミニウムを均質に含む混合物とする。In addition, when using an organic polymer substance that generates carbon by thermal decomposition with aluminum oxide, the weight ratio L of aluminum oxide and carbon generated by thermal decomposition is 0.4 to 1:
1.0, when using an organic polymer substance that generates carbon by thermal decomposition with aluminum hydroxide, the weight ratio of aluminum hydroxide and carbon generated by thermal decomposition is 1:0.
Aluminum oxide or aluminum hydroxide is mixed with the organic polymer material in a solvent such as dimethylformamide in which the organic polymer material can be dissolved at a ratio of 35 to 1:0.85. This mixing method is as follows: - Mix aluminum oxide or aluminum hydroxide into a solvent, then add an organic polymer substance and mix. - Dissolve the organic polymer substance in a solvent, then add aluminum oxide or aluminum hydroxide. Method of Adding and Mixing (2) Any method of simultaneously adding and mixing aluminum oxide or aluminum hydroxide organic polymeric substances to the solvent may be used. Thereafter, the mixed solution is put into a solvent that coagulates an organic polymer substance to form a mixture homogeneously containing aluminum oxide or aluminum hydroxide.
このときもちいる溶媒は酸化アルミニウムもしくは水酸
化アルミニウムを溶解せず、有機高分子物質を凝固させ
るものであれば特に限定されない。The solvent used at this time is not particularly limited as long as it does not dissolve aluminum oxide or aluminum hydroxide and coagulates the organic polymer substance.
例えば、水、塩水溶液、界面活性剤の水溶液等である。For example, water, an aqueous salt solution, an aqueous solution of a surfactant, and the like.
酸化アルミニウムと水酸化アルミニウムの混合物をもち
いる場合の混合比は何ら規定するものではない。さらに
カーボンブラックまたは加熱分解により生成する炭素と
の重量比はＡｈ（ｈ ： Ｃとして１ ： ０．４〜１
：１．Ｏの範囲で混合し、混合物とする。When a mixture of aluminum oxide and aluminum hydroxide is used, the mixing ratio is not specified at all. Furthermore, the weight ratio of carbon black or carbon produced by thermal decomposition is Ah (1:0.4 to 1 as h:C).
:1. Mix within the O range to form a mixture.
前記の方法で調整された混合物を黒鉛ルッポに入れ、水
を含む窒素ガス雰囲気下の反応炉中で加熱することによ
り繊維状窒化アルミニウムが得られる。窒素ガス雰囲気
中に含まれる水の量は２００ｐｐａ＋以上５０００ｐｐ
ｍ以下であり、好ましくは５００ｐｐｒ＊以上５０００
ｐｐｎ＋以下である。水の量が２００ｐｐｍ未満では
繊維状窒化アルミニウムの生成率が低くなり、粒状の窒
化アルミニウムとなる。また、５０００ｐｐｍ以上にな
ると生成する繊維状窒化アルミニウムの表面が酸化され
ＡＩ２０．となるため純度が悪くなる。加熱温度は、１
３００’Ｃ〜１７００″Ｃ、好ましくは１４００℃〜１
７００℃、さらに好ましくは１５５０”Ｃ〜１７００℃
である。また、得られた繊維状窒化アルミニウム中に未
反応の残留炭素がある場合には、酸素を含む雰囲気中に
おいて５５０″Ｃ〜７ ０ ０ ’Ｃで加熱することに
より除去できる。あるいはアンモニアを含有した雰囲気
下で１０００”Ｃ〜１５００”Ｃに加熱することにより
残留炭素を除去できる。Fibrous aluminum nitride is obtained by putting the mixture prepared by the above method into a graphite Lupo and heating it in a reactor under a nitrogen gas atmosphere containing water. The amount of water contained in the nitrogen gas atmosphere is 200 ppa + 5000 pp
m or less, preferably 500 ppr* or more 5000
ppn+ or less. If the amount of water is less than 200 ppm, the production rate of fibrous aluminum nitride will be low, resulting in granular aluminum nitride. In addition, when the concentration exceeds 5000 ppm, the surface of the fibrous aluminum nitride that is generated is oxidized and the AI20. As a result, purity deteriorates. The heating temperature is 1
300'C~1700''C, preferably 1400°C~1
700°C, more preferably 1550”C to 1700°C
It is. In addition, if there is unreacted residual carbon in the obtained fibrous aluminum nitride, it can be removed by heating at 550''C to 700''C in an oxygen-containing atmosphere. Residual carbon can be removed by heating to 1000"C to 1500"C in an atmosphere.
上記繊維状窒化アルミニウムの製造にもちいる炉は、バ
ッチ炉、ブッシャ炉、シャフト炉、堅型炉をもちいるこ
とができる。The furnace used for producing the above-mentioned fibrous aluminum nitride may be a batch furnace, a Buscher furnace, a shaft furnace, or a vertical furnace.
本発明により製造される生成物のＸ線回折による不純物
の同定は理学電気■製ガイガーフレックス型Ｄ−９Ｃに
より行った。形状観察は日立製作所製Ｓ − ６５０型
走査型電子顕微鏡により行った。Identification of impurities in the product produced according to the present invention by X-ray diffraction was carried out using a Geigerflex model D-9C manufactured by Rigaku Denki. Shape observation was performed using a scanning electron microscope model S-650 manufactured by Hitachi, Ltd.
〔実施例］ 以下実施例によって本発明を具体的に説明する。〔Example] EXAMPLES The present invention will be specifically explained below with reference to Examples.
実施例１
遠心沈降法による平均粒子径が０．７４μｍ、純度が９
９．９９４重量％の酸化アルミニウム（旭化成工業■社
製）３００ｇとポリアクリロニトリル２６５ｇをジメチ
ルホルムアミド２５００ ｇ中で混合溶解したのち、該
混合液を水中に滴下して酸化アルミニウムとポリアクリ
ロニトリルからなる均質な混合物を得た。該混合物を黒
鉛ルツボに充填し、水１０００ｐｐｍを含む窒素ガス雰
囲気下の反応炉中温度１６５０℃で７時間保持した。内
容物を黒鉛ルツボから取り出し、大気中６００℃の温度
で熱処理し残留する炭素を除去した。得られた生成物の
Ｘ線回折をおこなった結果、窒化アルミニウムのみから
なる生成物であった。形状を走査電子顕微鏡により観察
した結果、直径０．２μｍ ＝ １ ． ０μｍ、長さ
１００μｍ以上の繊維状窒化アルミニウムであった。Example 1 Average particle diameter by centrifugal sedimentation method is 0.74 μm, purity is 9
After mixing and dissolving 300 g of 9.994% by weight aluminum oxide (manufactured by Asahi Kasei Corporation) and 265 g of polyacrylonitrile in 2500 g of dimethylformamide, the mixture was dropped into water to form a homogeneous mixture of aluminum oxide and polyacrylonitrile. A mixture was obtained. The mixture was filled into a graphite crucible and maintained at a temperature of 1650° C. for 7 hours in a reactor under a nitrogen gas atmosphere containing 1000 ppm of water. The contents were taken out from the graphite crucible and heat treated in the atmosphere at a temperature of 600°C to remove residual carbon. X-ray diffraction of the obtained product revealed that it was a product consisting only of aluminum nitride. As a result of observing the shape with a scanning electron microscope, the diameter was 0.2 μm = 1. It was fibrous aluminum nitride with a length of 0 μm and a length of 100 μm or more.
実施例２
遠心沈降法による平均粒子径が０．７４μＩ、純度が９
９． ９９４重量％の酸化アルミニウム（旭化成工業■
社製）３００ｇとカーボンプラック １５０ｇを水２０
００ ｇ中で混合しスプレードライヤーにより均質な粒
状混合物を得た。該混合物を黒鉛ルッポに充填し、水２
０００ ｐｐｍを含む窒素ガス雰囲気下の反応炉中、温
度１６５０℃で７時間保持した。Example 2 Average particle size by centrifugal sedimentation method was 0.74μI, purity was 9
9. 994% by weight aluminum oxide (Asahi Kasei Corporation■
) 300g and 150g of carbon plaque and 20g of water
A homogeneous granular mixture was obtained by mixing in 0.00 g and using a spray dryer. Fill a graphite Lupo with the mixture and add 2 ml of water.
The temperature was maintained at 1650° C. for 7 hours in a reactor under a nitrogen gas atmosphere containing 000 ppm.
内容物を黒鉛ルッポからとりだし、大気中６００℃の温
度で熱処理し残留する炭素を除去した。得られた生成物
のＸ線回折をおこなった結果窒化アルミニウムのみから
なる生成物であった。形状を走査型電子顕微鏡により観
察した結果、直径０．２μＩＩ１〜１．０μｍ、長さ１
０ ０ ａｍ以上の繊維状窒化アルミニウムであった
。The contents were taken out from the graphite Lupo and heat treated in the atmosphere at a temperature of 600°C to remove residual carbon. X-ray diffraction of the obtained product revealed that the product consisted only of aluminum nitride. As a result of observing the shape with a scanning electron microscope, the diameter was 0.2 μII1 to 1.0 μm, and the length was 1 μm.
It was fibrous aluminum nitride of 0.00 am or more.
比較例
実施例１と同一装置、混合物、加熱条件をもちい、水０
．５ ｐｐｍ以下を含む窒化ガス雰囲気下の反応炉中で
生成反応させた。得られた生成物を大気中６００℃の温
度で熱処理し残留する炭素を除去した。得られた生成物
のＸ線回折をおこなった結果、窒化アルミニウムのみか
らなる生成物であった。形状を走査型電子顕微鏡で観察
した結果、繊維状物質の生成は認められなかった。Comparative Example Using the same equipment, mixture, and heating conditions as in Example 1, with 0 water.
．． The production reaction was carried out in a reactor under an atmosphere of nitriding gas containing 5 ppm or less. The obtained product was heat treated in the air at a temperature of 600°C to remove residual carbon. X-ray diffraction of the obtained product revealed that it was a product consisting only of aluminum nitride. As a result of observing the shape with a scanning electron microscope, no formation of fibrous substances was observed.
〔発明の効果］
本発明によれば、従来法に比べ安価な酸化アルミニウム
もしくは水酸化アルミニウムを原料とし、１３００℃〜
１７００℃の低い温度領域で効率よく、繊維状窒化アル
ミニウムを製造することかできる。したがって低いコス
トでの量産化が可能となり、各種の複合用途に有効な強
化材として提供できる。[Effect of the invention] According to the present invention, aluminum oxide or aluminum hydroxide, which is cheaper than the conventional method, is used as a raw material and
Fibrous aluminum nitride can be efficiently produced in the low temperature range of 1700°C. Therefore, mass production at low cost is possible, and it can be provided as an effective reinforcing material for various composite uses.
特許出順人 旭化成工業株式会社 代 理 人 渡 辺 雄Patent issuer Asahi Kasei Industries, Ltd. teenager Reason Man Watari side male
Claims (1)
それらの混合物とカーボンブラックまたは加熱分解によ
り炭素を生成する有機高分子物質とを混合して均質な混
合物とし、該混合物を水２００ｐｐｍ以上５０００ｐｐ
ｍ以下含む窒素ガス雰囲気下の反応炉中で１３００℃〜
１７００℃に加熱することを特徴とする繊維状窒化アル
ミニウムの製造方法。Aluminum oxide and aluminum hydroxide alone or a mixture thereof are mixed with carbon black or an organic polymer substance that generates carbon by thermal decomposition to form a homogeneous mixture, and the mixture is mixed with 200 ppm or more of water and 5000 ppm of water.
1300℃ ~ in a reactor under a nitrogen gas atmosphere containing less than m
A method for producing fibrous aluminum nitride, which comprises heating to 1700°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP708590A JPH03215399A (en) | 1990-01-18 | 1990-01-18 | Method for preparing fibrous aluminum nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP708590A JPH03215399A (en) | 1990-01-18 | 1990-01-18 | Method for preparing fibrous aluminum nitride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03215399A true JPH03215399A (en) | 1991-09-20 |
Family
ID=11656254
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP708590A Pending JPH03215399A (en) | 1990-01-18 | 1990-01-18 | Method for preparing fibrous aluminum nitride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03215399A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5693305A (en) * | 1995-10-19 | 1997-12-02 | Advanced Refractory Technologies, Inc. | Method for synthesizing aluminum nitride whiskers |
| CN1055143C (en) * | 1998-07-24 | 2000-08-02 | 清华大学 | Manufacture of aluminum nitride fiber |
| WO2008018320A1 (en) * | 2006-08-09 | 2008-02-14 | Shin-Etsu Chemical Co., Ltd. | MATERIAL FOR FABRICATING SINGLE CRYSTAL SiC, METHOD FOR FABRICATING THE MATERIAL, METHOD FOR FABRICATING SINGLE CRYSTAL SiC USING THE MATERIAL, AND SINGLE CRYSTAL SiC OBTAINED BY THE METHOD FOR FABRICATING SINGLE CRYSTAL SiC |
| JP2010138056A (en) * | 2008-12-15 | 2010-06-24 | Mitsubishi Chemicals Corp | Aluminum nitride having high aspect ratio, method of manufacturing the same, resin composition using the same |
| JP2010235842A (en) * | 2009-03-31 | 2010-10-21 | Mitsubishi Chemicals Corp | Thermosetting resin composition containing anisotropic aluminum nitride filler |
| JP2012041254A (en) * | 2010-08-23 | 2012-03-01 | Tohoku Univ | Aluminum nitride wire, method for producing the same, and apparatus for producing aluminum nitride wire |
-
1990
- 1990-01-18 JP JP708590A patent/JPH03215399A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5693305A (en) * | 1995-10-19 | 1997-12-02 | Advanced Refractory Technologies, Inc. | Method for synthesizing aluminum nitride whiskers |
| CN1055143C (en) * | 1998-07-24 | 2000-08-02 | 清华大学 | Manufacture of aluminum nitride fiber |
| WO2008018320A1 (en) * | 2006-08-09 | 2008-02-14 | Shin-Etsu Chemical Co., Ltd. | MATERIAL FOR FABRICATING SINGLE CRYSTAL SiC, METHOD FOR FABRICATING THE MATERIAL, METHOD FOR FABRICATING SINGLE CRYSTAL SiC USING THE MATERIAL, AND SINGLE CRYSTAL SiC OBTAINED BY THE METHOD FOR FABRICATING SINGLE CRYSTAL SiC |
| JP2008037720A (en) * | 2006-08-09 | 2008-02-21 | Shin Etsu Chem Co Ltd | SOURCE MATERIAL FOR MANUFACTURING SINGLE CRYSTAL SiC, METHOD FOR MANUFACTURING THE SAME, METHOD FOR MANUFACTURING SINGLE CRYSTAL SiC USING THE SOURCE MATERIAL, AND SINGLE CRYSTAL SiC OBTAINED BY THE METHOD |
| JP2010138056A (en) * | 2008-12-15 | 2010-06-24 | Mitsubishi Chemicals Corp | Aluminum nitride having high aspect ratio, method of manufacturing the same, resin composition using the same |
| JP2010235842A (en) * | 2009-03-31 | 2010-10-21 | Mitsubishi Chemicals Corp | Thermosetting resin composition containing anisotropic aluminum nitride filler |
| JP2012041254A (en) * | 2010-08-23 | 2012-03-01 | Tohoku Univ | Aluminum nitride wire, method for producing the same, and apparatus for producing aluminum nitride wire |
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