JPH03187998A - Production of aluminum nitride whisker - Google Patents
Production of aluminum nitride whiskerInfo
- Publication number
- JPH03187998A JPH03187998A JP32263389A JP32263389A JPH03187998A JP H03187998 A JPH03187998 A JP H03187998A JP 32263389 A JP32263389 A JP 32263389A JP 32263389 A JP32263389 A JP 32263389A JP H03187998 A JPH03187998 A JP H03187998A
- Authority
- JP
- Japan
- Prior art keywords
- aluminum
- aluminum nitride
- carbon powder
- powder
- nitride whiskers
- 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 40
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 17
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 3
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims 2
- 150000001875 compounds Chemical class 0.000 claims 2
- 238000010304 firing Methods 0.000 claims 2
- 230000001590 oxidative effect Effects 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 230000008021 deposition Effects 0.000 abstract 2
- 239000000463 material Substances 0.000 description 4
- 239000000835 fiber Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 230000002787 reinforcement Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 235000019687 Lamb Nutrition 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
- 239000006229 carbon black Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011005 laboratory method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は耐熱性、高熱伝導性を有する窒化アルミニラム
ウィスカーの製造方法に関するものであり、これら窒化
アルミニウムウィスカーは樹脂や金属、セラミックスの
耐熱性付与、補強材等として用いられる。[Detailed Description of the Invention] [Field of Industrial Application] The present invention relates to a method for producing aluminum nitride lamb whiskers having heat resistance and high thermal conductivity. It is used as a reinforcement material, reinforcement material, etc.
耐熱性を有する無機繊維あるいはウィスカーは樹脂や金
属あるいはセラミックスと複合化し耐熱性の向上及び補
強材料等として用いられる。具体的には、アルミナ、炭
化珪素、チタン酸カリウム等の繊維、ウィスカーが用い
られている。窒化アルミニウムはこれらの材料と同等も
しくはより優れた耐熱性、機械的強度を持ち、さらに高
い絶縁性と熱伝導性を兼ね備えた材料であるが、窒化ア
ルミニウムウィスカーを製造する方法としては実験室的
には、例えば鉱物学雑誌第１０巻第２号Ｐ９８〜Ｐ１０
４ （１９７０年１２月）に紹介されているような方法
が知られているが、工業的に安価に製造する方法は知ら
れていない。Heat-resistant inorganic fibers or whiskers are combined with resins, metals, or ceramics to improve heat resistance and are used as reinforcing materials. Specifically, fibers and whiskers of alumina, silicon carbide, potassium titanate, etc. are used. Aluminum nitride has heat resistance and mechanical strength equal to or superior to these materials, as well as higher insulation and thermal conductivity, but the method for producing aluminum nitride whiskers is a laboratory method. For example, Mineralogical Journal Vol. 10 No. 2 P98-P10
4 (December 1970) is known, but there is no known method for producing it industrially at low cost.
本発明は窒化アルミニウムウィスカーを工業的に安価に
製造する方法に関するものであり、気相からの窒化アル
ミニウムウィスカーの成長速度を、工業的な生産に十分
に見合うように高めることを課題とする。The present invention relates to a method for industrially producing aluminum nitride whiskers at low cost, and an object of the present invention is to increase the growth rate of aluminum nitride whiskers from the gas phase to a level sufficient for industrial production.
本発明は、アルミニウム蒸気を含む窒素ガス気流中より
炭素粉末表面に窒化アルミニウムウィスカーを析出させ
ることを特徴とする窒化アルミニウムウィスカーの製造
方法を提供するものである。The present invention provides a method for producing aluminum nitride whiskers, which is characterized by depositing aluminum nitride whiskers on the surface of carbon powder in a nitrogen gas stream containing aluminum vapor.
窒化アルミニウムウィスカーを生成させるために必要な
アルミニウム蒸気は１６００℃以上好ましくは１８００
℃以上２０００℃以下の温度で窒素気流中で生成させる
。アルミニウムの蒸気は金属アルミニウムあるいは酸化
アルミニウム粉末と炭素粉末の混合物を窒素気流中で加
熱することにより生成されるが、この際窒化アルミニウ
ムの生成が同時に起こる。この窒化アルミニウムの生成
によりアルミニウム蒸気が生成しにくくなるので連続的
に窒化アルミニウムウィスカーを得ようとする場合は、
アルミニウム蒸気の発生部に常に新しい金属アルミニウ
ムあるいは酸化アルミニウムを供給することが望ましい
。アルミニウム蒸気を含んだ窒素ガスは１３００℃〜１
６００℃程度に加熱された場所において窒化アルミニウ
ムウィスカーとして析出してくる。窒化アルミニウムウ
ィスカーを効率よく析出させるためには表面積の大きい
物質の表面に析出させることが好ましく、さらに析出さ
せた後のウィスカーの分離を容易にするために炭素粉末
を用いることが有用である。すなわち炭素粉末表面に析
出させた窒化アルミニウムウィスカーは、それを大気中
で７００℃程度に加熱し炭素を燃焼、除去することがで
きるからである。尚、この際の加熱温度は窒化アルミニ
ウムウィスカーの分解が起こらないよう８００℃以下で
行うことが望ましい。The temperature of the aluminum vapor required to generate aluminum nitride whiskers is 1600°C or higher, preferably 1800°C.
It is produced in a nitrogen stream at a temperature of 0.degree. C. or more and 2000.degree. C. or less. Aluminum vapor is produced by heating a mixture of metallic aluminum or aluminum oxide powder and carbon powder in a nitrogen stream, with simultaneous formation of aluminum nitride. This generation of aluminum nitride makes it difficult to generate aluminum vapor, so if you want to continuously obtain aluminum nitride whiskers,
It is desirable to constantly supply fresh metallic aluminum or aluminum oxide to the aluminum vapor generating section. Nitrogen gas containing aluminum vapor is 1300℃~1
It precipitates as aluminum nitride whiskers in places heated to about 600°C. In order to efficiently precipitate aluminum nitride whiskers, it is preferable to precipitate them on the surface of a substance with a large surface area, and it is also useful to use carbon powder to facilitate separation of the whiskers after they have been precipitated. That is, the aluminum nitride whiskers deposited on the surface of the carbon powder can be heated to about 700° C. in the atmosphere to burn and remove carbon. Note that the heating temperature at this time is preferably 800° C. or lower so as not to cause decomposition of the aluminum nitride whiskers.
さらに窒化アルミニウムウィスカーの析出を効率よく行
うためにＶＬＳ機構に基づく析出を行わせるため炭素粉
末に鉄分を微量添加することが望ましい。鉄分としては
、例えば鉄粉あるいは酸化鉄粉末を、０．１ｗｔ％〜１
０ｗｔ％程度添加すればよい。特に、炭素粉末に微粒の
酸化鉄粉末を混合したものを用いることが有用である。Furthermore, in order to efficiently precipitate aluminum nitride whiskers, it is desirable to add a small amount of iron to the carbon powder in order to perform the precipitation based on the VLS mechanism. As the iron content, for example, iron powder or iron oxide powder is used at a concentration of 0.1 wt% to 1
It is sufficient to add about 0 wt%. In particular, it is useful to use a mixture of carbon powder and fine iron oxide powder.
この様に酸化鉄粉末を炭素粉末と混ぜることは、酸化鉄
〔実施例〕
以下、実施例に基づいて、本発明の内容をさらに詳しく
説明するが、本発明の技術的範囲は、実施例に限定され
るものではない。Mixing the iron oxide powder with the carbon powder in this way is possible because the content of the present invention will be explained in more detail based on the examples below. It is not limited.
（実施例１）
第１図は、本発明の方法で、窒化アルミニウムウィスカ
ーを製造するための装置の断面図である。(Example 1) FIG. 1 is a sectional view of an apparatus for producing aluminum nitride whiskers by the method of the present invention.
左側の部分は、窒化アルミニウムウィスカーを析出させ
る部分で、炭素粉末としてカーボンブラックと酸化鉄（
Ｆｅ２０３）粉末を重量比で１００：１の割合で混合し
た粉末を２０ ｍ ｍ径に造粒したものを原料ホッパー
（１）及び黒鉛製反応管（３）に充填し、この反応管を
ヒーター（４）で１５５０℃に加熱した。そして、反応
管に充填された原料粒子はテーブルフィーダー（６）に
より連続的に排出され製品ホッパー（７）に貯めた。ま
た、第１図の右側の部分は窒化アルミニウムウィスカー
の生成に必要なアルミニウム蒸気と窒素ガスを供給する
部分であり、アルミニウム粉末と炭素粉末を重量比で１
： １の割合で混合した粉末を２０ガス導入管（１１）
より導入した。また、この反応管をヒーター（４）で１
８００℃に加熱した。The part on the left is the part where aluminum nitride whiskers are precipitated, and carbon black and iron oxide (as carbon powder) are deposited.
Fe203) powder mixed at a weight ratio of 100:1 was granulated to a diameter of 20 mm and filled into a raw material hopper (1) and a graphite reaction tube (3), and the reaction tube was heated with a heater ( 4) and heated to 1550°C. The raw material particles filled in the reaction tube were continuously discharged by a table feeder (6) and stored in a product hopper (7). In addition, the part on the right side of Figure 1 is the part that supplies aluminum vapor and nitrogen gas necessary for the generation of aluminum nitride whiskers, and the weight ratio of aluminum powder and carbon powder is 1.
: Powder mixed at a ratio of 1:2 to 20 gas inlet tubes (11)
It was introduced more. In addition, this reaction tube was heated with a heater (4) for 1
It was heated to 800°C.
そして、反応管に充填された原料粒子はテーブルフィー
ダー（６）により連続的に排出されホッパー（８）に貯
めた。The raw material particles filled in the reaction tube were continuously discharged by a table feeder (6) and stored in a hopper (8).
ここで、右側で生成したアルミニウム蒸気と窒素ガスは
黒鉛製の連結管（１２）により左側の窒化アルミニウム
ウィスカーの生成部に導入され反応管を経由し排ガス管
（９）により糸外へ排出される。Here, the aluminum vapor and nitrogen gas generated on the right side are introduced into the aluminum nitride whisker generation section on the left side through a graphite connecting pipe (12), passed through a reaction tube, and then discharged to the outside of the yarn through an exhaust gas pipe (9). .
この様にして炭素粉末粒子の表面に析出した窒化アルミ
ニウムウィスカーは大気中で７００℃で５時間焼成し炭
素を燃焼除去した。得られた窒化アルミニウムウィスカ
ーの結晶組成は窒化アルミニウム単相であり、線径は０
． ５〜３μで長さは１０〜３００μであった。The aluminum nitride whiskers thus deposited on the surface of the carbon powder particles were calcined in the air at 700° C. for 5 hours to burn off the carbon. The crystal composition of the obtained aluminum nitride whiskers is aluminum nitride single phase, and the wire diameter is 0.
．． The length was 10-300μ.
（実施例２）
実施例１と同様の装置で右側の原料に酸化アルミニウム
と炭素粉末を重量比で５：３の割合で混合し、２０ ｍ
ｍ径に造粒したものを用いたところ実施例１と同等の
窒化アルミニウムウィスカーが得られた。(Example 2) Using the same equipment as in Example 1, aluminum oxide and carbon powder were mixed with the raw material on the right at a weight ratio of 5:3, and 20 m
When granules having a diameter of m were used, aluminum nitride whiskers equivalent to those in Example 1 were obtained.
この窒化アルミニウムウィスカーの繊維の形状を示す電
子顕微鏡写真を第２図及び第３図に示す。Electron micrographs showing the shape of the fibers of this aluminum nitride whisker are shown in FIGS. 2 and 3.
以上説明したように、本発明により窒化アルミニウムウ
ィスカーを連続的に効率よく製造できるようになり、窒
化アルミニウムウィスカーの低コスト化が図られ、これ
を補強材として用いた樹脂あるいはセラミックスとの複
合材料の低コスト化が図れる。As explained above, according to the present invention, aluminum nitride whiskers can be manufactured continuously and efficiently, the cost of aluminum nitride whiskers can be reduced, and composite materials with resins or ceramics using these whiskers as reinforcement materials can be produced. Cost reduction can be achieved.
第１図は本発明の製造方法に適用される製造装置（断面
図）の−例を示すものである。
第２図及び第３図は製造された窒化アルミニウムウィス
カーの繊維の形状を示す電子顕微鏡写真である。FIG. 1 shows an example of a manufacturing apparatus (cross-sectional view) applied to the manufacturing method of the present invention. FIGS. 2 and 3 are electron micrographs showing the shape of the fibers of the produced aluminum nitride whiskers.
Claims (4)
粉末表面に窒化アルミニウムウィスカーを析出させるこ
とを特徴とする窒化アルミニウムウィスカーの製造方法
。(1) A method for producing aluminum nitride whiskers, which comprises depositing aluminum nitride whiskers on the surface of carbon powder in a nitrogen gas stream containing aluminum vapor.
あるいは酸化鉄粉末を重量百分率で０．１％〜１０％添
加することを特徴とする窒化アルミニウムウィスカーの
製造方法。(2) The method for producing aluminum nitride whiskers according to claim 1, characterized in that iron powder or iron oxide powder is added to the carbon powder in a weight percentage of 0.1% to 10%.
気を含む窒素ガスをアルミニウムと炭素粉末の混合物も
しくは酸化アルミニウムあるいは焼成により酸化アルミ
ニウムとなる化合物と炭素粉末の混合物を窒素気流中で
１６００℃〜２０００℃の温度範囲内で加熱することに
より得ることを特徴とする窒化アルミニウムウィスカー
の製造方法。(3) In claim 1, the nitrogen gas containing aluminum vapor is heated at 1600°C to 2000°C in a nitrogen stream to prepare a mixture of aluminum and carbon powder, aluminum oxide, or a mixture of carbon powder and a compound that becomes aluminum oxide by firing. A method for producing aluminum nitride whiskers, characterized in that they are obtained by heating within a temperature range of °C.
加熱帯及び冷却帯を有する反応容器の上部より予熱帯に
装入し、この原料を前記反応容器の予熱帯内を連続的あ
るいは間欠的に降下させて加熱帯に至らせ、この加熱帯
の温度を１３００℃〜１６００℃の温度範囲で間接加熱
し、さらにこの加熱帯にアルミニウムと炭素粉末の混合
物もしくは酸化アルミニウムあるいは焼成により酸化ア
ルミニウムとなる化合物と炭素粉末の混合物を窒素気流
中で１６００℃〜２０００℃の温度範囲内で加熱して得
られるアルミニウム蒸気を含む窒素ガスを導入すること
により窒化アルミニウムウィスカーを原料表面に析出さ
せ、次いでこの原料を冷却帯に降下させ非酸化性雰囲気
で冷却させた後、前記反応容器の冷却帯下部より連続的
あるいは間欠的に生成物を排出することを特徴とする窒
化アルミニウムウィスカーの製造方法。(4) The raw material mixed with carbon powder and iron oxide powder is placed in a preheating zone.
The raw material is charged into a preheating zone from the upper part of a reaction vessel having a heating zone and a cooling zone, and the raw material is lowered continuously or intermittently through the preheating zone of the reaction vessel to reach the heating zone, and the temperature of the heating zone is lowered. is indirectly heated in a temperature range of 1,300°C to 1,600°C, and then in this heating zone, a mixture of aluminum and carbon powder or a mixture of aluminum oxide or a compound that becomes aluminum oxide by firing and carbon powder is heated at a temperature of 1,600°C to 2,000°C in a nitrogen stream. Aluminum nitride whiskers are precipitated on the surface of the raw material by introducing nitrogen gas containing aluminum vapor obtained by heating within the temperature range of °C, and then this raw material is lowered into a cooling zone and cooled in a non-oxidizing atmosphere. . A method for producing aluminum nitride whiskers, characterized in that the product is discharged continuously or intermittently from the lower part of the cooling zone of the reaction vessel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32263389A JPH03187998A (en) | 1989-12-14 | 1989-12-14 | Production of aluminum nitride whisker |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32263389A JPH03187998A (en) | 1989-12-14 | 1989-12-14 | Production of aluminum nitride whisker |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03187998A true JPH03187998A (en) | 1991-08-15 |
Family
ID=18145891
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP32263389A Pending JPH03187998A (en) | 1989-12-14 | 1989-12-14 | Production of aluminum nitride whisker |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03187998A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5688320A (en) * | 1995-06-19 | 1997-11-18 | Societe Nationale Industrielle Et Aerospatiale | Process for manufacturing aluminum nitride whiskers |
| US5693305A (en) * | 1995-10-19 | 1997-12-02 | Advanced Refractory Technologies, Inc. | Method for synthesizing aluminum nitride whiskers |
| JP2019172936A (en) * | 2018-03-29 | 2019-10-10 | Jnc株式会社 | Composition for heat radiation member, heat radiation member, and electronic device |
| CN110431259A (en) * | 2017-03-17 | 2019-11-08 | 国立大学法人名古屋大学 | The manufacturing method and manufacturing device of AlN whisker, AlN whisker structure body and AlN whisker and resin-formed body and its manufacturing method |
-
1989
- 1989-12-14 JP JP32263389A patent/JPH03187998A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5688320A (en) * | 1995-06-19 | 1997-11-18 | Societe Nationale Industrielle Et Aerospatiale | Process for manufacturing aluminum nitride whiskers |
| US5693305A (en) * | 1995-10-19 | 1997-12-02 | Advanced Refractory Technologies, Inc. | Method for synthesizing aluminum nitride whiskers |
| CN110431259A (en) * | 2017-03-17 | 2019-11-08 | 国立大学法人名古屋大学 | The manufacturing method and manufacturing device of AlN whisker, AlN whisker structure body and AlN whisker and resin-formed body and its manufacturing method |
| CN110431259B (en) * | 2017-03-17 | 2021-12-28 | 国立大学法人名古屋大学 | Method and apparatus for producing AlN whiskers, AlN whisker structure, AlN whiskers, and resin molded body and method for producing same |
| JP2019172936A (en) * | 2018-03-29 | 2019-10-10 | Jnc株式会社 | Composition for heat radiation member, heat radiation member, and electronic device |
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