JP2006265042A - Aluminum nitride powder, its manufacturing method and ceramic sintered body - Google Patents
Aluminum nitride powder, its manufacturing method and ceramic sintered body Download PDFInfo
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本発明は、窒化アルミニウム粉末、その製造方法およびセラミックス焼結体に関する。 The present invention relates to an aluminum nitride powder, a method for producing the same, and a ceramic sintered body.
例えば窒化ケイ素（Ｓｉ３Ｎ４）、窒化アルミニウム（ＡｌＮ）、炭化ケイ素等のセラミックス焼結体の耐腐食性、耐熱性を高めるために、また更に耐熱衝撃性を付与するために、窒化ホウ素（ＢＮ）を複合化することが行われている。なかでも、優れた熱伝導性と電気特性を兼ね備え加工性に優れる窒化アルミニウム（ＡｌＮ）−窒化ホウ素（ＢＮ）複合材の検討が行われている。 For example, in order to increase the corrosion resistance and heat resistance of ceramic sintered bodies such as silicon nitride (Si 3 N 4 ), aluminum nitride (AlN), and silicon carbide, and further to impart thermal shock resistance, boron nitride ( BN) is being compounded. In particular, an aluminum nitride (AlN) -boron nitride (BN) composite material that combines excellent thermal conductivity and electrical characteristics and excellent workability has been studied.
ＡｌＮ−ＢＮ複合材は、窒化ホウ素粉末と窒化アルミニウム粉末の混合粉末を焼結して製造される（特許文献１）。しかし、窒化ホウ素粒子は鱗片状であるので、窒化アルミニウム粉末との混合性が良くないなどの理由によって得られた複合材の機械的強度が十分に高くはなかった。より微細な窒化ホウ素粒子を用いても機械的強度の大幅な改善はなかった。 The AlN-BN composite material is manufactured by sintering a mixed powder of boron nitride powder and aluminum nitride powder (Patent Document 1). However, since the boron nitride particles are scaly, the mechanical strength of the obtained composite material was not sufficiently high due to poor mixing with the aluminum nitride powder. There was no significant improvement in mechanical strength using finer boron nitride particles.
本発明の目的は、セラミックス焼結体の曲げ強度を改善できる窒化アルミニウム粉末、その容易な製造方法およびその窒化アルミニウム粉末を用いて製造されたセラミックス焼結体を提供することである。 An object of the present invention is to provide an aluminum nitride powder capable of improving the bending strength of a ceramic sintered body, an easy production method thereof, and a ceramic sintered body produced using the aluminum nitride powder.
本発明は、化学分析により測定されたB含有量が１０ｐｐｍ以上であることを特徴とする窒化アルミニウム粉末である。好ましいB含有量は１０〜１０００ｐｐｍである。 The present invention is an aluminum nitride powder characterized in that the B content measured by chemical analysis is 10 ppm or more. A preferable B content is 10 to 1000 ppm.
また、本発明は、金属アルミニウム粉末を含む窒化性ガスを、内面が窒化ホウ素で構成され反応管の内面に衝突させながら供給し、金属アルミニウム粉末を窒化させることを特徴とする窒化アルミニウム粉末の製造方法である。 According to another aspect of the present invention, there is provided a method for producing an aluminum nitride powder, characterized by supplying a nitriding gas containing metallic aluminum powder while the inner surface is made of boron nitride and colliding with the inner surface of the reaction tube to nitride the metallic aluminum powder. Is the method.
また、本発明は、本発明の窒化アルミニウム粉末、又は本発明の窒化アルミニウム粉末とこの窒化アルミニウム粉末以外のセラミックス粉末を含む混合粉末を焼結してなることを特徴とするセラミックス焼結体である。なかでも、窒化アルミニウム粉末と窒化ホウ素粉末を含む混合粉末を焼結して得られたＡｌＮ−ＢＮ複合材であることが好ましい。 The present invention is also a ceramic sintered body obtained by sintering the aluminum nitride powder of the present invention or a mixed powder containing the aluminum nitride powder of the present invention and ceramic powder other than the aluminum nitride powder. . Especially, it is preferable that it is an AlN-BN composite material obtained by sintering the mixed powder containing an aluminum nitride powder and a boron nitride powder.
窒化アルミニウム粉末に例えば窒化ホウ素粉末等のＢ成分を後添加してB含有量を１０ｐｐｍ以上とした混合物は知られている。本発明の窒化アルミニウム粉末は、これらとは異なり、製造された直後の窒化アルミニウム粉末のB含有量が１０ｐｐｍ以上である点において相違している。Ｂ含有量は、加圧酸分解−ＩＣＰ法により測定される。本発明の窒化アルミニウム粉末を用いて焼結されたセラミックス焼結体、特にＡｌＮ−ＢＮ複合材の曲げ強度が著しく向上する。 A mixture in which a B content is made to be 10 ppm or more by post-adding B component such as boron nitride powder to aluminum nitride powder is known. Unlike the above, the aluminum nitride powder of the present invention is different in that the B content of the aluminum nitride powder immediately after being produced is 10 ppm or more. The B content is measured by a pressure acid decomposition-ICP method. The bending strength of the ceramic sintered body, particularly the AlN-BN composite material, sintered using the aluminum nitride powder of the present invention is remarkably improved.
本発明の製造方法に用いる金属アルミニウム粉末には、特に制約はないが、窒化反応の起こりやすさ、爆発性の低さから、平均粒径が１０〜４０μmのアトマイズ粉が好ましい。金属アルミニウム粉末は窒化性ガスに同伴されて高温場の反応管に供給され、窒化されて窒化アルミニウム粉末となる。ここで、窒化性ガスとは、金属アルミニウムを窒化アルミニウムとするための窒素を含んだガスのことであり、窒素ガス単独、窒素と例えば水素、CO、アンモニア等との混合ガスなどを例示することができる。 Although there is no restriction | limiting in particular in the metal aluminum powder used for the manufacturing method of this invention, Atomized powder with an average particle diameter of 10-40 micrometers is preferable from the ease of nitriding reaction taking place and low explosiveness. The metal aluminum powder is entrained with a nitriding gas and supplied to a reaction tube in a high temperature field, and is nitrided to become aluminum nitride powder. Here, the nitriding gas is a gas containing nitrogen for converting metal aluminum into aluminum nitride, and examples include nitrogen gas alone, a mixed gas of nitrogen and, for example, hydrogen, CO, ammonia, and the like. Can do.
本発明は、内面が窒化ホウ素製である反応管を用い、窒化性ガスに同伴させた金属アルミニウム粉末を反応管の内面に積極的に衝突させながら供給し、高温場で窒化反応を起こさせるものである。窒化アルミニウム粉末のB含有量は、金属アルミニウム粉末の供給量や、金属アルミニウム粉末の反応管の内面への供給速度（衝突速度）などによってを制御することができる。また、金属アルミニウム粉末の反応管の内面への供給速度（衝突速度）は、反応管に絞り部等を設けることによって容易に行うことができる。金属アルミニウム粉末の供給量は、窒化性ガス１Ｎｍ３あたり１〜３ｋｇが好ましく、その供給速度は窒化性ガスの流速として５０〜１００ｍ／ｓであることが好ましい。また、反応管の温度は１９００〜２２００℃が好ましい。 The present invention uses a reaction tube whose inner surface is made of boron nitride, supplies metal aluminum powder entrained in a nitriding gas while actively colliding with the inner surface of the reaction tube, and causes a nitriding reaction in a high temperature field. It is. The B content of the aluminum nitride powder can be controlled by the supply amount of the metal aluminum powder, the supply speed (collision speed) of the metal aluminum powder to the inner surface of the reaction tube, and the like. In addition, the supply speed (collision speed) of the metal aluminum powder to the inner surface of the reaction tube can be easily performed by providing a throttle portion or the like in the reaction tube. The supply amount of the metal aluminum powder is preferably 1 to 3 kg per 1 Nm 3 of the nitriding gas, and the supply speed is preferably 50 to 100 m / s as the flow rate of the nitriding gas. The temperature of the reaction tube is preferably 1900 to 2200 ° C.
本発明で用いられる窒化アルミニウム粉末の製造装置の一例を図１に示した。反応炉は、高周波誘導加熱方式であり、窒化ホウ素製の反応管３は、その周囲に配設された発熱体８と、それを断熱体９で覆った石英外壁１０とで構成されている。反応管３は絞り部１１を有することが好ましい。７は高周波誘導加熱源、４は測温体である。反応炉の頂部には、金属アルミニウム粉末の供給機１と混合器２とからなる金属アルミニウム粉末の噴射手段が設置されている。混合器では金属アルミニウム粉末と窒化性ガスとが混合される。反応炉の底部は捕集系に接続されており、生成した窒化アルミニウム粉末は、ブロワー６で吸引されて捕集系に導かれ、例えばバッグフィルター、電気集塵機等の捕集装置５で捕集される。 An example of an apparatus for producing aluminum nitride powder used in the present invention is shown in FIG. The reaction furnace is a high frequency induction heating system, and the reaction tube 3 made of boron nitride is composed of a heating element 8 disposed around the reaction tube 3 and a quartz outer wall 10 covered with a heat insulator 9. The reaction tube 3 preferably has a throttle portion 11. 7 is a high frequency induction heating source, and 4 is a temperature measuring body. At the top of the reaction furnace, metallic aluminum powder injection means comprising a metallic aluminum powder feeder 1 and a mixer 2 is installed. In the mixer, the metal aluminum powder and the nitriding gas are mixed. The bottom of the reactor is connected to a collection system, and the produced aluminum nitride powder is sucked by the blower 6 and guided to the collection system, and collected by a collection device 5 such as a bag filter or an electric dust collector. The
本発明のセラミックス焼結体は、本発明の窒化アルミニウム粉末又は本発明の窒化アルミニウム粉末とそれ以外のセラミックス粉末との混合粉末の焼結体からなるものである。本発明のセラミックス焼結体は、本発明の窒化アルミニウム粉末又は本発明の窒化アルミニウム粉末とそれ以外のセラミックス粉末との混合粉末に、必要に応じて焼結助剤を配合し、成形後、焼結する工程を経て製造される。焼結助剤としては、例えばアルミナ、イットリア、カルシア等の粉末が用いられ、混合粉末中、２０質量％まで含有させることができる。 The ceramic sintered body of the present invention is composed of a sintered body of the aluminum nitride powder of the present invention or a mixed powder of the aluminum nitride powder of the present invention and other ceramic powder. The ceramic sintered body of the present invention is mixed with the aluminum nitride powder of the present invention or the mixed powder of the aluminum nitride powder of the present invention and the other ceramic powder, if necessary, and after molding, Manufactured through the process of tying. As the sintering aid, for example, a powder of alumina, yttria, calcia or the like is used, and it can be contained up to 20% by mass in the mixed powder.
焼結は、ホットプレス焼結、常圧焼結の何れであってもよい。ホットプレス焼結は、例えば窒素、アルゴン、一酸化炭素等の非酸化性雰囲気下、又は真空雰囲気下、温度1７００〜２３００℃、圧力５〜４０ＭＰａで行うことが好ましい。一方、常圧焼結は、原料粉末を例えば金型プレス法、静水圧プレス法、泥漿鋳込み成形法、押出し成形法、射出成形法等で成形した後、非酸化性雰囲気下、又は真空雰囲気下、温度1７００℃以上で行うことが好ましい。成形体の焼成は、窒化硼素製又は窒化硼素で内張りされた容器に入れて行うことが好ましい。 Sintering may be either hot press sintering or normal pressure sintering. Hot press sintering is preferably performed, for example, in a non-oxidizing atmosphere such as nitrogen, argon, carbon monoxide, or in a vacuum atmosphere at a temperature of 1700 to 2300 ° C. and a pressure of 5 to 40 MPa. On the other hand, normal pressure sintering is performed by molding the raw material powder by, for example, a die pressing method, an isostatic pressing method, a slurry casting molding method, an extrusion molding method, an injection molding method, etc., and then in a non-oxidizing atmosphere or a vacuum atmosphere. The temperature is preferably 1700 ° C. or higher. The molded body is preferably fired in a container made of boron nitride or lined with boron nitride.
混合粉末が、本発明の窒化アルミニウム粉末とそれ以外のセラミックス粉末との混合粉末である場合、そのセラミックス粉末としては、例えば本発明の窒化アルミニウム粉末以外の窒化アルミニウム粉末、窒化ケイ素粉末、窒化ホウ素粉末、アルミナ粉末、ムライト粉末、シリカ粉末、マグネシア粉末、炭化ケイ素粉末等が用いられ、その種類には特に制約はない。本発明の窒化アルミニウム粉末以外のセラミックス粉末の割合は、混合粉末中、８０質量％以下、特に６０質量％以下を例示することができる。なかでも、本発明の窒化アルミニウム粉末以外のセラミックス粉末として、窒化ホウ素粉末を選択したときに本発明の効果が顕著となる。混合粉末の平均粒径は０．５〜１０μｍであることが好ましい。 When the mixed powder is a mixed powder of the aluminum nitride powder of the present invention and other ceramic powder, examples of the ceramic powder include aluminum nitride powder other than the aluminum nitride powder of the present invention, silicon nitride powder, and boron nitride powder. Alumina powder, mullite powder, silica powder, magnesia powder, silicon carbide powder and the like are used, and there are no particular restrictions on the type thereof. The proportion of the ceramic powder other than the aluminum nitride powder of the present invention can be exemplified by 80% by mass or less, particularly 60% by mass or less in the mixed powder. Among them, the effect of the present invention becomes remarkable when boron nitride powder is selected as the ceramic powder other than the aluminum nitride powder of the present invention. The average particle diameter of the mixed powder is preferably 0.5 to 10 μm.
図１に示される装置を用いて窒化アルミニウム粉末を製造した。反応炉の容量は１７０ｋＶＡ、出力は１００ｋＷである。炉の中央内部には反応管３（窒化ホウ素製、内径４００ｍｍ、全長３０００ｍｍ、炉頂より１０００ｍｍの位置に絞り部がある。）が設置され、その周囲に発熱体８（黒鉛製）が配置され、高周波誘導加熱源７により加熱されて反応官が所定温度に保たれている。反応温度は発熱体中央部に設置した測温体４（グラッシーカーボン管）の温度を光温度計によって測定される。発熱体８は断熱材９（多孔質カーボンビーズ）によって保温され、石英外壁１０（内径６００ｍｍ、全長３０００ｍｍ）で保持されている。生成した窒化アルミニウム粉末は炉底からブロワー６で吸引し捕集装置５（バッグフィルター）で捕集した。 Aluminum nitride powder was produced using the apparatus shown in FIG. The capacity of the reactor is 170 kVA and the output is 100 kW. A reaction tube 3 (made of boron nitride, inner diameter of 400 mm, total length of 3000 mm, with a constricted portion at a position of 1000 mm from the top of the furnace) is installed in the center of the furnace, and a heating element 8 (made of graphite) is arranged around it. The reactor is heated to a predetermined temperature by being heated by the high frequency induction heating source 7. The reaction temperature is determined by measuring the temperature of the temperature measuring element 4 (glassy carbon tube) installed at the center of the heating element with an optical thermometer. The heating element 8 is kept warm by a heat insulating material 9 (porous carbon beads) and is held by a quartz outer wall 10 (inner diameter 600 mm, total length 3000 mm). The produced aluminum nitride powder was sucked from the furnace bottom with a blower 6 and collected with a collecting device 5 (bag filter).
実施例１〜３ 比較例１
金属アルミニウム粉末（純度９９．９７質量％）を金属アルミニウムの供給機（スクリューフィーダー）１より混合機２に搬送し、そこで窒化性ガス（窒素ガス）と混合しながら反応管３内に噴射した。反応管の絞り部の内径と、金属アルミニウム粉末の供給量を表１に示すように変更してＢ含有量の異なる窒化アルミニウム（ＡｌＮ）粉末を製造した。得られた窒化アルミニウム粉末はいずれも純度が９９質量％以上で、平均粒径がほぼ１．５μｍであった。
Examples 1-3 Comparative Example 1
Metal aluminum powder (purity 99.97 mass%) was conveyed from a metal aluminum feeder (screw feeder) 1 to the mixer 2 where it was injected into the reaction tube 3 while mixing with a nitriding gas (nitrogen gas). Aluminum nitride (AlN) powders having different B contents were produced by changing the inner diameter of the throttle part of the reaction tube and the supply amount of the metal aluminum powder as shown in Table 1. Each of the obtained aluminum nitride powders had a purity of 99% by mass or more and an average particle size of about 1.5 μm.
比較例２
電気炉を用いて、上記と同様の原料をカーボン容器中で窒化させB成分の含有しない窒化アルミニウム粉末を合成し、実施例１と同様にして複合材を製造した。
Comparative Example 2
Using an electric furnace, the same raw material as above was nitrided in a carbon container to synthesize aluminum nitride powder containing no B component, and a composite material was produced in the same manner as in Example 1.
得られたＡｌＮ粉末５０質量部、市販のＢＮ粉末（酸素量：１．２質量％、平均粒径：０．８μm）５０質量部、イットリア粉末１質量部をボールミルにて６時間混合し、それを２０ＭＰａの圧力で金型成形後、２００ＭＰａの圧力でＣＩＰ成形し、１気圧の窒素ガス雰囲気中、１９００℃で焼結してＡｌＮ−ＢＮ複合材を製造した。これらの複合材について、レーザーフラッシュ法による熱伝導率は、ビッカース硬度、ＪＩＳ法による３点曲げ強度を測定した。それらの結果を表１に示す。 50 parts by mass of the obtained AlN powder, 50 parts by mass of commercially available BN powder (oxygen amount: 1.2% by mass, average particle size: 0.8 μm), and 1 part by mass of yttria powder were mixed for 6 hours in a ball mill, Was molded at a pressure of 20 MPa, CIP molded at a pressure of 200 MPa, and sintered at 1900 ° C. in a nitrogen gas atmosphere of 1 atm to produce an AlN—BN composite material. About these composite materials, the heat conductivity by the laser flash method measured the Vickers hardness and the 3-point bending strength by JIS method. The results are shown in Table 1.
表１から、本発明の実施例によれば、Ｂ含有量が１０ｐｐｍ以上のＡｌＮ粉末を製造することができた。また、それを用いて製造されたＢＮ−ＡｌＮ複合材は、熱伝導率、硬度、曲げ強度に優れていた。 From Table 1, according to the Example of this invention, AlN powder whose B content is 10 ppm or more was able to be manufactured. Moreover, the BN-AlN composite material manufactured using the same was excellent in thermal conductivity, hardness, and bending strength.
本発明の窒化アルミニウム粉末は、セラミックス焼結体の製造原料の他に、樹脂等のフィラーとして使用することができる。また、本発明のセラミックス焼結体は、基板や鋼鉄工業用部材として使用することができる。 The aluminum nitride powder of the present invention can be used as a filler such as a resin in addition to a raw material for producing a ceramic sintered body. The ceramic sintered body of the present invention can be used as a substrate or a steel industrial member.
１ 金属アルミニウム粉末の供給機
２ 混合器
３ 反応管
４ 測温体
５ 捕集装置
６ ブロワー
７ 高周波誘導加熱源
８ 発熱体
９ 断熱体
１０ 石英外壁
１１ 反応管の絞り部
DESCRIPTION OF SYMBOLS 1 Metal aluminum powder supply machine 2 Mixer 3 Reaction tube 4 Temperature measuring body 5 Collection apparatus 6 Blower 7 High frequency induction heating source 8 Heating body 9 Heat insulator 10 Quartz outer wall 11 Restriction part of reaction tube
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003034511A (en) * | 2001-07-23 | 2003-02-07 | Denki Kagaku Kogyo Kk | Method of manufacturing aluminum nitride powder |
| CN105984859A (en) * | 2015-03-20 | 2016-10-05 | Oci有限公司 | Apparatus and method for producing aluminum nitride powder and aluminum nitride powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003034511A (en) * | 2001-07-23 | 2003-02-07 | Denki Kagaku Kogyo Kk | Method of manufacturing aluminum nitride powder |
| JP4545357B2 (en) * | 2001-07-23 | 2010-09-15 | 電気化学工業株式会社 | Method for producing aluminum nitride powder |
| CN105984859A (en) * | 2015-03-20 | 2016-10-05 | Oci有限公司 | Apparatus and method for producing aluminum nitride powder and aluminum nitride powder |
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