JP5152654B2 - Aluminum silicon carbide powder and method for producing the same - Google Patents
Aluminum silicon carbide powder and method for producing the same Download PDFInfo
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本発明は、六方晶系の結晶構造を持つアルミニウムケイ素炭化物粉末とその製造方法に関する。 The present invention relates to an aluminum silicon carbide powder having a hexagonal crystal structure and a method for producing the same.
アルミニウムケイ素炭化物（Ａｌ４ＳｉＣ４）は融点が約２０３７℃と高く、カーボンと比較して耐酸化性に優れることから、高温・構造材料としての応用が期待されている。また、カーボン／カーボン複合材料や耐火物に添加することにより耐酸化性や機械特性の向上も期待されている。
Ａｌ４ＳｉＣ４は、従来、金属アルミニウム、ケイ素、カーボン粉末の混合物の熱処理（非特許文献１）、酸化アルミニウム、二酸化ケイ素、グラファイトの混合物の熱炭素還元反応（非特許文献２）、アルミニウム炭化物、Ａｌ４Ｃ３、炭化ケイ素、ＳｉＣの混合物の熱処理（非特許文献１、３、４）、金属アルミニウム、ケイ素、カーボン、カオリンの混合物の熱炭素還元反応（非特許文献５）、モンモリロナイト、ポリアクリロニトリルの熱炭素還元反応（非特許文献６）により合成、が試みられているが、最終生成物に得られたＡｌ４ＳｉＣ４の粒子形状は不定形であり、理論上、六方晶系特有の形状とされる、六角板状の結晶性の高い粒子は得られていない。
Al 4 SiC 4 is conventionally a heat treatment of a mixture of metallic aluminum, silicon and carbon powder (Non-Patent Document 1), a thermal carbon reduction reaction of a mixture of aluminum oxide, silicon dioxide and graphite (Non-Patent Document 2), aluminum carbide, Heat treatment of a mixture of Al 4 C 3 , silicon carbide and SiC (Non-patent Documents 1, 3, and 4), thermal carbon reduction reaction of a mixture of metallic aluminum, silicon, carbon, and kaolin (Non-patent Document 5), montmorillonite, polyacrylonitrile Has been attempted by a thermal carbon reduction reaction (Non-patent Document 6) of Al 4 SiC 4 , but the particle shape of Al 4 SiC 4 obtained in the final product is indefinite, and theoretically a shape unique to the hexagonal system Hexagonal plate-like particles with high crystallinity are not obtained.
Ａｌ４ＳｉＣ４は高い耐酸化性、高温機械特性を持つが、結晶性の高い粒子の合成は難しい。
これは、従来、主に固相原料を混合したのちに熱処理を行っていたため、原料粉末を均一に混合することが難しく、生成反応として固相反応を主としているため反応の進行が遅く、結晶性の高いＡｌ４ＳｉＣ４を得ることが難しかった。
本発明は、このような従来得られなかった結晶性の良いＡｌ４ＳｉＣ４を得ると同時に、その製造技術を確立することを課題とする。
Al 4 SiC 4 has high oxidation resistance and high temperature mechanical properties, but it is difficult to synthesize particles with high crystallinity.
In the past, heat treatment was performed mainly after mixing the solid phase raw material, so it was difficult to mix the raw material powder uniformly, and the reaction progressed slowly because the main reaction was the solid phase reaction as the formation reaction. It was difficult to obtain high Al 4 SiC 4 .
An object of the present invention is to obtain Al 4 SiC 4 with good crystallinity, which has not been obtained in the past, and at the same time establish a manufacturing technique thereof.
発明１のアルミニウムケイ素炭化物粉末は、その結晶構造が六方晶であり、粒子の形状が六角板状であることを特徴とする。 The aluminum silicon carbide powder of the invention 1 is characterized in that the crystal structure is hexagonal and the shape of the particles is hexagonal plate.
発明２は、発明１のアルミニウムケイ素炭化物粉末において、Ｃ軸に垂直方向に選択的に成長して六角板状となっていることを特徴とする。 Invention 2 is characterized in that the aluminum silicon carbide powder of Invention 1 is selectively grown in a direction perpendicular to the C-axis to form a hexagonal plate.
発明３は、発明１又は２のアルミニウムケイ素炭化物粉末の製造方法であって、アルミニウム源と炭素源とケイ素源とからなる原料粉末を、真空あるいは不活性雰囲気中で熱処理して、アルミニウムケイ素炭化物とすることを特徴とする。 Invention 3 is a method for producing the aluminum silicon carbide powder of Invention 1 or 2, wherein a raw material powder comprising an aluminum source, a carbon source and a silicon source is heat-treated in a vacuum or in an inert atmosphere to obtain an aluminum silicon carbide powder. It is characterized by doing.
発明４は、発明３のアルミニウムケイ素炭化物粉末の製造方法において、アルミニウム源として水酸化アルミニウムを用いることを特徴とする。 Invention 4 is characterized in that in the method for producing aluminum silicon carbide powder of Invention 3, aluminum hydroxide is used as an aluminum source.
発明５は、発明３又は４のアルミニウムケイ素炭化物粉末の製造方法において、熱処理前に混合粉末を加圧成形により成形体を作製した後、熱処理することを特徴とする。 The invention 5 is characterized in that, in the method for producing an aluminum silicon carbide powder of the invention 3 or 4, a molded product is produced by pressure molding of the mixed powder before the heat treatment and then heat-treated.
本発明者は上記課題を解決するため、種々の原料を用いてＡｌ−Ｓｉ−Ｃ系化合物粉末の合成を行った結果、六角板状で結晶性の良いＡｌ４ＳｉＣ４粉末を合成するに至った。 As a result of synthesizing Al—Si—C-based compound powder using various raw materials in order to solve the above problems, the present inventors have synthesized Al 4 SiC 4 powder having a hexagonal plate shape and good crystallinity. It was.
本発明において、アルミニウム源としてアルミニウム、あるいはアルミニウム化合物、炭素源として炭素あるいは熱処理することにより炭素となる化合物、ケイ素源としてケイ素、あるいはケイ素化合物を原料として用いる。混合する割合は、Ａｌ４ＳｉＣ４組成であるが、熱処理中の反応により気相成分が発生するため、混合する際、より均一に混合を行うためには、アルミニウム源、炭素源、ケイ素源のうち少なくとも１種類は、液相であることが望ましい。これらをビーカー中でマグネチックスターラーを用いたり、ボールミル、遊星ミル等を用いたりして十分に混合する。得られた混合物を十分に乾燥した後、アルゴン気流中、約１０００℃まで熱分解処理する。この処理により、１０００℃までの処理で発生する気相成分をさせ、より高温での熱処理で不純物の混入を防ぐ。
このようにして得られたものを、カーボン製のルツボ中で、真空あるいはアルゴン等の不活性ガス中で1800℃（５０℃単位、以下同じ）から１９００℃で加熱する。中間生成物のAl4O4Cが約１８５０℃で溶融し始めるため、１９００℃よりも高温での加熱は、Ａｌ４ＳｉＣ４の生成には不利である。反応時間はＡｌ４ＳｉＣ４の生成を十分進め、粒成長させるためには長時間が望ましいが、粉末の焼結性の点からは、粒子径は小さい方が望ましく、熱処理時間は短い方がよい。
反応を十分進めるためには、ホットプレス法を用いたり、ルツボに充填する前に加圧法による予備成形を行うこともある。この方法により、六角板状の結晶性の良いＡｌ４ＳｉＣ４粒子が得られる。
なお、その後、必要に応じ、残留炭素分を取り除く処理を行うことも可能である。
In the present invention, aluminum as an aluminum source or an aluminum compound, carbon as a carbon source or a compound which becomes carbon by heat treatment, silicon as a silicon source, or a silicon compound is used as a raw material. The mixing ratio is Al 4 SiC 4 composition, but a gas phase component is generated by the reaction during the heat treatment. Therefore, in order to mix more uniformly when mixing, the aluminum source, the carbon source, and the silicon source are mixed. At least one of them is preferably a liquid phase. These are thoroughly mixed in a beaker using a magnetic stirrer, a ball mill, a planetary mill or the like. The resulting mixture is sufficiently dried and then pyrolyzed to about 1000 ° C. in an argon stream. By this treatment, gas phase components generated by the treatment up to 1000 ° C. are generated, and impurities are prevented from being mixed by heat treatment at a higher temperature.
The product thus obtained is heated from 1800 ° C. (in units of 50 ° C., the same applies hereinafter) to 1900 ° C. in a vacuum crucible or an inert gas such as argon. Since the intermediate product Al 4 O 4 C begins to melt at about 1850 ° C., heating above 1900 ° C. is disadvantageous for the production of Al 4 SiC 4. The reaction time is preferably long in order to sufficiently advance the generation of Al 4 SiC 4 and grow grains, but from the viewpoint of sinterability of the powder, a smaller particle size is desirable, and a shorter heat treatment time is better. .
In order to sufficiently advance the reaction, a hot press method may be used, or a pre-molding may be performed by a pressure method before filling the crucible. By this method, hexagonal plate-like Al 4 SiC 4 particles having good crystallinity can be obtained.
After that, it is possible to remove the residual carbon as necessary.
水酸化アルミニウム、シリカ、フェノール樹脂を、モル比でＡｌ（ＯＨ）３：ＳｉＯ２：Ｃ＝４：１：１２となるように、エタノールを分散媒として、プラスチック製のポット中、炭化ケイ素製のボールを用いて２４時間ボールミル混合した。得られた混合物を乾燥後、架橋反応を進めるため、真空乾燥機中１００℃で１２時間、熱処理を行った。
得られたゲル状物質を石英の反応管内でアルゴン気流中、１０００℃で１／２時間、熱分解処理した。熱分解後の粉末を、カーボンルツボ中、真空あるいはアルゴン気流中、１８００℃、１９００℃で３時間熱処理した。
得られた粉末を粉末Ｘ回折法により分析した結果（図１参照）、Ａｌ４ＳｉＣ４が主たる結晶相として確認された。（１０１）に起因する２θ＝３１．８１０度付近のピーク高さをＩ３１．８１０、（００１０）に起因する２θ＝４１．６５８度付近のピーク高さをＩ４１．６８５とすると、ＩＣＤＤカード３５−１０７２ではＩ４１．６８５／Ｉ３１．８１０＝０．７で、Ｉ３１．８１０＞Ｉ４１．６８５あるが、本結果では、Ｉ３１．８１０＜Ｉ４１．６８５であり、Ｃ軸に垂直な方向への結晶性が高いことが示唆される。また、走査型電子顕微鏡を用いて粒子を観察した結果（図２参照）、六角板状の粒子が多数確認された。これは、六方晶系であるＡｌ４ＳｉＣ４の自形が顕著に現れたものであり、粉末Ｘ線回折の結果からもわかるように、結晶性の高いＡｌ４ＳｉＣ４が得られた。（表１、Ｎｏ．２，３）
結晶性が高いと、
六角板状の結晶がより平になるように成長する。結晶性が高くなる指標としてＩ４１．６８５／Ｉ３１．８１０値を算定して比較した。
Aluminum hydroxide, silica, and phenol resin are made of silicon carbide in a plastic pot using ethanol as a dispersion medium so that the molar ratio is Al (OH) 3 : SiO 2 : C = 4: 1: 12. Ball mill mixing was performed using a ball for 24 hours. After drying the obtained mixture, heat treatment was performed at 100 ° C. for 12 hours in a vacuum dryer in order to proceed with the crosslinking reaction.
The obtained gel-like substance was pyrolyzed in a quartz reaction tube in an argon stream at 1000 ° C. for 1/2 hour. The pyrolyzed powder was heat-treated at 1800 ° C. and 1900 ° C. for 3 hours in a carbon crucible, vacuum or argon stream.
As a result of analyzing the obtained powder by the powder X diffraction method (see FIG. 1), Al 4 SiC 4 was confirmed as a main crystal phase. The peak height of around 2 [Theta] = 31.810 degrees due to (101) I 31.810, When I 41.685 peak heights around 2 [Theta] = 41.658 degrees due to (0010), ICDD card In 35-1072, I 41.85 / I 31.810 = 0.7 and I 31.810 > I 41.585 , but in this result, I 31.810 <I 41.855 , It is suggested that the crystallinity in the vertical direction is high. Further, as a result of observing the particles using a scanning electron microscope (see FIG. 2), a large number of hexagonal plate-like particles were confirmed. This is a remarkable manifestation of the hexagonal Al 4 SiC 4 self-form, and as can be seen from the results of powder X-ray diffraction, Al 4 SiC 4 having high crystallinity was obtained. (Table 1, No. 2, 3)
If the crystallinity is high,
Hexagonal plate-like crystals grow so as to become flatter. As an index for increasing crystallinity, I 41.855 / I 31.810 values were calculated and compared.
水酸化アルミニウム、シリカ、フェノール樹脂を、モル比でＡｌ（ＯＨ）３：ＳｉＯ２：Ｃ＝４：１：１２となるように、エタノールを分散媒として、プラスチック製のポット中、炭化ケイ素製のボールを用いて２４時間ボールミル混合した。得られた混合物を乾燥後、架橋反応を進めるため、真空乾燥機中１００℃で１２時間、熱処理を行った。得られたゲル状物質を石英の反応管内でアルゴン気流中、１０００℃で３０分間、熱分解処理した。熱分解後の粉末を加圧成形により予備成形し、カーボンルツボ中、真空あるいはアルゴン気流中、１８００℃で３時間熱処理した。得られた粉末を粉末Ｘ回折法により分析した結果（図３参照）、Ａｌ４ＳｉＣ４が主たる結晶相として確認された。Ｉ３１．８１０＜Ｉ４１．６８５であった。走査型電子顕微鏡を用いて粒子を観察した結果（図４参照）、六角板状の粒子が多数確認された。７００℃で１２時間、大気雰囲気にて、熱処理を行うことで、残留炭素分を取り除くことが可能である。 Aluminum hydroxide, silica, and phenol resin are made of silicon carbide in a plastic pot using ethanol as a dispersion medium so that the molar ratio is Al (OH) 3 : SiO 2 : C = 4: 1: 12. Ball mill mixing was performed using a ball for 24 hours. After drying the obtained mixture, heat treatment was performed at 100 ° C. for 12 hours in a vacuum dryer in order to proceed with the crosslinking reaction. The obtained gel-like substance was pyrolyzed in an argon stream at 1000 ° C. for 30 minutes in a quartz reaction tube. The pyrolyzed powder was preformed by pressure molding and heat treated at 1800 ° C. for 3 hours in a carbon crucible, vacuum or argon stream. As a result of analyzing the obtained powder by the powder X diffraction method (see FIG. 3), Al 4 SiC 4 was confirmed as a main crystal phase. It was I 31.810 <I 41.85 . As a result of observing the particles using a scanning electron microscope (see FIG. 4), a large number of hexagonal plate-like particles were confirmed. Residual carbon can be removed by heat treatment at 700 ° C. for 12 hours in an air atmosphere.
特に、予備成形体を、カーボンダイス中、アルゴン気流中、１８００℃で３時間、ホットプレス法により熱処理し、得られた粉末から炭素分を取り除くため７００℃で１２時間、大気雰囲気にて熱処理を行うと、得られた粉末は、粉末Ｘ回折法により分析した結果（図５参照）、Ａｌ４ＳｉＣ４のみが結晶相として確認された。Ｉ３１．８１０＜Ｉ４１．６８５であった。走査型電子顕微鏡を用いて粒子を観察した結果（図６参照）、六角板状の粒子が確認された。（表１、Ｎｏ．４，５）
なお、前記アルゴン気流中に代わり真空にて熱処理することによっても同様な結果を得られるものと考えられる。
In particular, the preform was heat-treated in a carbon die in an argon stream at 1800 ° C. for 3 hours by a hot press method, and heat treatment was performed in an air atmosphere at 700 ° C. for 12 hours in order to remove carbon from the obtained powder. Doing, resulting powder (see FIG. 5) was analyzed by a powder X diffraction, only Al 4 SiC 4 was identified as a crystal phase. It was I 31.810 <I 41.85 . As a result of observing the particles using a scanning electron microscope (see FIG. 6), hexagonal plate-like particles were confirmed. (Table 1, No. 4, 5)
In addition, it is thought that the same result can be obtained also by heat-processing in a vacuum instead of the said argon stream.
水酸化アルミニウム、シリカ、フェノール樹脂を、モル比でＡｌ（ＯＨ）３：ＳｉＯ２：Ｃ＝４：１：６〜１０となるように、エタノールを分散媒として、プラスチック製のポット中、炭化ケイ素製のボールを用いて２４時間ボールミル混合した。得られた混合物を乾燥後、架橋反応を進めるため、真空乾燥機中１００℃で１２時間、熱処理を行った。得られたゲル状物質を石英の反応管内でアルゴン気流中、１０００℃で１／２時間、熱分解処理した。熱分解後の粉末を加圧成形により予備成形し、カーボンルツボ中、真空あるいはアルゴン気流中、１７５０℃で３時間熱処理した。得られた粉末を粉末Ｘ回折法により分析した結果（図７参照）、Ａｌ４ＳｉＣ４が主たる結晶相として確認された。特に、フェノール樹脂のモル比が８の場合、Ａｌ４ＳｉＣ４単相が得られた。Ｉ３１．８１０とＩ４１．６８５の比は、６〜１０のときはＩ３１．８１０＜Ｉ４１．６８５だった。走査型電子顕微鏡を用いて粒子を観察した結果（図８参照）、６〜１０のときは六角板状の粒子が多数確認された。（表１、Ｎｏ．７〜９） Silicon carbide in a plastic pot with aluminum hydroxide, silica, and phenol resin as a dispersion medium so that the molar ratio of Al (OH) 3 : SiO 2 : C = 4: 1: 6-10 Ball mill mixing was performed for 24 hours using a manufactured ball. After drying the obtained mixture, heat treatment was performed at 100 ° C. for 12 hours in a vacuum dryer in order to proceed with the crosslinking reaction. The obtained gel-like substance was pyrolyzed in a quartz reaction tube in an argon stream at 1000 ° C. for 1/2 hour. The pyrolyzed powder was preformed by pressure molding and heat treated at 1750 ° C. for 3 hours in a carbon crucible, vacuum or argon stream. As a result of analyzing the obtained powder by the powder X diffraction method (see FIG. 7), Al 4 SiC 4 was confirmed as a main crystal phase. In particular, when the molar ratio of the phenol resin was 8, an Al 4 SiC 4 single phase was obtained. The ratio of I 31.810 to I 41.865 was I 31.810 <I 41.85 when it was 6-10. As a result of observing the particles using a scanning electron microscope (see FIG. 8), a large number of hexagonal plate-like particles were confirmed when the number was 6 to 10. (Table 1, No. 7-9)
水酸化アルミニウム、シリカ、フェノール樹脂を、モル比でＡｌ（ＯＨ）３：ＳｉＯ２：Ｃ＝４：０．９４〜０．７６：８となるように、エタノールを分散媒として、プラスチック製のポット中、炭化ケイ素製のボールを用いて２４時間ボールミル混合した。得られた混合物を乾燥後、架橋反応を進めるため、真空乾燥機中１００℃で１２時間、熱処理を行った。得られたゲル状物質を石英の反応管内でアルゴン気流中、１０００℃で１／２時間、熱分解処理した。熱分解後の粉末を加圧成形により予備成形し、カーボンルツボ中、真空あるいはアルゴン気流中、１７５０℃で３時間熱処理した。得られた粉末を粉末Ｘ回折法により分析した結果（図９参照）、Ａｌ４ＳｉＣ４が主たる結晶相として確認された。特に、シリカのモル比が０．８２の場合、Ａｌ４ＳｉＣ４単相が得られた。Ｉ３１．８１０とＩ４１．６８５の比は、いずれの場合もＩ３１．８１０＜Ｉ４１．６８５だった。（表１、Ｎｏ．１０〜１４） A plastic pot containing aluminum hydroxide, silica, and phenol resin in a molar ratio of Al (OH) 3 : SiO 2 : C = 4: 0.94 to 0.76: 8 using ethanol as a dispersion medium. Inside, ball mill mixing was performed for 24 hours using silicon carbide balls. After drying the obtained mixture, heat treatment was performed at 100 ° C. for 12 hours in a vacuum dryer in order to proceed with the crosslinking reaction. The obtained gel-like substance was pyrolyzed in a quartz reaction tube in an argon stream at 1000 ° C. for 1/2 hour. The pyrolyzed powder was preformed by pressure molding and heat treated at 1750 ° C. for 3 hours in a carbon crucible, vacuum or argon stream. As a result of analyzing the obtained powder by the powder X diffraction method (see FIG. 9), Al 4 SiC 4 was confirmed as a main crystal phase. In particular, when the molar ratio of silica was 0.82, an Al 4 SiC 4 single phase was obtained. The ratio of I 31.810 and I 41.685 is, in any case was I 31.810 <I 41.685. (Table 1, No. 10-14)
水酸化アルミニウム、シリカ、フェノール樹脂を、モル比でＡｌ（ＯＨ）３：ＳｉＯ２：Ｃ＝４：１：１２のとなるように、エタノールを分散媒として、プラスチック製のポット中、炭化ケイ素製のボールを用いて２４時間ボールミル混合した。得られた混合物を乾燥後、架橋反応を進めるため、真空乾燥機中１００℃で１２時間、熱処理を行った。得られたゲル状物質を石英の反応管内でアルゴン気流中、１０００℃で３０分間、熱分解処理した。熱分解後の粉末を、カーボンルツボ中、真空あるいはアルゴン気流中、１７００℃で３時間熱処理した。得られた粉末を粉末Ｘ回折法により分析した結果（図１０参照）、Ａｌ２Ｏ３が主たる結晶相として確認された。Ａｌ４ＳｉＣ４も結晶相として確認されたが、第２相に留まった。走査型電子顕微鏡を用いて粒子を観察した結果（図１１参照）、観察される粒子は不定形であり、六角板状の粒子は確認されなかった。これは、Ａｌ４ＳｉＣ４は生成しているものの、結晶性が低いためと考察される。（表１、Ｎｏ．１）本比較例では１７００℃での熱処理時間は３時間であるが、熱処理時間を長くすることにより、Ａｌ４ＳｉＣ４の生成反応を進め、結晶性の高いＡｌ４ＳｉＣ４粒子を得ることは可能である。 Aluminum hydroxide, silica and phenol resin are made of silicon carbide in a plastic pot using ethanol as a dispersion medium so that the molar ratio of Al (OH) 3 : SiO 2 : C = 4: 1: 12 And ball mill mixing for 24 hours. After drying the obtained mixture, heat treatment was performed at 100 ° C. for 12 hours in a vacuum dryer in order to proceed with the crosslinking reaction. The obtained gel-like substance was pyrolyzed in an argon stream at 1000 ° C. for 30 minutes in a quartz reaction tube. The pyrolyzed powder was heat-treated at 1700 ° C. for 3 hours in a carbon crucible, vacuum or argon stream. As a result of analyzing the obtained powder by the powder X diffraction method (see FIG. 10), Al 2 O 3 was confirmed as a main crystal phase. Al 4 SiC 4 was also confirmed as a crystal phase, but remained in the second phase. As a result of observing the particles using a scanning electron microscope (see FIG. 11), the observed particles were indeterminate and no hexagonal plate-like particles were confirmed. This is considered because Al 4 SiC 4 is generated but the crystallinity is low. (Table 1, No. 1) In this comparative example, the heat treatment time at 1700 ° C. is 3 hours, but by increasing the heat treatment time, the formation reaction of Al 4 SiC 4 is advanced and Al 4 SiC having high crystallinity is obtained. It is possible to obtain 4 particles.
水酸化アルミニウム、シリカ、フェノール樹脂を、モル比でＡｌ（ＯＨ）３：ＳｉＯ２：Ｃ＝４：１：１２となるように、エタノールを分散媒として、プラスチック製のポット中、炭化ケイ素製のボールを用いて２４時間ボールミル混合した。得られた混合物を乾燥後、架橋反応を進めるため、真空乾燥機中１００℃で１２時間、熱処理を行った。得られたゲル状物質を石英の反応管内でアルゴン気流中、１０００℃で１／２時間、熱分解処理した。熱分解後の粉末を加圧成形により予備成形し、カーボンルツボ中、真空あるいはアルゴン気流中、１７５０℃で３時間熱処理した。得られた粉末を粉末Ｘ回折法により分析した結果（図１２参照）、Ａｌ４ＳｉＣ４が主たる結晶相として確認された。Ｉ３１．８１０とＩ４１．６８５の比は、Ｉ３１．８１０＞Ｉ４１．６８５であった。走査型電子顕微鏡を用いて粒子を観察した結果（図１３参照）、粒子は不定形であった。これは、炭素が過剰に存在すると、Ａｌ４ＳｉＣ４の粒成長が抑制されるためと考えられる。（表１、Ｎｏ．６） Aluminum hydroxide, silica, and phenol resin are made of silicon carbide in a plastic pot using ethanol as a dispersion medium so that the molar ratio is Al (OH) 3 : SiO 2 : C = 4: 1: 12. Ball mill mixing was performed using a ball for 24 hours. After drying the obtained mixture, heat treatment was performed at 100 ° C. for 12 hours in a vacuum dryer in order to proceed with the crosslinking reaction. The obtained gel-like substance was pyrolyzed in a quartz reaction tube in an argon stream at 1000 ° C. for 1/2 hour. The pyrolyzed powder was preformed by pressure molding and heat treated at 1750 ° C. for 3 hours in a carbon crucible, vacuum or argon stream. As a result of analyzing the obtained powder by the powder X diffraction method (see FIG. 12), Al 4 SiC 4 was confirmed as a main crystal phase. The ratio of I 31.810 to I 41.865 was I 31.810 > I 41.585 . As a result of observing the particles using a scanning electron microscope (see FIG. 13), the particles were amorphous. This is thought to be because the grain growth of Al 4 SiC 4 is suppressed when carbon is present in excess. (Table 1, No. 6)
本発明は、融点が高く、カーボンと比較して高い耐酸化性をもつ、Ａｌ４ＳｉＣ４の結晶性の高い粒子、およびその製造方法に関するものであり、このようにして得られた粒子は、高温・構造用の複合材料、耐火物の分散粒子として好適である。また、Ａｌ４ＳｉＣ４の高純度焼結体用の原料粒子として好適である。 The present invention relates to a highly crystalline particle of Al 4 SiC 4 having a high melting point and high oxidation resistance compared to carbon, and a method for producing the same, and the particles thus obtained include: Suitable for high temperature / structural composite materials and refractory dispersed particles. Moreover, it is suitable as a raw material particle for high purity sintered bodies of Al 4 SiC 4 .
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