JP5110496B2 - Method for producing NaCl type silicon carbide - Google Patents
Method for producing NaCl type silicon carbide Download PDFInfo
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- JP5110496B2 JP5110496B2 JP2005337667A JP2005337667A JP5110496B2 JP 5110496 B2 JP5110496 B2 JP 5110496B2 JP 2005337667 A JP2005337667 A JP 2005337667A JP 2005337667 A JP2005337667 A JP 2005337667A JP 5110496 B2 JP5110496 B2 JP 5110496B2
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Description
本発明は、高密度のＮａＣｌ型炭化ケイ素を容易に製造することのできるＮａＣｌ型炭化ケイ素の製造方法に関する。 The present invention relates to a method for producing NaCl-type silicon carbide capable of easily producing high-density NaCl-type silicon carbide.
炭化ケイ素（ＳｉＣ）は、高温半導体、フォトニック材料、研磨剤、さらに構造用材料として応用されている。 Silicon carbide (SiC) is applied as a high-temperature semiconductor, a photonic material, an abrasive, and a structural material.
従来知られている炭化ケイ素は、３Ｃ立方晶型（格子定数０．４３６ｎｍ）や、４Ｈ、６Ｈ、１５Ｒ等の六方晶型である。最近、ダイヤモンド粉にシリコン（Ｓｉ）を混ぜ、２５００℃、６ＧＰａの高温高圧下で、高密度のＮａＣｌ型炭化ケイ素（格子定数０．４０８ｎｍ）を合成できることが報告されている（非特許文献１）。
ＮａＣｌ型炭化ケイ素は、理論的にはたとえば３Ｃ構造等の炭化ケイ素を圧縮すれば実現されるはずであるが、実際には、２５００℃、６ＧＰａの高温高圧下でも合成されていない。 Although the NaCl type silicon carbide should theoretically be realized by compressing silicon carbide having a 3C structure or the like, it is not actually synthesized under high temperature and high pressure of 2500 ° C. and 6 GPa.
本発明は、以上の事情に鑑みてなされたものであり、より高性能であると見込まれるＮａＣｌ型炭化ケイ素を容易に製造することのできるＮａＣｌ型炭化ケイ素の製造方法を提供することを解決すべき課題としている。 The present invention has been made in view of the above circumstances, and solves the problem of providing a method for producing NaCl-type silicon carbide that can easily produce NaCl-type silicon carbide that is expected to have higher performance. It should be a challenge.
本発明は、上記の課題を解決するために、孔径が０μｍより大きく１μｍ以下で柱状の細孔が形成された中空体の細孔内にトリクロロメチルシランを１Ｔｏｒｒ〜１００Ｔｏｒｒの減圧下で流通させ、９００℃〜１３００℃の温度で熱分解させて、中空体の内壁にＮａＣｌ型炭化ケイ素を生成させることを特徴としている。
The present invention, in order to you solve the above problem, a pore size of tri chloromethyl silane in the pores of greater than 1μm or less columnar hollow body pores are formed in 0μm under reduced pressure of 1Torr~100Torr It is characterized in that it is made to flow and thermally decomposed at a temperature of 900 ° C. to 1300 ° C. to produce NaCl type silicon carbide on the inner wall of the hollow body.
本発明によれば、高温、高圧を用いず、トリクロロメチルシランの熱分解という簡便な手法で高密度のＮａＣｌ型炭素ケイ素を製造することができる。低コストのトリクロロメチルシランを原料に用い、簡便な電気炉を使用することができるため、ＮａＣｌ型炭化ケイ素を安価に製造することができる。
According to the present invention, high temperature, without the use of high pressure, it is possible to produce a high density of NaCl-type carbon silicon by a simple method that the thermal decomposition of the tri-chloromethyl silane. Since the cost of tri chloromethyl silane used as a raw material, can be used a simple electric furnace, it is possible to inexpensively manufacture the NaCl-type silicon carbide.
以下実施例を示し、本発明のＮａＣｌ型炭化ケイ素の製造方法についてさらに説明する。 Hereinafter, the method for producing NaCl-type silicon carbide of the present invention will be further described with reference to examples.
図１に示したように、孔径が０μｍより大きく１μｍ以下で柱状の細孔１が形成された中空体２の細孔１内にクロロシラン３を流通させる。クロロシラン３の流通は、１Ｔｏｒｒ〜１００Ｔｏｒｒの減圧下で行い、キャリヤーとして水素ガス、アルゴンガス等を使用することができる。クロロシラン３は、中空体２の下方から上方へと導くことができる。クロロシラン３としては、メチルクロロシラン、エチルクロロシラン等が例示され、クロロシラン３は炭化水素を含有するものであってもよい。中空体２は、たとえば、薄膜を所定間隔で離間配置し、柱状の細孔１が形成されたものとすることができる。 As shown in FIG. 1, chlorosilane 3 is circulated in the pores 1 of the hollow body 2 in which the pore diameter is larger than 0 μm and not larger than 1 μm and the columnar pores 1 are formed. The chlorosilane 3 is circulated under a reduced pressure of 1 Torr to 100 Torr, and hydrogen gas, argon gas or the like can be used as a carrier. The chlorosilane 3 can be guided from the lower side to the upper side of the hollow body 2. Examples of the chlorosilane 3 include methylchlorosilane and ethylchlorosilane, and the chlorosilane 3 may contain a hydrocarbon. The hollow body 2 can be formed, for example, by forming thin columnar pores 1 at a predetermined interval to form columnar pores 1.
このような中空体２は電気炉内に配置することができ、クロロシラン３を流通させながら温度９００℃〜１３００℃の温度に加熱する。クロロシラン３は中空体２の細孔１内で熱分解し、炭化ケイ素が生成し、図２に示したように、中空体２の内壁にＮａＣｌ型の炭化ケイ素４が析出する。熱分解に必要な温度は９００℃〜１３００℃の範囲が適当であり、この範囲からはずれるとクロロシラン３の分解効率が低下する。 Such a hollow body 2 can be placed in an electric furnace and heated to a temperature of 900 ° C. to 1300 ° C. while circulating the chlorosilane 3. The chlorosilane 3 is thermally decomposed in the pores 1 of the hollow body 2 to produce silicon carbide, and NaCl-type silicon carbide 4 is deposited on the inner wall of the hollow body 2 as shown in FIG. The temperature required for the thermal decomposition is suitably in the range of 900 ° C. to 1300 ° C. If the temperature is out of this range, the decomposition efficiency of the chlorosilane 3 decreases.
このように、クロロシランの熱分解という簡便な手法によりＮａＣｌ型炭化ケイ素の製造が可能となり、製造に高温、高圧を要しない。クロロシランは安価な物質であり、簡便な電気炉を利用することができるため、ＮａＣｌ型炭化ケイ素の製造を低コストで行うことが可能となる。 In this way, NaCl type silicon carbide can be produced by a simple method of pyrolysis of chlorosilane, and high temperature and high pressure are not required for production. Since chlorosilane is an inexpensive substance and a simple electric furnace can be used, it is possible to manufacture NaCl-type silicon carbide at a low cost.
ＮａＣｌ型炭化ケイ素は、これまでの炭化ケイ素と比較して高密度であり、かつ高剛性を有する材料である。３Ｃ型の炭化ケイ素の約１．３倍の剛性を有することが予想され、炭化ケイ素の中で最も強度の高い物質であると考えられる。特に強度の要求される用途への応用が見込まれる。 NaCl type silicon carbide is a material having a higher density and higher rigidity than conventional silicon carbide. It is expected to have about 1.3 times the rigidity of 3C type silicon carbide, and is considered to be the strongest material among silicon carbide. In particular, application to applications requiring strength is expected.
孔径が０μｍより大きく１μｍ以下で柱状の細孔を有する非晶質アルミナ製の中空体を電気炉内に配置し、この中空体の細孔内に、１２０Ｔｏｒｒ、１０００℃で水素ガスをキャリヤーとしてトリクロロメチルシラン（ＣＨ３ＳｉＣｌ３）を約０．０１モル/分の流
量で下方から上方へ導いた。水素ガスの流量は１０００ＳＣＣＭとした。中空体の内壁に微粉状の析出物が生成した。
A hollow body made of amorphous alumina having a pore diameter larger than 0 μm and not larger than 1 μm and having columnar pores is placed in an electric furnace, and trichlorochloromethane is used as a carrier at 120 Torr and 1000 ° C. in the pores of the hollow body. Methylsilane (CH 3 SiCl 3 ) was introduced from below to above at a flow rate of about 0.01 mol / min. The flow rate of hydrogen gas was 1000 SCCM. A fine powdery precipitate was formed on the inner wall of the hollow body.
析出物を電子顕微鏡により観察した。図３に示したように、析出物は、外径が数ｎｍ〜数十ｎｍのチューブ状の物質であり、多結晶粒から形成されている。図４に示したマイクロ組織から格子間隔を計ると、ＮａＣｌ型炭化ケイ素の２００面間隔の約０．２ｎｍにほぼ一致している。析出物がＮａＣｌ型炭化ケイ素であると同定される。 The precipitate was observed with an electron microscope. As shown in FIG. 3, the precipitate is a tube-shaped substance having an outer diameter of several nanometers to several tens of nanometers, and is formed from polycrystalline grains. When the lattice spacing is measured from the microstructure shown in FIG. 4, the spacing between the 200 planes of NaCl-type silicon carbide is approximately equal to about 0.2 nm. The precipitate is identified as NaCl type silicon carbide.
次いで、Ｘ線回折を行った。図５に３Ｃ型の炭化ケイ素と合成されたＮａＣｌ型炭化ケイ素のＸ線回折パターンを示した。両Ｘ線回折パターンの比較から、ＮａＣｌ型炭化ケイ素はＣ型炭化ケイ素と明らかに異なる構造を有することが分かる。 Next, X-ray diffraction was performed. FIG. 5 shows X-ray diffraction patterns of 3C type silicon carbide and synthesized NaCl type silicon carbide. From a comparison of both X-ray diffraction patterns, it can be seen that NaCl-type silicon carbide has a clearly different structure from C-type silicon carbide.
１ 細孔
２ 中空体
３ クロロシラン
４ ＮａＣｌ型炭化ケイ素
DESCRIPTION OF SYMBOLS 1 Pore 2 Hollow body 3 Chlorosilane 4 NaCl type silicon carbide
Claims (1)
Pore size was circulated under a reduced pressure of 1Torr~100Torr tri chloromethyl silane in the pores of the hollow body pores columnar below larger 1μm than 0μm is formed by thermal decomposition at a temperature of 900 ° C. to 1300 ° C. A method for producing NaCl-type silicon carbide, characterized by producing NaCl-type silicon carbide on the inner wall of a hollow body.
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| JP2005337667A JP5110496B2 (en) | 2005-11-22 | 2005-11-22 | Method for producing NaCl type silicon carbide |
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| JP2005337667A JP5110496B2 (en) | 2005-11-22 | 2005-11-22 | Method for producing NaCl type silicon carbide |
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| JP2007137751A JP2007137751A (en) | 2007-06-07 |
| JP5110496B2 true JP5110496B2 (en) | 2012-12-26 |
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| FR2684091B1 (en) * | 1991-11-21 | 1994-02-25 | Pechiney Recherche | METHOD FOR MANUFACTURING METAL CARBIDES WITH A LARGE SPECIFIC SURFACE UNDER ATMOSPHERIC PRESSURE INERATED GAS SCANNING. |
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