JP2006124831A - Reaction vessel for vapor phase growth, and vapor phase growth method - Google Patents

Reaction vessel for vapor phase growth, and vapor phase growth method Download PDF

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JP2006124831A
JP2006124831A JP2005284931A JP2005284931A JP2006124831A JP 2006124831 A JP2006124831 A JP 2006124831A JP 2005284931 A JP2005284931 A JP 2005284931A JP 2005284931 A JP2005284931 A JP 2005284931A JP 2006124831 A JP2006124831 A JP 2006124831A
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reaction vessel
gas
phase growth
vapor phase
reaction
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Kiyoshi Sato
清 佐藤
Naoki Abe
直毅 阿部
Akira Asano
昭 浅野
Junichi Irimura
純一 入村
Naohiko Saeki
尚彦 佐伯
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Nichias Corp
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<P>PROBLEM TO BE SOLVED: To enhance the durability and reliability of a vaporphase growth vessel and to perform precipitation by a vapor growth method with high efficiency. <P>SOLUTION: The reaction vessel for vapor phase growth is used to cause vapor phase growth of a substance to be precipitated by reaction of treatment gas on an object to be treated by housing the object to be treated therein and introducing the treatment gas therein. The reaction vessel is a double tube structure comprising an outer tube provided with impact resistance and thermal impact resistance and an inner tube provided with heat resistance and corrosion resistance, wherein the space between the outer tube and the inner tube is airtightly maintained and the space is maintained under the nonoxidizing gaseous atmosphere. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

本発明は、気相成長装置に使用される気相成長用反応容器、並びに前記気相成長用反応容器を用いて行なう気相成長方法に関する。   The present invention relates to a vapor phase growth reaction vessel used in a vapor phase growth apparatus, and a vapor phase growth method performed using the vapor phase growth reaction vessel.

気相成長法は、被処理体を収容した反応容器に処理ガスを導入し、熱分解反応により被処理体上に処理ガスに由来する反応生成物を析出させる方法であり、種々の用途に使用されている。気相成長法の一つとして、多孔質基材を被処理体とし、その気孔内部を含めてセラミックスや炭素、金属等の各種物質を析出させる気相化学含浸法（ＣＶＩ：Ｃｈｅｍｉｃａｌ Ｖａｐｏｒ Ｉｎｆｉｌｔｒａｔｉｏｎ）が知られている。このＣＶＩ法は、処理ガスを多孔質基材の気孔内部にまで送り込み、多孔質材の骨格にも処理ガスに由来する反応生成物を析出させる方法である。   Vapor phase epitaxy is a method in which a processing gas is introduced into a reaction vessel containing an object to be processed, and a reaction product derived from the processing gas is deposited on the object to be processed by a thermal decomposition reaction. Has been. As one of the vapor phase growth methods, there is a vapor phase chemical impregnation method (CVI: Chemical Vapor Infiltration) in which a porous substrate is used as an object to be processed and various substances such as ceramics, carbon, and metal are deposited including the inside of the pores. Are known. This CVI method is a method in which a processing gas is fed into the pores of a porous substrate, and a reaction product derived from the processing gas is also deposited on the skeleton of the porous material.

ＣＶＩ法は、析出プロセスの形式により、減圧ＣＶＩ、強制流型ＣＶＩ、パルスＣＶＩ等に分類される。減圧ＣＶＩは、反応容器内を減圧にすることで、気体の拡散速度を増加させ、気孔内部への物質輸送を促進させる方法である。強制流型ＣＶＩは、多孔質基材にガスを流通させ、強制的に気孔内に処理ガスを導入し、生成ガスを排出する方法である。パルスＣＶＩ法は、反応容器の減圧と昇圧とを短周期で繰り返し行い、間歇的に処理ガスを気孔内部に供給し、生成ガスを排出する方法である。中でも、ガス供給・排出の形式から、パルスＣＶＩ法は、多孔質基材内部への均質成膜性に優れることが知られている。   The CVI method is classified into reduced pressure CVI, forced flow type CVI, pulse CVI, etc., depending on the type of precipitation process. The reduced pressure CVI is a method of increasing the gas diffusion rate by reducing the pressure in the reaction vessel and promoting the material transport into the pores. The forced flow type CVI is a method in which a gas is circulated through a porous substrate, a processing gas is forcibly introduced into the pores, and a generated gas is discharged. The pulse CVI method is a method in which the pressure reduction and pressure increase of the reaction vessel are repeated in a short cycle, the processing gas is intermittently supplied into the pores, and the generated gas is discharged. Among these, the pulse CVI method is known to be excellent in uniform film formation inside a porous substrate because of the form of gas supply / discharge.

但し、パルスＣＶＩ法では、反応容器が減圧と昇圧とを繰り返し受けるため、反応容器には特に耐圧性が要求される。従来は、石英ガラス製の反応容器が使用されているが（特許文献１、特許文献２参照）、石英ガラスは１０００℃以上で軟化変形するので、反応温度１０００℃以上を必要とする材料を析出させることはできない。特に装置を大型化した場合に、軟化変形の問題が大きくなる。また、石英ガラスは衝撃や過荷重により、簡単に脆性破壊するという欠点を持つ。   However, in the pulse CVI method, since the reaction vessel repeatedly receives pressure reduction and pressure increase, the reaction vessel is particularly required to have pressure resistance. Conventionally, reaction vessels made of quartz glass have been used (see Patent Document 1 and Patent Document 2). Since quartz glass is softened and deformed at 1000 ° C. or higher, a material that requires a reaction temperature of 1000 ° C. or higher is deposited. I can't let you. In particular, when the apparatus is enlarged, the problem of softening deformation increases. In addition, quartz glass has a drawback that it easily brittlely breaks due to impact or overload.

１０００℃以上の反応温度を実現するために、石英ガラスの代わりに、ＳｉＣ等の耐熱セラミックスを用いる方法も考えられる。しかし、大型のセラミック部品は、セラミックが持つ脆性ゆえに、強度の保証が難しい。また、生産性を上げるために、反応容器の急速昇温、急速冷却を行おうとすると、セラミックスの耐熱衝撃性の弱さが問題になる。   In order to realize a reaction temperature of 1000 ° C. or higher, a method using heat-resistant ceramics such as SiC instead of quartz glass is also conceivable. However, it is difficult to guarantee the strength of large ceramic parts due to the brittleness of ceramics. In addition, in order to increase the productivity, if the temperature of the reaction vessel is rapidly raised and rapidly cooled, the weak thermal shock resistance of ceramics becomes a problem.

石英ガラスやセラミックスの代わりに、耐熱金属で反応管を作成することも考えられるが、この場合、耐食性が問題となる。例えばインコネル等Ｎｉ基の耐熱合金を使用した場合、Ｓｉを含む処理ガスに高温で接触させると、その表面にＮｉ−Ｓｉ系の金属間化合物が生成する。Ｎｉ−Ｓｉ系の金属間化合物で融点の最も低いのはＮｉＳｉで、その共融点は９７０℃である。そのため、反応容器の温度を９７０℃以上に上げると、液相ＮｉＳｉによる、Ｎｉ基合金の侵食が進み、最悪の場合には腐蝕孔が開く。Ｎｉ基以外の耐熱合金にも、Ｎｉが含まれているので同様の問題が発生する。   It can be considered that the reaction tube is made of a heat-resistant metal instead of quartz glass or ceramics, but in this case, corrosion resistance becomes a problem. For example, when a Ni-based heat-resistant alloy such as Inconel is used, a Ni—Si based intermetallic compound is formed on the surface of the Ni-based heat-resistant alloy when it is brought into contact with a processing gas containing Si at a high temperature. NiSi has the lowest melting point among Ni-Si based intermetallic compounds, and its eutectic point is 970 ° C. Therefore, when the temperature of the reaction vessel is increased to 970 ° C. or more, the Ni-base alloy is eroded by the liquid phase NiSi, and in the worst case, corrosion holes are opened. A similar problem occurs because heat-resistant alloys other than Ni-based alloys also contain Ni.

また、炭素質の反応管を金属製の密閉容器に収め、密閉容器内に収めたヒータで炭素質反応管を加熱する構成の反応容器（特許文献３参照）や、更に炭素質反応管の表面をガス不透過性のＳｉＣで被覆して反応管の気密性を向上させた反応容器（特許文献４参照）も知られている。しかし、特許文献３の反応容器では、（１）冷却速度が遅い：密閉容器内に、反応管、ヒータ、断熱材が収められているので、熱容量が大きく冷めにくい、（２）試料の取り出しが頻繁である：試料が２重の密閉容器に収められているので、２つ以上のフランジを外さないと試料を取り出せない、という問題がある。また、特許文献４の反応容器では、ＳｉＣ被覆炭素管の信頼性に問題がある。実施例には５０回の運転に耐えたとあるが、例えば、急速冷却を行なうことで、ＳｉＣ層に亀裂が入れば、炭素質反応管の酸化が急激に進む危険がある。また、取り扱い上の不注意で、工具等を反応管にぶつけると、ＳｉＣ層が脱落し、やはり炭素質反応管の酸化が進む。パルスＣＶＩ法では、使用する処理ガスとして水素を使用することが多く、リークすると爆発の危険が高く、ＳｉＣ被覆炭素管は管理が難しく、実用的でない。   In addition, a carbonaceous reaction tube is housed in a metal sealed container, and the carbonaceous reaction tube is heated by a heater housed in the sealed container (see Patent Document 3), and the surface of the carbonaceous reaction tube. There is also known a reaction vessel (see Patent Document 4) in which gas-impermeable SiC is coated to improve the airtightness of the reaction tube. However, in the reaction vessel of Patent Document 3, (1) the cooling rate is slow: the reaction tube, the heater, and the heat insulating material are housed in the sealed vessel, so the heat capacity is large and it is difficult to cool down. (2) The sample is taken out. Frequent: Since the sample is contained in a double sealed container, there is a problem that the sample cannot be taken out unless two or more flanges are removed. Moreover, in the reaction container of patent document 4, there exists a problem in the reliability of a SiC covering carbon tube. In the embodiment, it is said that the device has endured 50 times. However, for example, if the SiC layer cracks due to rapid cooling, there is a risk that the oxidation of the carbonaceous reaction tube proceeds rapidly. In addition, if a tool or the like is struck against the reaction tube due to careless handling, the SiC layer falls off, and oxidation of the carbonaceous reaction tube proceeds. In the pulse CVI method, hydrogen is often used as a processing gas to be used, and if it leaks, there is a high risk of explosion, and the SiC-coated carbon tube is difficult to manage and is not practical.

特開平８−９１９６３号公報JP-A-8-91963 特開平８−１８８４８９号公報Japanese Patent Laid-Open No. 8-188489 特開平６−３４５５６９号公報Japanese Patent Laid-Open No. 6-345569 特開平６−５７４３３号公報JP-A-6-57433

上記のように、従来の反応容器には耐久性に問題があり、反応容器のメンテナンスや交換のための費用が製造コストを高めている。また、パルスＣＶＩ法においては、処理ガスの導入−保持−排気サイクルが短いほど処理効率は高まるが、反応容器の耐久性のためにおのずと限度がある。   As described above, the conventional reaction vessel has a problem in durability, and the cost for maintenance and replacement of the reaction vessel increases the manufacturing cost. In the pulse CVI method, the processing efficiency increases as the introduction / holding / exhaust cycle of the processing gas is shorter, but there is a limit to the durability of the reaction vessel.

本発明は上記のような状況に鑑みてなされたものであり、気相成長用容器の耐久性及び信頼性を高め、高効率で気相成長法による析出を行なうことを目的とする。   The present invention has been made in view of the above situation, and an object of the present invention is to improve the durability and reliability of a vapor phase growth vessel and to perform precipitation by a vapor phase growth method with high efficiency.

本発明は、上記の課題を解決するために、下記に示す気相成長用反応容器及び気相成長方法を提供する。
（１）被処理体を収容し、処理ガスを導入して前記被処理体に該処理ガスの反応により析出する物質を気相成長させるために使用される気相成長用反応容器において、
耐衝撃性及び耐熱衝撃性を備える外管と、耐熱性及び耐腐食性を備える内管とからなる二重管構造であり、前記外管と前記内管との間の空間が気密に保持されるとともに、前記空間が非酸化性ガス雰囲気に保持されることを特徴とする気相成長用反応容器。
（２）前記外管がＮｉ基、Ｆｅ基またはＣｏ基の耐熱合金からなり、かつ前記内管が炭素質またはセラミック質からなることを特徴とする上記（１）記載の気相成長用反応容器。
（３）前記内管の表面が封止処理されていることを特徴とする上記（２）記載の気相成長用反応容器。
（４）前記外管が、非酸化性ガスの導入口及び排気口を備えることを特徴とする上記（１）〜（３）の何れか１項に記載の気相成長用反応容器。
（５）前記被処理体を載置する試料台が、前記処理ガスを導入するガス導入口と、前記処理ガスを前記反応容器外に排気するガス排気口とを備えることを特徴とする上記（１）〜（４）の何れか１項に記載の気相成長用反応容器。
（６）前記ガス導入口と前記ガス排気口とが共有化されるとともに、略均等に分散配置されていることを特徴とする上記（５）記載の気相成長用反応容器。
（７）前記気相成長が、反応容器内に処理ガスを導入し、所定時間保持した後、排気を行なうサイクルを所定回数繰り返し行なうパルスＣＶＩ法により行なわれることを特徴とする上記（１）〜（６）の何れか１項に記載の気相成長用反応容器。
（８）反応容器内に被処理体を配置し、前記反応容器を加熱しながら処理ガスを導入して前記被処理体に処理ガスの反応により析出する物質を気相成長させる気相成長方法において、
外管と内管とからなる二重構造の反応容器を用い、処理中、前記外管と前記内管との間に形成された空間を非酸化性ガス雰囲気に保持することを特徴とする気相成長方法。
（９）前記処理ガスに四塩化珪素ガス、メタンガス及び水素を用いるとともに、前記非酸化性ガスにアルゴンガスを用いることを特徴とする上記（８）記載の気相成長方法。
（１０）前記反応容器内に処理ガスを導入し、所定時間保持した後、排気を行なうサイクルを所定回数繰り返し行なうことを特徴とする上記（８）または（９）記載の気相成長方法。 In order to solve the above-mentioned problems, the present invention provides the following vapor phase growth reaction vessel and vapor phase growth method.
(1) In a reaction vessel for vapor phase growth used for containing a target object, introducing a processing gas, and vapor-depositing a substance deposited on the target object by reaction of the processing gas,
It is a double tube structure consisting of an outer tube with impact resistance and thermal shock resistance and an inner tube with heat resistance and corrosion resistance, and the space between the outer tube and the inner tube is kept airtight. And the space is maintained in a non-oxidizing gas atmosphere.
(2) The reaction vessel for vapor phase growth as described in (1) above, wherein the outer tube is made of a Ni-based, Fe-based or Co-based heat-resistant alloy, and the inner tube is made of carbonaceous material or ceramic material. .
(3) The reaction vessel for vapor phase growth as described in (2) above, wherein the surface of the inner tube is sealed.
(4) The reaction vessel for vapor phase growth according to any one of (1) to (3), wherein the outer tube includes a non-oxidizing gas introduction port and an exhaust port.
(5) The sample stage on which the object to be processed is mounted includes a gas introduction port for introducing the processing gas, and a gas exhaust port for exhausting the processing gas to the outside of the reaction container. The reaction vessel for vapor phase growth according to any one of 1) to (4).
(6) The vapor phase growth reaction vessel as described in (5) above, wherein the gas introduction port and the gas exhaust port are shared, and are arranged substantially uniformly.
(7) The vapor phase growth is performed by a pulse CVI method in which a processing gas is introduced into a reaction vessel, held for a predetermined time, and then evacuated for a predetermined number of times. The reaction vessel for vapor phase growth according to any one of (6).
(8) In a vapor phase growth method in which an object to be processed is disposed in a reaction vessel, a process gas is introduced while heating the reaction vessel, and a substance that is deposited on the object to be processed by a reaction of the process gas is vapor-phase grown. ,
A double-structured reaction vessel comprising an outer tube and an inner tube is used, and a space formed between the outer tube and the inner tube is maintained in a non-oxidizing gas atmosphere during processing. Phase growth method.
(9) The vapor phase growth method as described in (8) above, wherein silicon tetrachloride gas, methane gas and hydrogen are used as the processing gas, and argon gas is used as the non-oxidizing gas.
(10) The vapor phase growth method as described in (8) or (9) above, wherein the process gas is introduced into the reaction vessel and held for a predetermined time, and then the exhaust cycle is repeated a predetermined number of times.

本発明の気相成長用反応容器は、二重構造で、処理中に非酸化性ガス雰囲気に維持されるため耐久性が高まる。また、この気相成長用反応容器を用いることにより、効率良く気相成長を行なうことができ、製造コストの低減を図ることができる。   The vapor deposition reactor of the present invention has a dual structure and is maintained in a non-oxidizing gas atmosphere during processing, so that durability is enhanced. Further, by using this reaction vessel for vapor phase growth, vapor phase growth can be performed efficiently, and the production cost can be reduced.

以下、本発明に関して図面を参照して詳細に説明する。   Hereinafter, the present invention will be described in detail with reference to the drawings.

図１は、本発明の気相成長用反応容器（以下、「反応容器」という）を示す断面図及びＡ部分の拡大図である。図示されるように、反応容器３０は、内管３１と外管３２との二重構造になっている。内管３１は、処理ガスと接触するために耐食性を有する必要があり、炭素材料で形成することが好適である。内管３１に加工するには、黒鉛の押出し材やＣＩＰ材を所定形状に切削する方法が一般的である。   FIG. 1 is a sectional view showing a reaction vessel for vapor phase growth (hereinafter referred to as “reaction vessel”) of the present invention and an enlarged view of a portion A. As illustrated, the reaction vessel 30 has a double structure of an inner tube 31 and an outer tube 32. The inner pipe 31 needs to have corrosion resistance in order to come into contact with the processing gas, and is preferably formed of a carbon material. In order to process the inner tube 31, a method of cutting an extruded graphite material or CIP material into a predetermined shape is generally used.

尚、押出し材は、ミリオーダーの黒鉛粒子とコールタールピッチ等のバインダーとを混合してなる混捏物を押出プレスにて成形して得られる。また、ＣＩＰ材は、粒径が１０〜１００μｍオーダーの微細な黒鉛粒子とバインダーとの混捏物粉をゴムケースに充填し、気密シールした後、圧力媒体（水や油）が貯留された高圧容器内に入れ、圧力媒体を加圧し、圧力媒体を介してゴムケース内の混捏物粉を成形したものである。ＣＩＰ材は、圧力媒体を通じて全方向から均一に加圧されるため、黒鉛粒子はランダムに配向し、人造等方性黒鉛とも称される。また、ＣＩＰ材は黒鉛粒子が微細であることから、気孔サイズが小さく、ガスが透過し難いという特性があり、反応容器の材料として好ましい。   The extruded material is obtained by molding a kneaded material obtained by mixing millimeter-order graphite particles and a binder such as coal tar pitch with an extrusion press. The CIP material is a high-pressure container in which a pressure mixture (water or oil) is stored after a rubber case is filled with a mixture of fine graphite particles having a particle size of the order of 10 to 100 μm and a binder, hermetically sealed. The mixture is put in, the pressure medium is pressurized, and the mixture powder in the rubber case is formed through the pressure medium. Since the CIP material is uniformly pressed from all directions through the pressure medium, the graphite particles are randomly oriented and are also referred to as artificial isotropic graphite. Further, since the CIP material has fine graphite particles, it has the characteristics that the pore size is small and the gas hardly permeates, and it is preferable as the material for the reaction vessel.

また、内管３１は、炭化珪素（ＳｉＣ）等のセラミックス製とすることもできる。   The inner tube 31 can also be made of ceramics such as silicon carbide (SiC).

また、より気体透過性を下げるために、内管３１の表面に封止処理を施すことが好ましい。この封止処理は、例えば、内管３１にフェノール樹脂を塗布して含浸させ、乾燥した後、真空または非酸化性雰囲気中で１０００℃程度の温度で焼成してフェノール樹脂を炭化させればよい。尚、フェノール樹脂は炭化に際して２分の１以下に収縮して気孔が残存するおそれがあるため、目止処理は複数回にわたり行なうことが好ましい。   In order to further reduce the gas permeability, it is preferable to perform a sealing process on the surface of the inner tube 31. For example, the sealing treatment may be performed by applying and impregnating the inner pipe 31 with a phenolic resin, drying it, and then baking it in a vacuum or a non-oxidizing atmosphere at a temperature of about 1000 ° C. to carbonize the phenolic resin. . In addition, since a phenol resin shrink | contracts to 1/2 or less in carbonization, and there exists a possibility that a pore may remain | survive, it is preferable to perform a sealing process in multiple times.

一方、外管３２は、加熱装置により直接加熱されるため、耐熱合金、例えばインコネル等のＮｉ基合金製とすることが好適である。   On the other hand, since the outer tube 32 is directly heated by a heating device, the outer tube 32 is preferably made of a heat-resistant alloy, for example, a Ni-based alloy such as Inconel.

上記の内管３１と外管３２とは気密構造とされる。気密構造とするには、例えばＡ部分の拡大図に示すような構造とすることができる。即ち、外管３２の下端には、外周面から垂直に突出した後、外周面と平行に垂下するフランジ３２ａが形成されており、内管３１の外周面との間でリング状の空所を形成する。内管３１は、その下端に僅かに突出するフランジ３１ａが形成されており、外管３２のフランジ３２ａとの隙間をゴムパッキン３３でシールする。また、内管３１と外管３２のフランジ３２ａとの空所には、第１の押えリング３６がＯリング３５を介在させて収容され、更に第１の押えリング３６の内部には小径の第２の押えリング３７が収容され、両押えリング３６，３７はリング固定ボルト３８により外管３２のフランジ３２ａに固定される。そして、外管３２のフランジ３２ａを反応容器の下部フランジ３９に、Ｏリング４０を介して固定ボルト４１で固定することにより、Ｏリング３５と第１の押えリング３６とが圧縮され、反応容器３０は気密構造となる。   The inner tube 31 and the outer tube 32 have an airtight structure. In order to obtain an airtight structure, for example, a structure as shown in the enlarged view of the portion A can be used. That is, the lower end of the outer tube 32 is formed with a flange 32a that protrudes perpendicularly from the outer peripheral surface and then hangs parallel to the outer peripheral surface. Form. The inner tube 31 has a flange 31 a that slightly protrudes at the lower end thereof, and a gap between the outer tube 32 and the flange 32 a is sealed with a rubber packing 33. A first presser ring 36 is accommodated in the space between the inner pipe 31 and the flange 32 a of the outer pipe 32 with an O-ring 35 interposed therebetween. Two presser rings 37 are accommodated, and both presser rings 36 and 37 are fixed to the flange 32 a of the outer tube 32 by ring fixing bolts 38. Then, by fixing the flange 32a of the outer tube 32 to the lower flange 39 of the reaction vessel with the fixing bolt 41 via the O-ring 40, the O-ring 35 and the first holding ring 36 are compressed, and the reaction vessel 30 is compressed. Has an airtight structure.

また、下部フランジ３９は、処理ガスの導入及び排気を行なう通気口４２が形成されており、通気口４２を塞ぐように、被処理体４３を載置する炭素製の試料台４５が固定されている。試料台４５には、処理ガスの導入及び排気を行なう通気口４６を備えるが、この通気口４６は、下部フランジ３９の通気口４２に連通する本管４６ａと、本管４６ａと連通して試料台４５の周壁に等間隔で複数設けられた開口に達する枝管４６ｂとで構成される。このような通気口４６により、処理ガスが枝管４６ｂを通じて試料台４５の複数箇所から放出され、処理ガスが早期に内管３１の全体に拡散する。また、排気も枝管４６ｂを通じて複数箇所で行なわれるため、排気効率も高まる。   Further, the lower flange 39 is formed with a vent 42 for introducing and exhausting a processing gas, and a carbon sample stage 45 on which the workpiece 43 is placed is fixed so as to close the vent 42. Yes. The sample stage 45 is provided with a vent 46 for introducing and evacuating process gas. The vent 46 communicates with the main pipe 46a communicating with the vent 42 of the lower flange 39 and the main pipe 46a. The branch pipe 46b reaches a plurality of openings provided at equal intervals on the peripheral wall of the table 45. Through such a vent 46, the processing gas is released from a plurality of locations on the sample stage 45 through the branch pipe 46b, and the processing gas diffuses throughout the inner tube 31 at an early stage. Further, since exhaust is performed at a plurality of locations through the branch pipe 46b, exhaust efficiency is also increased.

試料台４５には、通気口４６の周囲を空洞とし、空洞にセラミックウール等からなる断熱材４７を配置してもよい。気相成長法では、加熱されている反応容器の内部温度を下げないように、処理ガスを加熱してから反応容器に導入することがあるが、試料台４５を断熱構造にすることにより、加熱された処理ガスが試料台４５を通過しても温度低下を起こすことがなくなる。   The sample stage 45 may be provided with a heat insulating material 47 made of ceramic wool or the like in the cavity around the vent 46. In the vapor phase growth method, the processing gas may be heated and then introduced into the reaction vessel so as not to lower the internal temperature of the heated reaction vessel. Even if the processed gas passes through the sample stage 45, the temperature does not decrease.

内管３１と外管３２との間には、析出を行なう期間、具体的には反応容器３０の加熱開始から加熱終了までの期間、非酸化性ガスを流通させる。ガスの供給及び排気は、外管３２の適所に導入口４７及び排気口４８を設ければよい。これにより、内管３１から微量の処理ガスが漏れても、処理ガスが反応容器３０から排除されるため、爆発を起こす危険性がなくなる。非反応性ガスとしては、アルゴンガスの他、窒素ガスを用いることができる。   A non-oxidizing gas is circulated between the inner pipe 31 and the outer pipe 32 during the period of precipitation, specifically, the period from the start of heating of the reaction vessel 30 to the end of heating. For gas supply and exhaust, an introduction port 47 and an exhaust port 48 may be provided at appropriate positions of the outer tube 32. Thereby, even if a very small amount of processing gas leaks from the inner pipe 31, the processing gas is excluded from the reaction vessel 30, so that there is no risk of explosion. As the non-reactive gas, nitrogen gas can be used in addition to argon gas.

本発明の反応容器３０は上記の如く構成されるが、高温で処理ガスと接触する部分が炭素質またはセラミック質の内管３１であるから、処理ガスに対する耐性に優れる。内管３１は炭素質またはセラミック質であるため、高温の大気と接触すると容易に酸化するので、単独では使用できず、簡単に脆性破壊するが、耐熱合金からなる外管３２で覆うことにより内管３１の酸化の問題は解決される。また、内管３１は外管３２によって力学的に保護されており、取り扱いミスにより割れるおそれもない。もし、何らかの原因で反応中に内管３１が破壊して処理ガスが漏洩しても、外管３２により爆発を防ぐことができる。更には、炭素質またはセラミック質の内管３１及び耐熱合金製の外管３２は、石英ガラスやセラミックスに比べて、耐熱衝撃性に優れるため急熱と急冷が可能であり、処理時間を短縮することができるという利点も有する。   Although the reaction vessel 30 of the present invention is configured as described above, the portion that comes into contact with the processing gas at a high temperature is the carbonaceous or ceramic inner pipe 31 and thus has excellent resistance to the processing gas. Since the inner tube 31 is carbonaceous or ceramic, it easily oxidizes when it comes into contact with high-temperature air. Therefore, the inner tube 31 cannot be used alone and is easily brittlely broken. The problem of oxidation of the tube 31 is solved. Further, the inner tube 31 is mechanically protected by the outer tube 32, and there is no possibility of breaking due to a handling mistake. Even if the inner tube 31 is broken during the reaction for some reason and the processing gas leaks, the outer tube 32 can prevent explosion. Furthermore, the inner tube 31 made of carbon or ceramic and the outer tube 32 made of a heat-resistant alloy are excellent in thermal shock resistance compared to quartz glass and ceramics, and thus can be rapidly heated and cooled, thereby shortening the processing time. It also has the advantage of being able to.

本発明の反応容器３０はこのような利点を有し、一般的な気相成長法に使用することができるが、耐久性が要求されるパルスＣＶＩ法への適用において特にその効果を発揮する。以下に、本発明の反応容器３０を用いたパルスＣＶＩ法について、被処理体に炭化珪素を析出させる場合を例示して説明する。   The reaction vessel 30 of the present invention has such advantages and can be used for a general vapor deposition method, but exhibits its effect particularly in application to a pulse CVI method requiring durability. Hereinafter, the pulse CVI method using the reaction vessel 30 of the present invention will be described by exemplifying a case where silicon carbide is deposited on the object to be processed.

図２はパルスＣＶＩ装置の主要部を示す概略図であり、処理ガス発生装置１０から本発明の反応容器３０に供給し、処理ガスを反応容器３０に所定時間保持した後、反応容器３０を排気する構成となっている。   FIG. 2 is a schematic diagram showing the main part of the pulse CVI apparatus. After supplying the processing gas from the processing gas generator 10 to the reaction vessel 30 of the present invention and holding the processing gas in the reaction vessel 30 for a predetermined time, the reaction vessel 30 is evacuated. It is the composition to do.

処理ガス発生装置１０は、例えば液化四塩化珪素（ＳｉＣｌ４）を貯蔵したバブリングタンク１１を備え、ここへ水素ガス（Ｈ２）を供給してバブリングさせ、原料ガスとなる四塩化珪素ガスを発生させる。水素ガスのガスボンベにはレギュレータＲＧ５、流量計ＦＭ５及びエアオペレーバルブ（以下、「バルブ」という）Ｖ５が連結しており、流量や供給時期が制御される。発生した四塩化珪素ガスは、手動流量調整バルブＮＶ１で流量調整され、処理ガス貯留容器２０に送られる。処理ガスの処理ガス貯留容器２０への供給はバルブＶ６で制御される。 The processing gas generator 10 includes, for example, a bubbling tank 11 that stores liquefied silicon tetrachloride (SiCl 4 ). Hydrogen gas (H 2 ) is supplied to the bubbling tank 11 to generate a silicon tetrachloride gas as a raw material gas. Let A regulator RG5, a flow meter FM5, and an air operated valve (hereinafter referred to as “valve”) V5 are connected to the hydrogen gas cylinder, and the flow rate and supply timing are controlled. The generated silicon tetrachloride gas is adjusted in flow rate by the manual flow rate adjustment valve NV1 and sent to the processing gas storage container 20. Supply of the processing gas to the processing gas storage container 20 is controlled by a valve V6.

尚、流量調整バルブＮＶ１は、圧力遮断弁として機能し、その開度を適度に絞ることで、四塩化珪素の発生量が安定する。圧力遮断弁が無い場合、バブリングタンク１１の圧力は処理ガス貯留容器２０の圧力と連動してパルス的に変動することがあり、例えば、バブリングタンク１１の圧力が下がると原料ガスの発生量が所定量より増えるようになる。そこで圧力遮断弁を設け、これを適度に絞ると、バブリングタンク１１の圧力変動が抑えられ、原料ガスの発生量が安定する。   The flow rate adjustment valve NV1 functions as a pressure cutoff valve, and the amount of silicon tetrachloride generated is stabilized by appropriately reducing the opening degree. In the absence of a pressure shut-off valve, the pressure in the bubbling tank 11 may fluctuate in a pulsed manner in conjunction with the pressure in the processing gas storage container 20. For example, when the pressure in the bubbling tank 11 decreases, the amount of raw material gas generated increases. It becomes more than quantitative. Therefore, if a pressure shut-off valve is provided and is appropriately throttled, pressure fluctuations in the bubbling tank 11 are suppressed, and the amount of source gas generated is stabilized.

また、処理ガス貯留容器１０には、その他の原料ガスとなるメタン（ＣＨ４）、水素ガス（Ｈ２）、パージガスとしてアルゴンガス（Ａｒ）が供給される。尚、図中のＶ２〜Ｖ４はバルブ、符号ＲＧ２〜ＲＧ４はレギュレータ、ＦＭ２〜ＦＭ４は流量計である。この処理ガス貯留ガス２０において、各原料ガスの混合を安定して行なう。 The processing gas storage container 10 is supplied with methane (CH 4 ), hydrogen gas (H 2 ) as other source gases, and argon gas (Ar) as a purge gas. In the figure, V2 to V4 are valves, symbols RG2 to RG4 are regulators, and FM2 to FM4 are flow meters. In this process gas storage gas 20, each raw material gas is stably mixed.

処理ガス貯留容器２０は、バルブＶ７を介して反応容器３０に接続しており、試料台４５の通気口４６を通じて処理ガスを反応容器３０に供給する。   The processing gas storage container 20 is connected to the reaction container 30 via a valve V 7, and supplies the processing gas to the reaction container 30 through the vent 46 of the sample stage 45.

反応容器３０は、加熱装置５０により加熱される。加熱装置５０は、例えばクレーン等により吊り上げ、移動できる構成とすることが好ましい。処理後、反応容器３０は冷却されるが、通常は、加熱装置５０に収容したまま加熱装置５０を降温することで反応容器３０の冷却を行なっている。そこで、クレーンで加熱容器５０を吊り上げて反応容器３０を外気に曝すことにより、冷却時間を大幅に短縮することができるようになる。その際、反応容器３０は二重構造であり、外管３２のみが固定されているため、急速冷却しても内管３１と外管３２との熱膨張差による熱応力は発生せず、破壊等を起こすことがない。本発明の反応容器３０はこのような利点を併せ持つ。   The reaction vessel 30 is heated by the heating device 50. The heating device 50 is preferably configured to be lifted and moved by, for example, a crane. After the treatment, the reaction vessel 30 is cooled. Usually, the reaction vessel 30 is cooled by lowering the temperature of the heating device 50 while being accommodated in the heating device 50. Therefore, the cooling time can be greatly shortened by lifting the heating vessel 50 with a crane and exposing the reaction vessel 30 to the outside air. At that time, since the reaction vessel 30 has a double structure and only the outer tube 32 is fixed, thermal stress due to a difference in thermal expansion between the inner tube 31 and the outer tube 32 does not occur even when rapidly cooled, and the destruction is broken. It does not cause etc. The reaction vessel 30 of the present invention has such advantages.

また、反応容器３０には、処理中、内管３１と外管３２との間に非酸化性ガスであるアルゴンガス（Ａｒ）が供給される。   Further, argon gas (Ar), which is a non-oxidizing gas, is supplied to the reaction vessel 30 between the inner tube 31 and the outer tube 32 during processing.

更に、反応容器３０は、バルブＶ８を介して排気ガス貯留容器６０に接続しており、排気ガス貯留容器６０の後段に真空ポンプ７０が接続している。排気ガス貯留容器６０は、反応容器３０からの排気ガスを一時保持するために使用される。また、真空ポンプ７０の排ガスはガス処理装置８０で無害化処理が施される。   Further, the reaction container 30 is connected to the exhaust gas storage container 60 via the valve V8, and the vacuum pump 70 is connected to the rear stage of the exhaust gas storage container 60. The exhaust gas storage container 60 is used to temporarily hold the exhaust gas from the reaction container 30. Further, the exhaust gas from the vacuum pump 70 is detoxified by the gas processing device 80.

気相成長の工程は、従来のパルスＣＶＩ法に従うことができ、先ず、被処理体４３を試料台４５に載置し、反応容器３０、加熱装置５０をセットする。   The vapor phase growth process can follow the conventional pulse CVI method. First, the object 43 is placed on the sample stage 45, and the reaction vessel 30 and the heating device 50 are set.

次いで、バルブＶ８以外を閉じて系内を真空引きし、所定の圧力となった後加熱装置５０を通電して反応容器３０を加熱する。それと同時に、バルブＶ１を開いて反応容器３０の内管３１と外管３２との空間にアルゴンガスを供給し、更にバルブＶ９を開く。   Next, the system other than the valve V8 is closed to evacuate the inside of the system, and after reaching a predetermined pressure, the heating device 50 is energized to heat the reaction vessel 30. At the same time, the valve V1 is opened, argon gas is supplied to the space between the inner tube 31 and the outer tube 32 of the reaction vessel 30, and the valve V9 is further opened.

次いで、バルブＶ８を閉じ、バルブＶ４及びバルブＶ７を開いて水素ガスを処理ガス貯留容器２０及び反応容器３０に流通させた後、バルブＶ７を閉じ、反応容器３０内に水素ガスを所定時間保持する。保持後、バルブＶ８を開いて反応容器３０内を排気する。この処理ガスの導入及び排気を所定回数繰り返し、クリーニングを行なう。   Next, the valve V8 is closed, and the valves V4 and V7 are opened to allow hydrogen gas to flow through the processing gas storage container 20 and the reaction container 30, and then the valve V7 is closed and the hydrogen gas is held in the reaction container 30 for a predetermined time. . After holding, the valve V8 is opened to evacuate the reaction vessel 30. Cleaning is performed by introducing and exhausting the processing gas a predetermined number of times.

次いで、以下の操作を行ない被処理体４３への析出を行なう。先ず、バルブＶ７、バルブＶ８を閉じ、バルブＶ３、バルブＶ４、バルブＶ５及びバルブＶ６を開いて処理ガス貯留容器２０に各原料ガスを供給する。原料ガスの供給が安定した後、バルブＶ７を開いて処理ガスを反応容器３０に供給する。しかる後、バルブＶ７を閉じて処理ガスを反応容器３０内に保持する。保持時間としては０．２〜１０秒が一般的である。所定時間保持した後、バルブＶ８を開いて反応容器３０内を排気する。この処理ガスの導入及び排気を所定回数繰り返し行ない、被処理体４５に炭化珪素を析出させる。そして、バルブＶ３、バルブＶ４、バルブＶ５及びバルブＶ６を閉じ、バルブＶ７を開いて析出処理が完了する。尚、流量調整バルブＮＶ１は、予め開度を調整しておき、処理中は固定する。   Next, the following operation is performed to deposit on the workpiece 43. First, the valve V7 and the valve V8 are closed, and the valve V3, the valve V4, the valve V5, and the valve V6 are opened to supply each source gas to the processing gas storage container 20. After the supply of the source gas is stabilized, the valve V7 is opened to supply the processing gas to the reaction vessel 30. Thereafter, the valve V7 is closed to hold the processing gas in the reaction vessel 30. The holding time is generally 0.2 to 10 seconds. After holding for a predetermined time, the valve V8 is opened and the reaction vessel 30 is evacuated. The introduction and exhaust of the processing gas are repeated a predetermined number of times to deposit silicon carbide on the object to be processed 45. Then, the valve V3, the valve V4, the valve V5, and the valve V6 are closed, and the valve V7 is opened to complete the deposition process. The flow rate adjustment valve NV1 is adjusted in advance and fixed during processing.

析出完了後、水素ガスを流通させた後、系内の真空引きを行ない、その後、加熱装置５０の通電を停止して反応容器３０を冷却する。冷却に際して、加熱装置５０を吊り上げて反応容器３０と離間させても良い。冷却後、バルブＶ１を閉じて反応容器３０の二重管の隙間へのアルゴンガスの供給を停止する。   After the completion of the deposition, hydrogen gas is circulated, the inside of the system is evacuated, and then the energization of the heating device 50 is stopped to cool the reaction vessel 30. During cooling, the heating device 50 may be lifted and separated from the reaction vessel 30. After cooling, the valve V1 is closed and the supply of argon gas to the gap between the double tubes of the reaction vessel 30 is stopped.

以下、実施例を挙げて本発明を更に説明する。   Hereinafter, the present invention will be further described with reference to examples.

メカニカルカーボン製の人造等方性黒鉛材（密度１．７ｇ／ｃｍ３）を用いて、外径１７０ｍｍ、内径１５０ｍｍ、長さ４１０ｍｍの内管を作製した。この内管には、更に、気体透過性を抑えるために、下記の目止処理を施した。 Using an artificial isotropic graphite material (density 1.7 g / cm 3 ) made of mechanical carbon, an inner tube having an outer diameter of 170 mm, an inner diameter of 150 mm, and a length of 410 mm was produced. The inner tube was further subjected to the following sealing treatment in order to suppress gas permeability.

先ず、大日本インキ化学工業製のフェノール樹脂（フェノライトＪ−３２５）とエタノールとを１：１で混合して溶液を調製し、内管のシール部を除く外面全面に塗布して含浸させ、９０℃で１０時間乾燥してから、電気炉に入れ、真空中、１５℃／ｍｉｎ（但し１５０〜５００℃までは５℃／ｍｉｎ）の昇温速度で１１００℃まで昇温し、３０分保持して焼成した。次いで、スラリーを内管の両面に塗布し、同様の処理を２回行なった。   First, a phenol resin (Phenolite J-325) manufactured by Dainippon Ink and Chemicals, and ethanol were mixed at a ratio of 1: 1 to prepare a solution, which was applied and impregnated on the entire outer surface excluding the seal portion of the inner tube, After drying at 90 ° C. for 10 hours, put it in an electric furnace, raise the temperature to 1100 ° C. at a rate of 15 ° C./min (5 ° C./min up to 150 to 500 ° C.) in vacuum, and hold for 30 minutes And fired. Next, the slurry was applied to both surfaces of the inner tube, and the same treatment was performed twice.

また、外径１９０ｍｍ、内径１８０ｍｍ、長さ５６０ｍｍのインコネル６０１製の外管３２を作製した。そして、内管と外管とで二重構造の反応容器とした。尚、気密構造にするために、図１に示すような連結構造とした。この反応容器の内容積は約９Ｌである。   In addition, an outer tube 32 made of Inconel 601 having an outer diameter of 190 mm, an inner diameter of 180 mm, and a length of 560 mm was produced. And it was set as the reaction container of the double structure with the inner tube | pipe and the outer tube | pipe. In addition, in order to make an airtight structure, it was set as the connection structure as shown in FIG. The internal volume of this reaction vessel is about 9L.

そして、図２に示すように、作製した反応容器と、容量約３２Ｌの処理ガス貯留容器とを用い、図２に示すような配管にてパルスＣＶＩ装置を構築した。   Then, as shown in FIG. 2, a pulse CVI apparatus was constructed with piping as shown in FIG. 2 using the produced reaction container and a processing gas storage container having a capacity of about 32 L.

被処理体として、寸法８０×８０×４０ｍｍで、気孔径約１ｍｍの炭素質スポンジ（ウレタン発泡体にフェノライトＪ−３２５を含浸・液切り・乾燥してから、１０００℃の非酸化雰囲気で炭化させたもの）を、反応容器の試料台に設置した。そして、原料ガスに、ＳｉＣｌ４、ＣＨ４、Ｈ２、パージガスにＡｒを用い、炭化珪素の析出を行なった。 Carbonaceous sponge with dimensions of 80 x 80 x 40 mm and pore size of about 1 mm as the object to be processed (urethane foam was impregnated with fenolite J-325, drained and dried, then carbonized in a non-oxidizing atmosphere at 1000 ° C. Was placed on the sample stage of the reaction vessel. Then, SiCl 4 , CH 4 , H 2 was used as a raw material gas, and Ar was used as a purge gas to deposit silicon carbide.

先ず、反応容器を真空引きし、内管と外管をパージするためにＡｒガスを１Ｌ／ｍｉｎ（０℃標準状態換算）流しながら、１１００℃に昇温した。   First, the reaction vessel was evacuated and heated to 1100 ° C. while flowing Ar gas at 1 L / min (converted to 0 ° C. standard state) in order to purge the inner tube and the outer tube.

次いで、処理ガス貯留容器及び反応容器を真空引きした状態で、モル流量で、Ｈ２：１．３４ｍｏｌ／ｍｉｎ、ＣＨ４：０．６ｍｏｌ／ｍｉｎ、ＳｉＣｌ４；０．６ｍｏｌ／ｍｉｎとなるように各原料ガス供給量及びＳｉＣｌ４の発生量を調整した。尚、流量調整バルブＮＶ１（ｓｗａｇｅｌｏｋ ＳＳ−８ＲＳ４）の開度は、全閉から２回転ほど開いた位置とした。この開度は予備実験で、バブリングタンクの圧力が変動しないように調整した結果である。 Next, in a state where the processing gas storage container and the reaction container are evacuated, the molar flow rates are such that H 2 : 1.34 mol / min, CH 4 : 0.6 mol / min, SiCl 4 ; 0.6 mol / min. Each raw material gas supply amount and the generation amount of SiCl 4 were adjusted. In addition, the opening degree of the flow rate adjustment valve NV1 (swagelok SS-8RS4) was set to a position opened about two rotations from the fully closed state. This opening degree is a result of adjustment in a preliminary experiment so that the pressure of the bubbling tank does not fluctuate.

析出に際し、先ず、処理ガス導入用のバルブ（図２のバルブＶ７）を閉じてから、排気用のバルブ（図２のバルブＶ８）を２．１秒開いて、反応容器の排気を行った（ＳＴＥＰ１）。次に、バルブＶ８を閉じてから、バルブＶ７を０．３秒開いて、処理ガス貯留容器に滞留した処理ガスを反応容器に導入した（ＳＴＥＰ２）。次に、バルブＶ７を閉じて、反応容器を封じた状態に０．６秒間保持した（ＳＴＥＰ３）。次に、ＳＴＥＰ１に戻った。このＳＴＥＰ１からＳＴＥＰ３に至る工程を１パルスとし、３０００パルスの運転を行った。約１００パルスで系の圧力バランスがとれ、反応容器のパルス圧は、最高圧７５ｋＰａ ａｂｓ、最低圧１０ｋＰａ ａｂｓとなった。   During deposition, first, the processing gas introduction valve (valve V7 in FIG. 2) was closed, and then the exhaust valve (valve V8 in FIG. 2) was opened for 2.1 seconds to evacuate the reaction vessel ( STEP 1). Next, after the valve V8 was closed, the valve V7 was opened for 0.3 seconds, and the processing gas retained in the processing gas storage container was introduced into the reaction container (STEP 2). Next, the valve V7 was closed, and the reaction vessel was kept sealed for 0.6 seconds (STEP 3). Next, it returned to STEP1. The process from STEP 1 to STEP 3 was set to 1 pulse, and operation of 3000 pulses was performed. The system pressure balance was achieved at about 100 pulses, and the pulse pressure in the reaction vessel became a maximum pressure of 75 kPa abs and a minimum pressure of 10 kPa abs.

所定のパルス運転が終了してから、加熱容器に収容したまま反応容器を真空引きしつつ冷却を行なった。１時間後に、反応容器の温度が５００℃まで低下した時点で、加熱装置をクレーンで吊り上げて離間させ、反応容器の冷却を引き続き行なった。約１時間で反応容器の温度は約８０℃まで低下した。尚、比較のために、加熱装置の離間を行わずに冷却した場合、約８０℃まで冷却するのに、約６時間を要した。即ち、２重構造の反応容器を用い、加熱装置の離間を行なうことで、冷却時間は４時間短縮した。   After completion of the predetermined pulse operation, the reaction vessel was cooled while being evacuated while being accommodated in the heating vessel. One hour later, when the temperature of the reaction vessel decreased to 500 ° C., the heating device was lifted and separated by a crane, and the reaction vessel was continuously cooled. In about 1 hour, the temperature of the reaction vessel dropped to about 80 ° C. For comparison, when cooling was performed without separating the heating device, it took about 6 hours to cool to about 80 ° C. That is, the cooling time was shortened by 4 hours by using a reaction vessel having a double structure and separating the heating devices.

被処理体を取り出し、Ｘ線回折法で析出物を調べたところ、β−ＳｉＣであった。ＳｉＣの析出により、処理前のかさ密度０．０１４ｇ／ｃｍ３が０．０２８ｇ／ｃｍ３まで上昇した。 When the to-be-processed object was taken out and the precipitate was investigated by the X ray diffraction method, it was (beta) -SiC. The deposition of SiC, bulk density 0.014 g / cm 3 before treatment was increased to 0.028 g / cm 3.

また、同条件で２０バッチの運転を行ったが、外管の腐蝕、内管の破壊等のトラブルは一切発生しなかった。   Further, 20 batches were operated under the same conditions, but no troubles such as corrosion of the outer tube and destruction of the inner tube occurred.

本発明の気相成長用反応容器の構成を示す図である。It is a figure which shows the structure of the reaction container for vapor phase growth of this invention. 本発明の気相成長用反応容器を用いて気相成長法を実施するための装置の一例（パルスＣＶＩ装置）の構成を示す図である。It is a figure which shows the structure of an example (pulse CVI apparatus) for implementing a vapor phase growth method using the reaction vessel for vapor phase growth of this invention.

符号の説明Explanation of symbols

３０ 反応容器
３１ 内管
３２ 外管
４３ 被処理体
４５ 試料台
４６ 通気口
４７ 断熱材 30 Reaction vessel 31 Inner tube 32 Outer tube 43 Object 45 Sample base 46 Vent 47 Heat insulation

Claims (10)

被処理体を収容し、処理ガスを導入して前記被処理体に該処理ガスの反応により析出する物質を気相成長させるために使用される気相成長用反応容器において、
耐衝撃性及び耐熱衝撃性を備える外管と、耐熱性及び耐腐食性を備える内管とからなる二重管構造であり、前記外管と前記内管との間の空間が気密に保持されるとともに、前記空間が非酸化性ガス雰囲気に保持されることを特徴とする気相成長用反応容器。 In a reaction vessel for vapor phase growth used for containing a target object, introducing a processing gas, and vapor-depositing a substance deposited on the target object by reaction of the processing gas,
It is a double tube structure consisting of an outer tube with impact resistance and thermal shock resistance and an inner tube with heat resistance and corrosion resistance, and the space between the outer tube and the inner tube is kept airtight. And the space is maintained in a non-oxidizing gas atmosphere. 前記外管がＮｉ基、Ｆｅ基またはＣｏ基の耐熱合金からなり、かつ前記内管が炭素質またはセラミック質からなることを特徴とする請求項１記載の気相成長用反応容器。   2. The reaction vessel for vapor phase growth according to claim 1, wherein the outer tube is made of a Ni-based, Fe-based or Co-based heat-resistant alloy, and the inner tube is made of carbon or ceramic. 前記内管の表面が封止処理されていることを特徴とする請求項２記載の気相成長用反応容器。   The reaction vessel for vapor phase growth according to claim 2, wherein a surface of the inner tube is sealed. 前記外管が、非酸化性ガスの導入口及び排気口を備えることを特徴とする請求項１〜３の何れか１項に記載の気相成長用反応容器。   The reaction vessel for vapor phase growth according to any one of claims 1 to 3, wherein the outer tube includes a non-oxidizing gas introduction port and an exhaust port. 前記被処理体を載置する試料台が、前記処理ガスを導入するガス導入口と、前記処理ガスを前記反応容器外に排気するガス排気口とを備えることを特徴とする請求項１〜４の何れか１項に記載の気相成長用反応容器。   The sample stage on which the object to be processed is mounted includes a gas introduction port for introducing the processing gas and a gas exhaust port for exhausting the processing gas to the outside of the reaction container. The reaction vessel for vapor phase growth according to any one of the above. 前記ガス導入口と前記ガス排気口とが共有化されるとともに、略均等に分散配置されていることを特徴とする請求項５記載の気相成長用反応容器。   6. The reaction vessel for vapor phase growth according to claim 5, wherein the gas introduction port and the gas exhaust port are shared and are distributed substantially uniformly. 前記気相成長が、反応容器内に処理ガスを導入し、所定時間保持した後、排気を行なうサイクルを所定回数繰り返し行なうパルスＣＶＩ法により行なわれることを特徴とする請求項１〜６の何れか１項に記載の気相成長用反応容器。   7. The vapor phase growth is performed by a pulse CVI method in which a processing gas is introduced into a reaction vessel, held for a predetermined time, and then evacuation is repeated a predetermined number of times. The reaction vessel for vapor phase growth according to item 1. 反応容器内に被処理体を配置し、前記反応容器を加熱しながら処理ガスを導入して前記被処理体に処理ガスの反応により析出する物質を気相成長させる気相成長方法において、
外管と内管とからなる二重構造の反応容器を用い、処理中、前記外管と前記内管との間に形成された空間を非酸化性ガス雰囲気に保持することを特徴とする気相成長方法。 In a vapor phase growth method in which an object to be processed is disposed in a reaction vessel, a process gas is introduced while heating the reaction vessel, and a substance deposited by reaction of the process gas is vapor-phase grown on the object to be processed.
A double-structured reaction vessel comprising an outer tube and an inner tube is used, and a space formed between the outer tube and the inner tube is maintained in a non-oxidizing gas atmosphere during processing. Phase growth method. 前記処理ガスに四塩化珪素ガス、メタンガス及び水素を用いるとともに、前記非酸化性ガスにアルゴンガスを用いることを特徴とする請求項８記載の気相成長方法。   9. The vapor phase growth method according to claim 8, wherein silicon tetrachloride gas, methane gas and hydrogen are used as the processing gas, and argon gas is used as the non-oxidizing gas. 前記反応容器内に処理ガスを導入し、所定時間保持した後、排気を行なうサイクルを所定回数繰り返し行なうことを特徴とする請求項８または９記載の気相成長方法。   10. The vapor phase growth method according to claim 8 or 9, wherein a cycle of introducing a processing gas into the reaction vessel and holding it for a predetermined time and then exhausting it is repeated a predetermined number of times.
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