JP5906318B2 - 耐熱複合材料の製造方法及び製造装置 - Google Patents
耐熱複合材料の製造方法及び製造装置 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims description 47
- 238000004519 manufacturing process Methods 0.000 title claims description 45
- 239000007789 gas Substances 0.000 claims description 186
- 239000000654 additive Substances 0.000 claims description 90
- 230000000996 additive effect Effects 0.000 claims description 90
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 60
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 59
- 239000012159 carrier gas Substances 0.000 claims description 46
- 238000006243 chemical reaction Methods 0.000 claims description 42
- 239000000460 chlorine Substances 0.000 claims description 34
- 230000015572 biosynthetic process Effects 0.000 claims description 30
- 238000009826 distribution Methods 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 26
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 25
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 23
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 23
- 239000005055 methyl trichlorosilane Substances 0.000 claims description 23
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 21
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 18
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 18
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- 238000011144 upstream manufacturing Methods 0.000 claims description 17
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 16
- 229910052801 chlorine Inorganic materials 0.000 claims description 16
- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical compound ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 claims description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 12
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 12
- 239000005977 Ethylene Substances 0.000 claims description 12
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 12
- 238000005229 chemical vapour deposition Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 10
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 10
- 238000000151 deposition Methods 0.000 claims description 10
- 239000005049 silicon tetrachloride Substances 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 7
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 claims description 6
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 6
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 6
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 229910000077 silane Inorganic materials 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical group ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000005470 impregnation Methods 0.000 claims description 5
- 239000001294 propane Substances 0.000 claims description 5
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims description 5
- 239000005052 trichlorosilane Substances 0.000 claims description 5
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 5
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 3
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims 4
- 239000003779 heat-resistant material Substances 0.000 claims 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 2
- FBBDOOHMGLLEGJ-UHFFFAOYSA-N methane;hydrochloride Chemical compound C.Cl FBBDOOHMGLLEGJ-UHFFFAOYSA-N 0.000 claims 1
- 239000010408 film Substances 0.000 description 58
- 239000010453 quartz Substances 0.000 description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 22
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 14
- 230000007246 mechanism Effects 0.000 description 11
- 239000002994 raw material Substances 0.000 description 11
- 229940050176 methyl chloride Drugs 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 150000002431 hydrogen Chemical class 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910003902 SiCl 4 Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- BUMGIEFFCMBQDG-UHFFFAOYSA-N dichlorosilicon Chemical compound Cl[Si]Cl BUMGIEFFCMBQDG-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/32—Carbides
- C23C16/325—Silicon carbide
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/04—Coating on selected surface areas, e.g. using masks
- C23C16/045—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
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Description
図1は、耐熱複合材料の製造装置の概略的な構成を示す図である。この製造装置は、化学気相堆積(CVD)装置又は化学気相浸透(CVI)装置を構成し、反応炉として横型のホットウォール型炉11を備えている。ホットウォール型炉11は、所定の温度・圧力に維持され、原料ガスのメチルトリクロロシラン(CH3SiCl3:MTS)、キャリアガスの水素(H2)、添加ガスの塩化水素(HCl)を含む混合ガスが供給されている。
制御部は、このような制御を行うことにより、プリフォーム100の微細構造に堆積される製膜の成長速度と埋込の均一性を両立させるようにしている。換言すると、所定の成長速度によりプリフォーム100に炭化ケイ素を含浸した耐熱複合物質の量産性を確保するとともに、所定の埋込の均一性によりプリフォーム100の微細構造への炭化ケイ素の充填性を保証している。
炭化ケイ素の製膜種が1次反応機構にしたがう場合には、炭化ケイ素の製膜の成長速度は製膜種の濃度と1次の関係にある。このような場合、制御部は、付着確率の小さな製膜種を大量に発生させるように制御する。このような付着確率の小さな製膜種は、プリフォームの微細構造に均一に付着して製膜の埋込の均一性を確保するとともに、製膜種が大量に発生されるために製膜の成長速度も確保することができ、成長速度と埋込の均一性を両立させることができる。
炭化ケイ素の製膜種がラングミュア・ヒンシェルウッド型速度式に基づく反応機構の場合には、製膜種が高濃度になるにつれて濃度に対する製膜の成長速度が飽和し、成長速度が製膜種の濃度に依存しない0次反応領域が存在する。制御部は、製膜種の濃度が0次反応領域に相当するように、製膜種が所定値以上の高濃度になるように制御する。このような製膜種の0次反応領域では、濃度に関らず製膜の成長速度が一定であるので、製膜の埋め込みの均一性を確保するとともに、濃度を高めることにより成長速度を増加させることができ、成長速度と埋込の均一性を両立させることができる。
製膜種がいずれの反応機構にしたがう場合にも、塩素を含む添加ガスはエッチング作用を有するので、添加ガスが石英管12に供給される上流側においてプリフォーム100の微細構造に製膜される炭化ケイ素をエッチングする効果が大きくなる。このようなエッチングの効果により、製膜による微細構造の閉塞が起こりにくくなり、製膜の埋込の均一性を確保することができる。
一方、耐熱複合材料を工業的規模で製造する場合、例えば数メートル程度まで及ぶ長寸のホットウォール型炉11を設け、石英管12の上流側から下流側の方向に複数のプリフォーム100を並べて格納し、これらのプリフォーム100に炭化ケイ素を同時に製膜することがある。
12 石英管
21 原料ガス供給源
22 キャリアガス供給源
23 添加ガス供給源
24、25、26 流量制御装置
31 自動弁
32 ロータリーポンプ
100 プリフォーム
Claims (35)
- 化学気相堆積法又は化学気相含浸法を用い、反応炉に微細構造を有する基材を格納して原料ガス及びキャリアガスを流し、前記基材に炭化ケイ素を堆積させて製膜するものであって、
前記原料ガス及びキャリアガスに添加ガスを加え、当該添加ガスの添加量によって前記炭化ケイ素の製膜の成長速度及び埋込の均一性を制御し、
前記添加ガスは、エタン、エチレン、アセチレン及びメタン、分解や反応によりエタン、エチレン及びアセチレンの少なくとも1つを生成できるガス、並びに塩素を含む分子を含むガスの少なくとも1つを含むこと
を特徴とする耐熱複合材料の製造方法。 - 前記炭化ケイ素の製膜は1次反応に従い、前記添加ガスの添加量によって前記基材に対する製膜種の付着確率を制御することによって、前記炭化ケイ素の製膜の成長速度及び埋込の均一性を制御することを特徴とする請求項1記載の耐熱複合材料の製造方法。
- 前記炭化ケイ素の製膜はラングミュア・ヒンシェルウッド型速度式に従い、前記添加ガスの添加量によってラングミュア・ヒンシェルウッド型速度式の0次反応領域を利用するように制御することによって、前記炭化ケイ素の製膜の成長速度及び埋込の均一性を制御することを特徴とする請求項1記載の耐熱複合材料の製造方法。
- 前記炭化ケイ素の製膜の成長速度及び埋込の均一性について最適化することを特徴とする請求項2又は3記載の耐熱複合材料の製造方法。
- 前記添加ガスの添加量によって、前記反応炉内の位置について、前記炭化ケイ素の製膜の成長速度の分布を制御することを特徴とする請求項1〜4のいずれか一項に記載の耐熱複合材料の製造方法。
- 前記成長速度の分布が均一になるように最適化することを特徴とする請求項5記載の耐熱複合材料の製造方法。
- 前記原料ガスは、前記反応炉の上流側から下流側に至る複数の位置から供給することを特徴とする請求項5又は6記載の耐熱複合材料の製造方法。
- 前記原料ガスは、メチルトリクロロシラン、ジメチルジクロロシラン、トリメチルクロロシラン、四塩化ケイ素、シラン及びプロパンの少なくとも1つを含むことを特徴とする請求項1〜7のいずれか一項に記載の耐熱複合材料の製造方法。
- 前記キャリアガスは、水素、窒素、ヘリウム及びアルゴンの少なくとも1つを含むことを特徴とする請求項1〜8のいずれか一項に記載の耐熱性材料の製造方法。
- 前記添加ガスは、エタン、エチレン、アセチレン及びメタンの少なくとも1つを含むことを特徴とする請求項1〜9のいずれか一項に記載の耐熱性材料の製造方法。
- 前記添加ガスは、分解や反応によりエタン、エチレン及びアセチレンの少なくとも1つを生成できるガスを含むことを特徴とする請求項1〜9にいずれか一項に記載の耐熱複合材料の製造方法。
- 前記添加ガスは、塩素を含む分子を含むことを特徴とする請求項1〜11のいずれか一項に記載の耐熱複合材料の製造方法。
- 前記添加ガスは、塩化水素、塩素、塩化メタン、ジクロロメタン、クロロホルム、四塩化炭素、塩化ビニル、塩化ベンゼン、四塩化珪素、トリクロロシラン、ジクロロシラン、ジクロロエチレン、テトラクロロエタン、トリクロロエタン及びジクロロエタンの少なくとも1つを含むことを特徴とする請求項12に記載の耐熱複合材料の製造方法。
- 前記原料ガスがメチルトリクロロシランであり、アセチレンのメチルトリクロロシランの流量に対する比流量が4.9×10−1を超えないことを特徴とする請求項10に記載の耐熱複合材料の製造方法。
- 前記添加ガスは、エッチング作用を有することを特徴とする請求項1〜14のいずれか一項に記載の耐熱複合材料の製造方法。
- 前記基材は、繊維のプリフォーム、トレンチを設けた基板及び多孔質の基板の少なくとも1つを含むことを特徴とする請求項1〜15のいずれか一項に記載の耐熱複合材料の製造方法。
- 前記反応炉は、ホットウォール型炉であることを特徴とする請求項1〜16のいずれか一項に記載の耐熱複合材料の製造方法。
- 化学気相堆積法又は化学気相含浸法を用い、微細構造を有する基材に炭化ケイ素を堆積させて製膜するものであって、
基材を格納した反応炉と、
前記反応炉に原料ガスを供給する原料ガス供給源と、
前記反応炉にキャリアガスを供給するキャリアガス供給源と、
前記反応炉に添加ガスを供給する添加ガス供給源と、
前記添加ガスの供給量を制御する制御手段と、を有し、
前記制御手段は、当該添加ガスの添加量によって前記炭化ケイ素の製膜の成長速度及び埋込の均一性を制御し、
前記添加ガスは、エタン、エチレン、アセチレン及びメタン、分解や反応によりエタン、エチレン及びアセチレンの少なくとも1つを生成できるガス、並びに塩素を含む分子を含むガスの少なくとも1つを含むこと
を特徴とする耐熱複合材料の製造装置。 - 前記炭化ケイ素の製膜は1次反応に従い、前記制御手段は、前記添加ガスの添加量によって前記基材に対する製膜種の付着確率を制御することによって、前記炭化ケイ素の製膜の成長速度及び埋込の均一性を制御することを特徴とする請求項18記載の耐熱複合材料の製造装置。
- 前記炭化ケイ素の製膜はラングミュア・ヒンシェルウッド型速度式に従い、前記制御手段は、前記添加ガスの添加量によってラングミュア・ヒンシェルウッド型速度式の0次反応領域を利用するように制御することによって、前記炭化ケイ素の製膜の成長速度及び埋込の均一性を制御することを特徴とする請求項18記載の耐熱複合材料の製造装置。
- 前記制御手段は、前記炭化ケイ素の製膜の成長速度及び埋込の均一性について最適化することを特徴とする請求項19又は20記載の耐熱複合材料の製造装置。
- 前記制御手段は、前記添加ガスの添加量によって、前記反応炉内の位置について、前記炭化ケイ素の製膜の成長速度の分布を制御することを特徴とする請求項18〜21のいずれか一項に記載の耐熱複合材料の製造装置。
- 前記成長速度の分布が均一になるように最適化することを特徴とする請求項22記載の耐熱複合材料の製造装置。
- 前記原料ガスを前記反応炉の上流側から下流側に至る複数の位置から供給する供給路を有することを特徴とする請求項22又は23記載の耐熱複合材料の製造装置。
- 前記原料ガスは、メチルトリクロロシラン、ジメチルジクロロシラン、トリメチルクロロシラン、四塩化ケイ素、シラン及びプロパンの少なくとも1つを含むことを特徴とする請求項18〜24のいずれか一項に記載の耐熱複合材料の製造装置。
- 前記キャリアガスは、水素、窒素、ヘリウム及びアルゴンの少なくとも1つを含むことを特徴とする請求項18〜25のいずれか一項に記載の耐熱性材料の製造装置。
- 前記添加ガスは、エタン、エチレン、アセチレン及びメタンの少なくとも1つを含むことを特徴とする請求項18〜26のいずれか一項に記載の耐熱性材料の製造装置。
- 前記添加ガスは、分解や反応によりエタン、エチレン及びアセチレンの少なくとも1つを生成できるガスを含むことを特徴とする請求項18〜26のいずれか一項に記載の耐熱複合材料の製造装置。
- 前記添加ガスは、塩素を含む分子を含むことを特徴とする請求項18〜28のいずれか一項に記載の耐熱複合材料の製造装置。
- 前記添加ガスは、塩化水素、塩素、塩化メチル、ジクロロメタン、クロロホルム、四塩化炭素、塩化ビニル、塩化ベンゼン、四塩化珪素、トリクロロシラン、ジクロロシラン、ジクロロエチレン、テトラクロロエタン、トリクロロエタン及びジクロロエタンの少なくとも1つを含むことを特徴とする請求項29に記載の耐熱複合材料の製造装置。
- 前記原料ガスがメチルトリクロロシランであり、アセチレンのメチルトリクロロシランの流量に対する比流量が4.9×10−1を超えないことを特徴とする請求項27に記載の耐熱複合材料の製造装置。
- 前記添加ガスは、エッチング作用を有することを特徴とする請求項18〜31のいずれか一項に記載の耐熱複合材料の製造装置。
- 前記基材は、セラミックのプリフォーム、トレンチを設けた基板及び多孔質の基板の少なくとも1つを含むことを特徴とする請求項18〜32のいずれか一項に記載の耐熱複合材料の製造装置。
- 前記原料ガス供給源から供給する前記原料ガスの供給量を制御する原料ガス供給量制御手段と、
前記キャリアガス供給源から供給する前記キャリアガスの供給量を制御するキャリアガス供給量制御手段と、
前記添加ガス供給源から供給する前記添加ガスの供給量を制御する添加ガス供給量制御手段と、を有することを特徴とする請求項18〜33のいずれか一項に記載の耐熱複合材料の製造装置。 - 前記反応炉は、ホットウォール型炉であることを特徴とする請求項18〜34のいずれか一項に記載の耐熱複合材料の製造装置。
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WO2014027472A1 (ja) | 2014-02-20 |
US20150152547A1 (en) | 2015-06-04 |
JPWO2014027472A1 (ja) | 2016-07-25 |
CN104619881A (zh) | 2015-05-13 |
EP2896718A1 (en) | 2015-07-22 |
US9822445B2 (en) | 2017-11-21 |
EP2896718A4 (en) | 2016-04-06 |
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