JPS5928564A - 清浄な化学蒸着膜の製造法 - Google Patents

清浄な化学蒸着膜の製造法

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Publication number
JPS5928564A
JPS5928564A JP13577382A JP13577382A JPS5928564A JP S5928564 A JPS5928564 A JP S5928564A JP 13577382 A JP13577382 A JP 13577382A JP 13577382 A JP13577382 A JP 13577382A JP S5928564 A JPS5928564 A JP S5928564A
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JP
Japan
Prior art keywords
vapor deposition
chemical vapor
halide
reaction gas
deposition film
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP13577382A
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English (en)
Inventor
Minoru Nakano
稔 中野
Naoharu Fujimori
直治 藤森
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Sumitomo Electric Industries Ltd
Original Assignee
Sumitomo Electric Industries Ltd
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Application filed by Sumitomo Electric Industries Ltd filed Critical Sumitomo Electric Industries Ltd
Priority to JP13577382A priority Critical patent/JPS5928564A/ja
Publication of JPS5928564A publication Critical patent/JPS5928564A/ja
Pending legal-status Critical Current

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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
    • C23C16/34—Nitrides
    • C23C16/345—Silicon nitride
    • 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
    • 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
    • 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
    • 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
    • C23C16/34—Nitrides
    • 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
    • C23C16/34—Nitrides
    • C23C16/342—Boron nitride
    • 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
    • C23C16/36—Carbonitrides
    • 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
    • C23C16/40—Oxides
    • C23C16/403—Oxides of aluminium, magnesium or beryllium
    • 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
    • C23C16/40—Oxides
    • C23C16/405—Oxides of refractory metals or yttrium

Landscapes

  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。

Description

【発明の詳細な説明】 （イ）技術分野 本発明は化学蒸着法でセラミックス蒸着膜を製造する際
の改良に関する。
（ロ）背景技術 ＴｉＣＸ　５ｉＣＸ　ＴｉＮ５　Ｂ４Ｃ％　　Ｓｉ３Ｎ
４　、　ＡｔＮ。
ＢＮ、　　Ａｔ２０３などのセラミックスは、耐摩耗性
、耐食性、耐酸化性にすぐれており、超硬合金、ハイス
などには数μ被覆して耐摩耗性に優れた工具材料として
用いられている。また最近では、これらの耐食性、耐エ
ロージヨン性に優れるなどの性質を生かして、これらの
特性を要求される構造用材料、真空用部品の内壁などに
使用されている。これらの薄膜製造法としては、一般に
ハロゲン化物などの反応原料ガスを加熱した基板上に送
ってＨ２、Ｎ２、ＣＨ４と反応させる、いわゆる化学蒸
着法がよく用いられる。この化学蒸着法で生成する蒸着
膜には、ハロゲン化物を原料とする場合、膜中に微量の
ハロゲンが残留される。従来、このような残留ハロゲン
は工具材料などでは全く問題にされていなかった。しか
し真空機器、特に機器内がプラズマ等の侵食性の高い雰
囲気にさらされる場合、薄膜の一部が気化、蒸発する際
、残留ハロゲンも同時に気化し、真空機器の排気装置を
腐食し問題になってきている。このハロゲン、特に塩素
量は薄膜中に１０−２％を越えると腐食が著しく進行す
ることが判明した。
０→発明の開示 本発明者等はこの残留ハロゲンを除去する方法について
種々検討した結果、次の知見を得、本発明に至シ達した
ものである。
すなわちＴｉ、５ｉＸｋｌ、　Ｂのハロゲン化物とＮ２
　の比率を０．００５〜０．１にて、炭化水素、Ｃ０２
、Ｎ２、Ｎ２、ＩＪＨ３等の反応ガスを９９．０〜９？
、９９％の純度のものを用いて、化学蒸着を行うと蒸着
膜中のハロゲン含有量が１×１０−５〜ＩＸＩＱ−２％
となることを見出したものである。
Ｔ１、Ｓｉ、Ａｊ、　Ｂ　　のハロゲン化物とＮ２　　
の比率を０，１よｐ大とすると蒸着膜のハロゲン含有量
が１０−２％を越え、比率を０．００５以下にすると薄
膜成長速度が著しく低下するため好捷しくない。また炭
化水素、ＣＯ２、Ｎ２、Ｎ２、ＮＨ３等のガス純度が９
９．０％より小だと１０−２％　以−上の・・ロゲンが
薄膜中に残留するので、９９．０係以上が好寸し７く、
一方９９．９９チ以上の純度のガスは価格が非常に高く
て工業的ではないし、ハロゲン含有量が１×１０−５係
以下であれば排気系への残留ハロゲンの影響はほとＮ７
ど無視できることが判った。
本発明は以上の知見に基いて為されたもので、ＴｉＸ５
ｉＸｋｌ、　Ｂのハロゲン化物をＮ２およびＮ２、炭化
水素、ＣＯ２、ＮＨ３等の反応ガス雰囲気中で反応させ
化学蒸着法により、Ｔ１、Ｓｉ、　ＢＸＡｔの炭化物、
蟹化物、炭窒化物、酸化物およびそれらの複合体の１種
以上から措成される薄膜を形成する際、Ｔ１、ｓ］、Ａ
ｔ、、　Ｂのハロゲン化物とＮ２　　比率を０．００５
〜０．１とし、かつＮ２　　および反応ガス純度が９９
．０％〜９９．９９％のものを用いることを特徴とする
、薄膜中のハロゲン含有量を低下させた清浄な化学蒸着
膜の製造法に関するものである。
なお薄膜を生成する方法としては、単なる化学蒸着法（
ＣＶＯ）だけでなく、プラズマＣｖＤ法を用いても本発
明の効果は損なわれない。
また原料としてのノ・ロゲン化合物は塩素化合物が一般
的で、本発明の効果も特に著しいが他の・・ロゲン化物
を用いても本発明の効果が十分奏される。
に）発明を実施するための最良の形態 実施例１） １０問角、厚み２ｗｎのＭＯ板に、 Ｔｉ　Ｃ１４＋　ＣＦ（４＋　Ｎ２→Ｔｉ　Ｃ＋ＨＣＬ
の化学反応にて、第１表の各反応条件下で丁ＩＣを１０
μｍ　被覆した。
第　　１　　表 Ａ−Ｅの条件下で生成した薄膜をエネルギー分散型Ｘ線
集光器（ＥＤＸ）で分析したところ、塩素含有量がＡ：
５Ｘ１０’％、Ｂ：９Ｘ１０”係。
Ｃ：３×１０−３％、Ｄ：３ＸＩＱ−”係、Ｅ、：３Ｘ
１０’チであった。
実施例２） 真空機器の内壁を５ＱＸ３０ｍｍ、厚み１５惰に分割し
、化学蒸着装置内で、Ａｔ２０３　。
ＴｉＮ、　５ｊ３Ｎ４　　を第２表の条件で作成した。
Ａｌ　Ｃ１０＋　１（２＋　Ｃ０２→　Ａｌ−２０３＋
Ｃｏ　十ＨＣ４Ｔｉ　Ｃ１０４−Ｎ２　＋　Ｎ２　　→
’Ｌ’ｉ　Ｎ　　十ＨＣｔＳｉ　Ｃ１４＋　Ｎ２　＋　
Ｎ２　　→Ｓｉ３　Ｎ４　＋ＴＩＣ１ＥＤＸで塩素量を
分析したところ、ｌ’ｒ：５ＸＩＱ−３憾、　　ｏ：５
×１ｏ−２ＬＩ）、　　）■：４Ｘ１０−’係、Ｉ：３
Ｘ１０−２チ、　　Ｊ　：　７Ｘ１０−３％、に：０．
１係であった。
Ｆ−に才での条件下で１０　μｍのＡｔ２０３゜’Ｉ’
ｉＮ、　　Ｓｉ３Ｎ４　　を被覆した内壁をプラズマ発
生装置内にとりつけ、排気装置の寿命時間を比較したと
ころ、第３表のような結果を得た。
第　　３　　表

Claims (1)

    【特許請求の範囲】
  1. Ｔ１、Ｓｉ、ｋｔＸＢ　　のハロゲン化物をＨ２および
    Ｎ２、炭化水素、ＣＯ２、ＮＨ３等の反応ガス雰囲気中
    で反応させ化学蒸着法によ’ｊ）　、Ｔ　ｉ　、Ｓ　１
    ．８％Ａｔ　の炭化物、窒化物、炭窒化物、酸化物およ
    びこれらの複合体の１種以上から構成される薄膜を形成
    する際、Ｔ１％　Ｓ１％　ＡｔＮ　Ｂ　　のハ、ロゲン
    化物とＨ２比率をｏ、ｏｏｓ〜０．１とし、かつＨ２お
    よび反応ガス純度がｑｑ、ｏ％〜９９−９９％のものを
    用いることを特徴とする、薄膜中のハロ５゜ゲン含有量
    を低下させた清浄な化学蒸着膜の製造法。
JP13577382A 1982-08-05 1982-08-05 清浄な化学蒸着膜の製造法 Pending JPS5928564A (ja)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP13577382A JPS5928564A (ja) 1982-08-05 1982-08-05 清浄な化学蒸着膜の製造法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP13577382A JPS5928564A (ja) 1982-08-05 1982-08-05 清浄な化学蒸着膜の製造法

Publications (1)

Publication Number Publication Date
JPS5928564A true JPS5928564A (ja) 1984-02-15

Family

ID=15159515

Family Applications (1)

Application Number Title Priority Date Filing Date
JP13577382A Pending JPS5928564A (ja) 1982-08-05 1982-08-05 清浄な化学蒸着膜の製造法

Country Status (1)

Country Link
JP (1) JPS5928564A (ja)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5021943A (ja) * 1973-06-28 1975-03-08
JPS5421409A (en) * 1977-07-18 1979-02-17 Mitsubishi Metal Corp Method of making tungstenncarbide coating layer

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5021943A (ja) * 1973-06-28 1975-03-08
JPS5421409A (en) * 1977-07-18 1979-02-17 Mitsubishi Metal Corp Method of making tungstenncarbide coating layer

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