JPS58156594A - Preparation of hard coating film - Google Patents

Preparation of hard coating film

Info

Publication number
JPS58156594A
JPS58156594A JP57037042A JP3704282A JPS58156594A JP S58156594 A JPS58156594 A JP S58156594A JP 57037042 A JP57037042 A JP 57037042A JP 3704282 A JP3704282 A JP 3704282A JP S58156594 A JPS58156594 A JP S58156594A
Authority
JP
Japan
Prior art keywords
substrate
plasma
heated
gas
coil
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.)
Granted
Application number
JP57037042A
Other languages
Japanese (ja)
Other versions
JPH0366280B2 (en
Inventor
Naoharu Fujimori
直治 藤森
Akira Doi
陽 土居
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Electric Industries Ltd
Original Assignee
Sumitomo Electric Industries Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Sumitomo Electric Industries Ltd filed Critical Sumitomo Electric Industries Ltd
Priority to JP57037042A priority Critical patent/JPS58156594A/en
Publication of JPS58156594A publication Critical patent/JPS58156594A/en
Publication of JPH0366280B2 publication Critical patent/JPH0366280B2/ja
Granted legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/04—Diamond

Abstract

PURPOSE:To apply a hard diamond film on a substrate, in high efficiency, by introducing a gaseous mixture of hydrocarbons and hydrogen into a closed vessel containing a heated substrate, and heating the gas with red-hot metal wire and at the same time generating a plasma in the gas. CONSTITUTION:A table containing a heating coil 11 is placed in a closed vessel 5, and a substrate 10 is placed on the table. The substrate is heated by operating the electric source 12, and a mixed gas of hydrocarbons 2 and hydrogen 1 supplied through the flow meters 3, 4 is introduced into the vessel 5. A plasma is generated in the mixed gas by the coil 7 connected to the electric source 8, and the gas is heated with red-hot heater 8 heated by the electric source 9 between the plasma coil 7 and the substrate 10 to accelerate the reaction. A hard diamond coating film is formed on the substrate 10 by this process.

Description

【発明の詳細な説明】 本発明はダイヤモンドの気相合成特に被覆膜の合成に適
した製造法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a manufacturing method suitable for vapor phase synthesis of diamond, particularly for the synthesis of coatings.

ダイヤモンドは物質中膜も硬い物質であり、高熱伝導度
を有しながら絶縁体であるという独特の性質を持ってい
る為に各種の工業的応用が考えられている。しかしなが
ら周知の如くダイヤモンドは天然でも合成でも極めて高
価な物質であるのでその用途は限定されていた。しかし
近年気相からのダイヤモンド合成もしくは被覆技術が進
歩し工業的に実用可能とまで云われている。発明者等は
気相よりダイヤモンド被膜を歩留よく合成する方法につ
いて種々検討し、本発明に至った。Diamond is a hard material and has a unique property of being an insulator while having high thermal conductivity, so it is being considered for various industrial applications. However, as is well known, diamond is an extremely expensive substance, whether natural or synthetic, so its uses have been limited. However, in recent years, diamond synthesis or coating technology from the gas phase has progressed, and it is said to be industrially practical. The inventors have conducted various studies on methods for synthesizing diamond coatings in a high yield from the gas phase, and have arrived at the present invention.

従来より希薄な炭化水素雰囲気中でのダイヤモンドの成
長について知られているが、この反応は高温においても
生成速度があまりにも遅く工業的に採用されるに至って
いない。これを解決する為にタングステン等の金属線に
直接通電して高温にしてガスを通過する時に炭化水素に
分解を起すことが提案されている。Although diamond growth in a dilute hydrocarbon atmosphere has been known, the growth rate of this reaction is too slow even at high temperatures and has not been adopted industrially. In order to solve this problem, it has been proposed to directly apply electricity to a metal wire such as tungsten, raise the temperature, and cause it to decompose into hydrocarbons when gas passes through it.

本発明の特徴は、金属線によるガスの加熱と同時シープ
ラズマを発生させて反応を促進することにある。一般に
プラズマ中でイオンや電子が反応促進効果を果すとされ
ているが、本発明においては金属線による加熱とプラズ
マ発生を組合せることによってピ・イ・ヤモンド被膜を
効率よく生成させることができることを見出した。A feature of the present invention is that the reaction is promoted by heating the gas with a metal wire and simultaneously generating sea plasma. It is generally believed that ions and electrons have a reaction promoting effect in plasma, but in the present invention, it is possible to efficiently generate a P.I.Yamond film by combining heating with a metal wire and plasma generation. I found it.

第１図は本発明の方法に用いる装置の一例を示す概念図
であり、基板ｌＯを電源１２より通電発熱する加熱コイ
ル１１を内蔵する台の上に載せ、これを密閉容器５の中
に設置し、流量８．４にょつて調製されたＨｓ　　及び
炭化水素を流す。この混合ガスは電源８に接続するコイ
ル７によってプラズマを発生し、基板に至る途中に設け
られた電源９によって赤熱するタングステン等の一ビ、
−タｓがあり、これを通過して基板ｌＯ上に被覆層（ダ
イヤモンド）を形成せしめるものである。FIG. 1 is a conceptual diagram showing an example of the apparatus used in the method of the present invention, in which a substrate 10 is placed on a stand containing a heating coil 11 that is energized by a power source 12 and generates heat, and this is placed in a closed container 5. Then, flow the Hs and hydrocarbons prepared at a flow rate of 8.4. This mixed gas generates plasma by a coil 7 connected to a power source 8, and is heated by a power source 9 installed on the way to the substrate, such as tungsten or the like.
There is a -ta s through which a coating layer (diamond) is formed on the substrate IO.

上記プラズマは、高周波、直流、マ、イクロ波のいずれ
でも発生するが、本発明においてはそのいずれでも効果
は同じである。The above-mentioned plasma can be generated by any of high frequency, direct current, microwave, and microwave waves, but in the present invention, the effect is the same with any of them.

次に実施例によって説明する。Next, an example will be explained.

実施例 第１図においてＨｓ　ｌ及びＣＨ４２から流量計によっ
てＨ１＋１００　ＣＣ／ｍｉｎ　ｅ　ＣＨ４２ＣＣ／ｍ
ｉｎ　　に調整して混合ガスを導入した。石英の反応管
５の外周から人力２００Ｗで１３．５６　ＭＨｚの高周
波によってプラズマを発生せしめ、Ｗヒータ８によって
約２０００℃に加熱した。Ｓｉ　　単結晶基板ｌＯはヒ
ーターにより８００℃に保ち、バルブ６と１８の間を真
空ポンプ１４により５　Ｔｏｒｒ　　として１時間の処
理を行った。Example In Fig. 1, H1+100 CC/min e CH42CC/m is calculated from Hs l and CH42 by a flowmeter.
The mixed gas was introduced after adjusting the temperature to in. Plasma was generated from the outer periphery of the quartz reaction tube 5 by a high frequency of 13.56 MHz using 200 W of manual power, and heated to about 2000° C. by a W heater 8 . The Si single crystal substrate IO was kept at 800° C. with a heater, and the vacuum pump 14 was used to set the pressure between the valves 6 and 18 at 5 Torr for one hour.

これによって基板上に緻密なダイヤモンド被膜が第１図
において、上記と全く同じ条件でたＮ　、ＲＦコイルに
高周波電源を投入しないでプラズマ発生なしで処理した
場合は０，５μのダイヤモンドが生成したに過ぎず、本
発明の方法では８倍の生成速度であった。As a result, a dense diamond film was formed on the substrate as shown in Fig. 1. If the process was performed under the same conditions as above, without applying a high frequency power to the RF coil and without generating plasma, diamonds of 0.5μ would have been formed. However, the production rate was 8 times faster in the method of the present invention.

以上説明した如く、本発明の方法でダイヤモンドが効率
よく生成するため、ヒートシンク材各種工具等工業的に
広い範囲に応用することができる。As explained above, since diamond is efficiently generated by the method of the present invention, it can be applied to a wide range of industrial applications such as heat sink materials and various tools.

【図面の簡単な説明】[Brief explanation of drawings]

第１図は本発明の方法に用いる装置の１例を示す概念図
である。 １：水素ボンベ、２：炭化水素ボンベ、８．４：流量計
、５：反応容器、６．１８：パルプ、７：コイル、８：
プラズマ電源、９．１２：Ａｃ電源、８、ｌｌ：ヒータ
ー、１０：基板、１４：真空ポンプ。FIG. 1 is a conceptual diagram showing an example of an apparatus used in the method of the present invention. 1: Hydrogen cylinder, 2: Hydrocarbon cylinder, 8.4: Flowmeter, 5: Reaction vessel, 6.18: Pulp, 7: Coil, 8:
Plasma power supply, 9.12: Ac power supply, 8, 11: Heater, 10: Substrate, 14: Vacuum pump.

Claims (1)

【特許請求の範囲】[Claims] 密閉容器中に基板を加熱状態に設置し、該容器内に炭化
水素及び水素の混合ガス気流を通し赤熱した金属線を設
けると共に上記ガスでブラ゛ズマをA substrate is placed in a heated state in a sealed container, a red-hot metal wire is provided through a mixed gas flow of hydrocarbon and hydrogen in the container, and a plasma is generated with the gas.
JP57037042A 1982-03-08 1982-03-08 Preparation of hard coating film Granted JPS58156594A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP57037042A JPS58156594A (en) 1982-03-08 1982-03-08 Preparation of hard coating film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP57037042A JPS58156594A (en) 1982-03-08 1982-03-08 Preparation of hard coating film

Related Child Applications (1)

Application Number Title Priority Date Filing Date
JP1523091A Division JPH0645898B2 (en) 1991-02-06 1991-02-06 Hard coating manufacturing equipment

Publications (2)

Publication Number Publication Date
JPS58156594A true JPS58156594A (en) 1983-09-17
JPH0366280B2 JPH0366280B2 (en) 1991-10-16

Family

ID=12486539

Family Applications (1)

Application Number Title Priority Date Filing Date
JP57037042A Granted JPS58156594A (en) 1982-03-08 1982-03-08 Preparation of hard coating film

Country Status (1)

Country Link
JP (1) JPS58156594A (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60118694A (en) * 1983-11-29 1985-06-26 Mitsubishi Metal Corp Method for synthesizing diamond under low pressure
JPS60122794A (en) * 1983-12-01 1985-07-01 Mitsubishi Metal Corp Low pressure vapor phase synthesis method of diamond
JPS60124258A (en) * 1983-12-08 1985-07-03 Mitsubishi Metal Corp Surface-covered printing dot pin
JPS62158195A (en) * 1985-12-27 1987-07-14 Natl Inst For Res In Inorg Mater Synthesizing method of diamond
JPS63128179A (en) * 1986-11-18 1988-05-31 Sumitomo Electric Ind Ltd Method and apparatus for synthesizing hard boron nitride
JPS63182297A (en) * 1986-12-22 1988-07-27 ゼネラル・エレクトリック・カンパニイ Aggregate diamond
JPS63215595A (en) * 1987-03-02 1988-09-08 Nachi Fujikoshi Corp Method and apparatus for vapor phase synthesis of diamond
CN103553036A (en) * 2013-09-29 2014-02-05 陈晖� Circuit for synthesis of diamond

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5528547A (en) * 1978-08-18 1980-02-29 Matsushita Electric Ind Co Ltd Magnetic recorder/reproducer

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5528547A (en) * 1978-08-18 1980-02-29 Matsushita Electric Ind Co Ltd Magnetic recorder/reproducer

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60118694A (en) * 1983-11-29 1985-06-26 Mitsubishi Metal Corp Method for synthesizing diamond under low pressure
JPS60122794A (en) * 1983-12-01 1985-07-01 Mitsubishi Metal Corp Low pressure vapor phase synthesis method of diamond
JPS60124258A (en) * 1983-12-08 1985-07-03 Mitsubishi Metal Corp Surface-covered printing dot pin
JPH0459148B2 (en) * 1983-12-08 1992-09-21 Mitsubishi Materials Corp
JPS62158195A (en) * 1985-12-27 1987-07-14 Natl Inst For Res In Inorg Mater Synthesizing method of diamond
JPH0372038B2 (en) * 1985-12-27 1991-11-15 Kagaku Gijutsucho Mukizaishitsu Kenkyushocho
JPS63128179A (en) * 1986-11-18 1988-05-31 Sumitomo Electric Ind Ltd Method and apparatus for synthesizing hard boron nitride
JPS63182297A (en) * 1986-12-22 1988-07-27 ゼネラル・エレクトリック・カンパニイ Aggregate diamond
JPH0472798B2 (en) * 1986-12-22 1992-11-19 Gen Electric
JPS63215595A (en) * 1987-03-02 1988-09-08 Nachi Fujikoshi Corp Method and apparatus for vapor phase synthesis of diamond
CN103553036A (en) * 2013-09-29 2014-02-05 陈晖� Circuit for synthesis of diamond

Also Published As

Publication number Publication date
JPH0366280B2 (en) 1991-10-16

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