JPS59137311A - Method for synthesizing polycrystalline diamond - Google Patents
Method for synthesizing polycrystalline diamondInfo
- Publication number
- JPS59137311A JPS59137311A JP58008258A JP825883A JPS59137311A JP S59137311 A JPS59137311 A JP S59137311A JP 58008258 A JP58008258 A JP 58008258A JP 825883 A JP825883 A JP 825883A JP S59137311 A JPS59137311 A JP S59137311A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- polycrystalline diamond
- plasma
- diamond
- high frequency
- 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
Links
Classifications
-
- 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
- C23C16/442—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 using fluidised bed process
Abstract
Description
【発明の詳細な説明】
本発明は多結晶質ダイヤモンドの合成法に関する。更に
詳しくはプラズマ空間で粉体を流動させ、その粉体の表
向にプラズマ化学反応によって多結品質ダイヤモンドを
析出させる方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for synthesizing polycrystalline diamond. More specifically, the present invention relates to a method of flowing powder in a plasma space and depositing polycrystalline diamond on the surface of the powder by a plasma chemical reaction.
本発明者はさきにプラズマ発生室内に基体を設置し、該
プラズマ発生室内を排気した後、これに揮発性炭化水素
と水素ガスの混合ガスを導入した後、マイクロ波まだは
高周波を入射してプラズマを誘発し、基体上に多結晶質
ダイヤモンドを析出させる方法を開発した。The present inventor first installed a substrate in a plasma generation chamber, evacuated the plasma generation chamber, introduced a mixed gas of volatile hydrocarbon and hydrogen gas, and then injected microwave or high frequency waves into the plasma generation chamber. We have developed a method to induce plasma and deposit polycrystalline diamond on a substrate.
該方法によると、ダイヤモンドの析出速度が満足すべき
程度でない問題点があった。According to this method, there was a problem that the diamond precipitation rate was not satisfactory.
本発明はこの問題点を解決すべくなされたもので、ダイ
ヤモンドの析出速度を高め、且つ微細な結晶粒子よりな
る緻密な多結晶質ダイヤモンドの合成法を提供するにあ
る。The present invention has been made to solve this problem, and its object is to provide a method for increasing the diamond precipitation rate and synthesizing dense polycrystalline diamond made of fine crystal grains.
本発明者らはダイヤモンドの析出速度のおそい原因につ
いて検討した結果、その析出の過程は加熱した基体表面
への反応物体の気体の輸送、加熱した基体表面での化学
反応による析出、化学反応によって副生じた副成生成物
の脱離、及び逆拡散などの過程を経ている。従って、加
熱した基体と反応カスの境界に拡散層が形成され、この
拡散層の存在が反応カスの基体表面への拡散速度を阻害
することに起因すること、そして析出速度を上昇させる
ためには、この拡散層を破り、副生気体の逆拡散を促進
することが必要であり、そのためには基体として粉体を
用い、これをプラズマ中で流動させると粉体間の衝突が
生じ、その衝突の際に拡散層が破られ、ダイヤモンドの
析出速度が促進されることが分った。この究明事実に基
いて本発明を完成した。The present inventors investigated the causes of the slow precipitation rate of diamond and found that the precipitation process involves transport of reactant gas to the heated substrate surface, precipitation due to a chemical reaction on the heated substrate surface, and side effects caused by a chemical reaction. The resulting by-products undergo processes such as desorption and back-diffusion. Therefore, a diffusion layer is formed at the boundary between the heated substrate and the reaction scum, and the existence of this diffusion layer inhibits the diffusion rate of the reaction scum to the substrate surface, and in order to increase the precipitation rate, , it is necessary to break this diffusion layer and promote back-diffusion of by-product gases.To do this, powder is used as a substrate, and when it is flowed in a plasma, collisions between the powders occur, and the collisions occur. It was found that during this process, the diffusion layer was broken and the rate of diamond precipitation was accelerated. The present invention was completed based on this finding.
；本発明の要旨は、揮発性炭化水素と水素との混’、＆
、：’ガスに高周波まだはマイクロ波を入射してプラ１
・
ズマを誘発させ、このプラズマ空間でダイヤモンド粉末
または金属、非金属無機質粉末を流動させて、これら粉
末の表面に多結晶質ダイヤモンドを被覆または粉末を核
として粒状多結晶質ダイヤモンドを合成することを特徴
とする多結晶質ダイヤモンドの合成法にある。; The gist of the present invention is the mixing of volatile hydrocarbons and hydrogen;
, :'Injecting high frequency or microwave into the gas
- By inducing Zuma and flowing diamond powder or metal or non-metallic inorganic powder in this plasma space, the surface of these powders can be coated with polycrystalline diamond or granular polycrystalline diamond can be synthesized using the powder as a core. The main feature lies in the method of synthesizing polycrystalline diamond.
本発明の方法を図面に基いて説明すると、第１図は高周
波プラズマを用い、粉末の流動を音波によって振動板を
振動させて行う方法、第２図はマイクロ波てラズマを用
い、粉末の流動を機械的な方法によって振動板を振動さ
せて行う方法の概要図を示す。図中、１は低周波発振機
、２は増幅機、３は拡声器、４は振動板、５は高周波発
振機、６は同軸ケーブル、７は高周波コイル、８はプラ
ズマ発生室、９は粉体、１０はガス供給装置、１１は混
合ガス供給管、１２は排気装置、１３，１４゜１５．１
６は調整弁、１７はマイクロ波発振機、１８は導波管、
１９は電磁石を示す。The method of the present invention will be explained based on the drawings. Figure 1 shows a method in which high-frequency plasma is used to cause powder flow by vibrating a diaphragm using sound waves, and Figure 2 shows a method in which powder flow is performed using microwave lasma. A schematic diagram of a method for performing this by mechanically vibrating a diaphragm is shown. In the figure, 1 is a low frequency oscillator, 2 is an amplifier, 3 is a loudspeaker, 4 is a diaphragm, 5 is a high frequency oscillator, 6 is a coaxial cable, 7 is a high frequency coil, 8 is a plasma generation chamber, 9 is a powder 10 is a gas supply device, 11 is a mixed gas supply pipe, 12 is an exhaust device, 13, 14゜15.1
6 is a regulating valve, 17 is a microwave oscillator, 18 is a waveguide,
19 indicates an electromagnet.
先ず、プラズマ発生室８に粉体９を入れ、排気装置１２
を作動して装置内を減圧した後、調整弁１３．１４．１
５を調整してガス供給装置１０より水素ガス、揮発性炭
化水素との混合ガスを混合ガス供給管１１を通じ□てプ
ラズマ発生室８内に供給して所定の圧力に保持する。次
に低周波発振機１、増幅機２を作動し、拡声器３または
電磁石１９により振動板４を振動させ、低周波発振機１
０周波数、増幅機２の出力を調整して粉体９を適切な状
態で流動させる。First, the powder 9 is put into the plasma generation chamber 8, and the exhaust device 12
After reducing the pressure inside the device by operating the regulating valve 13.14.1
5, a gas mixture of hydrogen gas and volatile hydrocarbon is supplied from the gas supply device 10 into the plasma generation chamber 8 through the mixed gas supply pipe 11 and maintained at a predetermined pressure. Next, the low frequency oscillator 1 and the amplifier 2 are activated, the diaphragm 4 is vibrated by the loudspeaker 3 or the electromagnet 19, and the low frequency oscillator 1
0 frequency and the output of the amplifier 2 are adjusted to flow the powder 9 in an appropriate state.
第１図においては高周波発振機５を作動してそΩ：出力
を高周波コイル７に与え、流動層中にプラズマを誘発す
る。第２図においてはマイクロ波発振機１７を作動して
、その出力を導波管１８を通じてプラズマ発生室８内に
入射し、流動層中にプラズマを誘発する。In FIG. 1, a high frequency oscillator 5 is operated to apply an output to a high frequency coil 7 to induce plasma in the fluidized bed. In FIG. 2, the microwave oscillator 17 is activated and its output is input into the plasma generation chamber 8 through the waveguide 18 to induce plasma in the fluidized bed.
本発明に用いる揮発性炭化水素としては、例えば、メタ
ン、エタン、アセチレン、ブタン等が挙げられる。メタ
ンは安価で入手し易い点で好ましい。揮発性炭化水素と
水素との割合は、２０：ｉ：１．ｐ ｏ 、望ましくは
５・１００以下あること、ままた１粉体としでは、ダイ
ヤモンド、α−Ａ１２０５ ＋り；・ ・
トン−ンル、モリブデン等が基げられる。その粒度は３
００μｍ以下であることが好捷しい。Examples of volatile hydrocarbons used in the present invention include methane, ethane, acetylene, and butane. Methane is preferred because it is cheap and easily available. The ratio of volatile hydrocarbon to hydrogen is 20:i:1. po is desirably 5.100 or less, and examples of the powder include diamond, α-A1205 + tons, molybdenum, and the like. Its particle size is 3
It is preferable that the thickness is 00 μm or less.
実施例１゜
第１図の装置において、粉体としてダイヤモンド粉末（
３０μｍ）、反応ガスとして、メタンと水素との混合カ
スを使用した。排気装Ｎ１２を作動してプラズマ発生室
８内を充分排気した後、カス供給装置１０より調整弁１
３，１４，１５．１６を調整してメタンガス濃度３％の
水素との混合ガスタプライマ発生￥８内に導入し、該プ
ラズマ発生室８内の圧力を０．０６気圧になるように混
合カスの流速５０ ＣＩＬ／ ｍｉｎで供給した。次に
低周波発振機１．増幅機２を調整して拡声器３に８０ヘ
ルツ、５Ｗの出力を与えて振動板４を振動させてダイヤ
モンド粉末９を流動させた。ついで、高周波発振機５
（１３，５６ＭＨｚ ） 、８００Ｗの出力を同軸ケー
ブル６を通じて高周波コイル７に与え、流動層中にプラ
ズマを誘発させた。３時間析出を行ったところ、粒径４
２μｍの粒状多結晶体ダイヤモンドが得られた。Example 1 In the apparatus shown in Fig. 1, diamond powder (
30 μm), and a mixed residue of methane and hydrogen was used as the reaction gas. After operating the exhaust system N12 to sufficiently exhaust the inside of the plasma generation chamber 8, the control valve 1 is opened from the waste supply device 10.
3, 14, 15, and 16 are adjusted and introduced into the gas star primer generation ¥8 with methane gas concentration of 3% and hydrogen, and the mixed gas is adjusted so that the pressure inside the plasma generation chamber 8 becomes 0.06 atm. It was supplied at a flow rate of 50 CIL/min. Next, low frequency oscillator 1. The amplifier 2 was adjusted to give an output of 80 Hz and 5 W to the loudspeaker 3 to vibrate the diaphragm 4 and cause the diamond powder 9 to flow. Next, high frequency oscillator 5
(13.56 MHz) and an output of 800 W was applied to the high frequency coil 7 through the coaxial cable 6 to induce plasma in the fluidized bed. After 3 hours of precipitation, the particle size was 4.
A 2 μm granular polycrystalline diamond was obtained.
実施例２゜
実施例１と同様な条件でマイクロ波（２４５０ＭＨｚ
） 、６００Ｗの出力をプラズマ発生室８内に入射し、
流動層中にプラズマを誘発した。振動板４の振動は低周
波発振機１、及び増幅機２を作動し、゛電磁石１９を作
用させて行った。３時間析出を行ったところ、粒径５０
μｍの粒状多結晶体ダイヤモンドが得られた。Example 2゜ Microwave (2450MHz
), an output of 600 W is input into the plasma generation chamber 8,
A plasma was induced in the fluidized bed. The diaphragm 4 was vibrated by operating the low frequency oscillator 1 and the amplifier 2, and by using the electromagnet 19. After 3 hours of precipitation, the particle size was 50.
A granular polycrystalline diamond of μm size was obtained.
実施例３゜
、実施例１と同様な条件で粉体としてアルミナ（２０μ
ｍ）、タンタル（２０μｍ）を使用した場合、３時間析
出を行ったところ各々、粒径３０μｍ、３５μｍの多結
晶体ダイヤモンドが得られた。Example 3゜Alumina (20μ
m), when tantalum (20 μm) was used, polycrystalline diamonds with grain sizes of 30 μm and 35 μm were obtained after 3 hours of precipitation, respectively.
本発明の方法によると、静止した板状の基体表面に析出
させる場合に比較してその成長速度を数倍に上昇できる
。また添加物を加えることなしに粒状の多結晶体ダイヤ
モンドを合成することかで１図は高周波プラズマを用い
、粉末の流動を音波によって振動板全振動させて行う方
法、第２図はマイクロ波プラズマを用い、粉末の流動を
機械的な方法によって振動板を振動させる方法の概要図
である。According to the method of the present invention, the growth rate can be increased several times compared to when depositing on the surface of a stationary plate-like substrate. In addition, granular polycrystalline diamond can be synthesized without adding additives. Figure 1 shows a method using high-frequency plasma and the flow of powder is made by vibrating the entire diaphragm using sound waves, and Figure 2 shows a method using microwave plasma. FIG. 2 is a schematic diagram of a method of vibrating a diaphragm using a mechanical method of powder flow.
１：低周波発振機、 ２：増幅機、
３：拡声器、 ４：振動板、
５：高周波コイル、 ６：同軸ケーブル、７；；：
高周波コイル、 ８：プラズマ発生室、９：粉体、
１０：ガス供給装置、１１：混合ガス供給
管、 １２：排気装置、１３ 、１４ 、１５ 、１６
：調整弁、１７：マイクロ波発振機、１８：導波管、
１９：電磁石。1: Low frequency oscillator, 2: Amplifier, 3: Loudspeaker, 4: Diaphragm, 5: High frequency coil, 6: Coaxial cable, 7;;:
High frequency coil, 8: Plasma generation chamber, 9: Powder,
10: Gas supply device, 11: Mixed gas supply pipe, 12: Exhaust device, 13, 14, 15, 16
: Regulating valve, 17: Microwave oscillator, 18: Waveguide,
19: Electromagnet.
Claims (1)
はマイクロ波を入射してプラズマを誘発させ、このプラ
ズマ空間でダイヤモンド粉末または金属、非金属無機質
粉末を流動させて、これら粉末の表面に多結晶質ダイヤ
モンドを被覆または粉末を核として粒状多結晶質ダイヤ
モンドを合成することを特徴とする多結晶質ダイヤモン
ドの合成法。 ２ 流動を音波または機械的手段により振動板を振動さ
せることによって行う特許請求の範囲第１項記載の多結
晶質ダイヤモンドの合成法。[Claims] 1. Plasma is induced by injecting high frequency waves or microwaves into a mixed gas of volatile hydrocarbon and hydrogen, and diamond powder or metal or nonmetallic inorganic powder is made to flow in this plasma space. A method for synthesizing polycrystalline diamond characterized by coating the surface of these powders with polycrystalline diamond or synthesizing granular polycrystalline diamond using the powder as a core. 2. The method for synthesizing polycrystalline diamond according to claim 1, wherein the flow is carried out by vibrating a diaphragm using sound waves or mechanical means.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58008258A JPS59137311A (en) | 1983-01-21 | 1983-01-21 | Method for synthesizing polycrystalline diamond |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58008258A JPS59137311A (en) | 1983-01-21 | 1983-01-21 | Method for synthesizing polycrystalline diamond |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59137311A true JPS59137311A (en) | 1984-08-07 |
| JPS6257568B2 JPS6257568B2 (en) | 1987-12-01 |
Family
ID=11688118
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58008258A Granted JPS59137311A (en) | 1983-01-21 | 1983-01-21 | Method for synthesizing polycrystalline diamond |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59137311A (en) |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62138395A (en) * | 1985-12-09 | 1987-06-22 | Kyocera Corp | Preparation of diamond film |
| EP0226898A2 (en) * | 1985-12-24 | 1987-07-01 | Sumitomo Electric Industries, Ltd. | Composite powder, composite bodies and process for their production |
| JPS63156009A (en) * | 1986-12-19 | 1988-06-29 | Natl Inst For Res In Inorg Mater | Synthesis of fine diamond powder |
| US4767608A (en) * | 1986-10-23 | 1988-08-30 | National Institute For Research In Inorganic Materials | Method for synthesizing diamond by using plasma |
| WO1988007599A1 (en) * | 1987-03-23 | 1988-10-06 | Showa Denko Kabushiki Kaisha | Composite diamond particles |
| JPS63270394A (en) * | 1987-04-28 | 1988-11-08 | Showa Denko Kk | Flow type method for synthesizing diamond and apparatus therefor |
| JPH01108105A (en) * | 1987-10-20 | 1989-04-25 | Yoichi Hirose | Composite particle of diamond and production thereof |
| US4859493A (en) * | 1987-03-31 | 1989-08-22 | Lemelson Jerome H | Methods of forming synthetic diamond coatings on particles using microwaves |
| EP0448660A1 (en) * | 1989-09-15 | 1991-10-02 | TBX, Inc. | Conversion of organic/organometallic gaseous or vaporizable compounds into inert solids |
| US5110405A (en) * | 1988-06-09 | 1992-05-05 | Kabushiki Kaisha Toshiba | Method of manufacturing single-crystal diamond particles |
| US5180571A (en) * | 1990-05-30 | 1993-01-19 | Idemitsu Petrochemical Company Limited | Process for the preparation of diamond |
| US5372799A (en) * | 1988-10-20 | 1994-12-13 | Sumitomo Electric Industries, Ltd. | Process for the synthesis of granular diamond |
| US5783335A (en) * | 1992-04-07 | 1998-07-21 | The Regents Of The University Of California, Office Of Technology Transfer | Fluidized bed deposition of diamond |
| US6015597A (en) * | 1997-11-26 | 2000-01-18 | 3M Innovative Properties Company | Method for coating diamond-like networks onto particles |
| US6265068B1 (en) | 1997-11-26 | 2001-07-24 | 3M Innovative Properties Company | Diamond-like carbon coatings on inorganic phosphors |
-
1983
- 1983-01-21 JP JP58008258A patent/JPS59137311A/en active Granted
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62138395A (en) * | 1985-12-09 | 1987-06-22 | Kyocera Corp | Preparation of diamond film |
| EP0226898B1 (en) * | 1985-12-24 | 1992-08-26 | Sumitomo Electric Industries, Ltd. | Composite powder, composite bodies and process for their production |
| EP0226898A2 (en) * | 1985-12-24 | 1987-07-01 | Sumitomo Electric Industries, Ltd. | Composite powder, composite bodies and process for their production |
| US5672382A (en) * | 1985-12-24 | 1997-09-30 | Sumitomo Electric Industries, Ltd. | Composite powder particle, composite body and method of preparation |
| US4767608A (en) * | 1986-10-23 | 1988-08-30 | National Institute For Research In Inorganic Materials | Method for synthesizing diamond by using plasma |
| JPS63156009A (en) * | 1986-12-19 | 1988-06-29 | Natl Inst For Res In Inorg Mater | Synthesis of fine diamond powder |
| WO1988007599A1 (en) * | 1987-03-23 | 1988-10-06 | Showa Denko Kabushiki Kaisha | Composite diamond particles |
| US5080975A (en) * | 1987-03-23 | 1992-01-14 | Showa Denko K. K. | Composite diamond granules |
| US4859493A (en) * | 1987-03-31 | 1989-08-22 | Lemelson Jerome H | Methods of forming synthetic diamond coatings on particles using microwaves |
| JPS63270394A (en) * | 1987-04-28 | 1988-11-08 | Showa Denko Kk | Flow type method for synthesizing diamond and apparatus therefor |
| JPH01108105A (en) * | 1987-10-20 | 1989-04-25 | Yoichi Hirose | Composite particle of diamond and production thereof |
| US5110405A (en) * | 1988-06-09 | 1992-05-05 | Kabushiki Kaisha Toshiba | Method of manufacturing single-crystal diamond particles |
| US5372799A (en) * | 1988-10-20 | 1994-12-13 | Sumitomo Electric Industries, Ltd. | Process for the synthesis of granular diamond |
| EP0448660A1 (en) * | 1989-09-15 | 1991-10-02 | TBX, Inc. | Conversion of organic/organometallic gaseous or vaporizable compounds into inert solids |
| US5180571A (en) * | 1990-05-30 | 1993-01-19 | Idemitsu Petrochemical Company Limited | Process for the preparation of diamond |
| US5783335A (en) * | 1992-04-07 | 1998-07-21 | The Regents Of The University Of California, Office Of Technology Transfer | Fluidized bed deposition of diamond |
| US6015597A (en) * | 1997-11-26 | 2000-01-18 | 3M Innovative Properties Company | Method for coating diamond-like networks onto particles |
| US6197120B1 (en) | 1997-11-26 | 2001-03-06 | 3M Innovative Properties Company | Apparatus for coating diamond-like networks onto particles |
| US6265068B1 (en) | 1997-11-26 | 2001-07-24 | 3M Innovative Properties Company | Diamond-like carbon coatings on inorganic phosphors |
| US6548172B2 (en) | 1997-11-26 | 2003-04-15 | 3M Innovative Properties Company | Diamond-like carbon coatings on inorganic phosphors |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6257568B2 (en) | 1987-12-01 |
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