JPH0725637B2 - Method for producing diamond fine particles - Google Patents
Method for producing diamond fine particlesInfo
- Publication number
- JPH0725637B2 JPH0725637B2 JP61124638A JP12463886A JPH0725637B2 JP H0725637 B2 JPH0725637 B2 JP H0725637B2 JP 61124638 A JP61124638 A JP 61124638A JP 12463886 A JP12463886 A JP 12463886A JP H0725637 B2 JPH0725637 B2 JP H0725637B2
- Authority
- JP
- Japan
- Prior art keywords
- fine particles
- diamond
- reaction vessel
- diamond fine
- fibrous body
- 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.)
- Expired - Lifetime
Links
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- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】 〔概 要〕 炭化水素ガスを用いたプラズマCVD法によってダイヤモ
ンド微粒子を析出させる際に、金属繊維状体を使用して
ダイヤモンドの核生成空間密度を高めて生産量を高め
る。Detailed Description [Summary] When depositing diamond fine particles by plasma CVD method using hydrocarbon gas, metal fibrous material is used to increase nucleation space density of diamond and increase production amount. .
本発明のダイヤモンド微粒子の製造方法、より詳しく
は、プラズマCVD法によるダイヤモンド微粒子製造方法
に関するものである。The present invention relates to a method for producing diamond fine particles, and more particularly to a method for producing diamond fine particles by a plasma CVD method.
ダイヤモンド微粒子は、その高硬度等の特性を利用して
研摩材、砥粒、あるいは切削・研削工具、その他用途で
の焼結用材料として用いられている。近年、超精密加工
を行なうようになり、またファインセラミックなどの高
硬度材料の加工を行なうようになるなどでダイヤモンド
の需要が増大し、安価にかつ多量にダイヤモンド微粒子
を製造する方法が求められている。Diamond fine particles are used as an abrasive, an abrasive grain, a cutting / grinding tool, or a sintering material for other purposes by utilizing the characteristics such as high hardness. In recent years, the demand for diamond has increased due to the use of ultra-precision processing and the processing of high hardness materials such as fine ceramics, and there has been a demand for a method of manufacturing diamond fine particles inexpensively and in large quantities. There is.
従来、ダイヤモンド微粒子は、天然ダイヤモンドのほか
に人工ダイヤモンドがあり衝撃法や金属触媒法などの高
圧合成法で作られているが、天然ダイヤモンドはその産
出量が限られており、高圧合成法でもその生産量は多く
なくしかも高価である。Conventionally, fine diamond particles include artificial diamond in addition to natural diamond, and are produced by high-pressure synthesis methods such as impact method and metal catalyst method. It does not produce much and is expensive.
最近、炭化水素ガス（CH4,C4H10,C2H6など）を原料とし
たプラズマCVD（Chemical Vapour Deposition,気相反
応）法によって、ダイヤモンドを合成して微粒子又は薄
膜を形成する方法が試みられている。このような方法で
は大気圧以下の低圧力下でダイヤモンド合成ができるの
で装置が高圧合成法よりも簡単であり、さらに原料に炭
化水素ガスを用いているので安価なダイヤモンド生産生
産が可能である。Recently, a method of synthesizing diamond to form fine particles or thin film by plasma CVD (Chemical Vapor Deposition) method using hydrocarbon gas (CH 4 , C 4 H 10 , C 2 H 6 etc.) as a raw material. Is being attempted. In such a method, diamond synthesis can be performed under a low pressure of atmospheric pressure or less, so that the apparatus is simpler than the high-pressure synthesis method, and since hydrocarbon gas is used as a raw material, inexpensive diamond production and production is possible.
上述のプラズマCVD法によるダイヤモンド微粒子の製造
方法では、ダイヤモンド成長の核生成場所を有する基体
としてシリンコン（Si）あるいはモリブデン（Mo）など
の板を用いている。そのために、核生成場所はこの板表
面に限定されているのでダイヤモンド微粒子の生産量は
少ない。In the above-mentioned method for producing diamond fine particles by the plasma CVD method, a plate made of syrincon (Si) or molybdenum (Mo) is used as a substrate having a nucleation site for diamond growth. Therefore, since the nucleation site is limited to this plate surface, the production amount of diamond fine particles is small.
本発明の目的は、炭化水素ガスのプラズマCVD法による
ダイヤモンド微粒子の製造方法を改善して生産量を高め
ることである。An object of the present invention is to improve the production method of diamond fine particles by plasma CVD method of hydrocarbon gas to increase the production amount.
上記目的を達成するために、炭化水素ガスを原料とした
プラズマCVD法において、従来の板に代えて金属繊維状
体を基板として用い、これを減圧反応容器内に配置しか
つ加熱してその表面上にダイヤモンド微粒子を析出させ
る。In order to achieve the above object, in a plasma CVD method using a hydrocarbon gas as a raw material, a metal fibrous body is used as a substrate instead of a conventional plate, and this is placed in a depressurized reaction vessel and the surface thereof is heated Precipitate diamond particles on top.
減圧反応容器内に炭化水素ガスのプラズマを発生させか
つ配置した金属繊維状体を加熱するために、この反応容
器の周囲に高周波誘導コイルを設けるのが好ましい。A high frequency induction coil is preferably provided around the reaction vessel in order to generate plasma of hydrocarbon gas and heat the arranged metal fibrous body in the depressurized reaction vessel.
金属繊維状体の金属にはダイヤモンドの核生成しやすい
金属であるモリブデン、タングステン（Ｗ）、ニオブ
（Nb）、チタン（Ti）などが望ましく、誘導加熱によっ
て発熱するものである。As the metal of the metal fibrous body, molybdenum, tungsten (W), niobium (Nb), titanium (Ti), etc., which are metals that easily nucleate diamond, are desirable, and heat is generated by induction heating.
本発明にしたがって金属繊維状体とすることによって体
積当りの表面積を極めて大きくすることができ、このこ
とが核生成場所を従来の板よりも格段に多くすることに
なり、したがって、ダイヤモンド微粒子の析出が多くな
り生産量を増大することができる。The surface area per volume can be made extremely large by using the metal fibrous body according to the present invention, which makes the number of nucleation sites much larger than that of the conventional plate, and therefore the deposition of diamond fine particles. Can be increased and the production amount can be increased.
以下、添付図面を参照して本発明の実施例によって本発
明を詳しく説明する。Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.
第１図は、本発明に係るダイヤモンド微粒子の製造方法
を実施するための装置の概略図である。FIG. 1 is a schematic view of an apparatus for carrying out the method for producing diamond fine particles according to the present invention.
第１図に示したダイヤモンド微粒子の製造装置は、反応
容器（例えば、内径60mmの石英管）１と、原料ガス源で
あるメタン（CH4）ガスボンベ２および水素（H2）ガス
ボンベ３と、反応容器１をとりまく誘導コイル４および
高周波電源５（例えば、13.56MHz,500W）と、反応容器
内を排気する真空ポンプ（図示せず）とからなる。ガス
ボンベ２および３はパイプ６を介して反応容器１と連通
しており、それぞれのボンベに流動計（図示せず）と弁
7,8が設けられている。反応容器１の下流側には真空ポ
ンプにつながるパイプ９があり矢印Ａ方向に排気して反
応容器内を減圧状態にできる。この反応容器１はその中
にボート（例えば、石英ボート）11に載せた金属繊維状
体（例えば、太さ約50μｍのモリブデン線状態）12を挿
入し、そして取出すことができるようになっており、第
１図に示すようにボート11は誘導コイル４の内部領域内
に配置される。The diamond fine particle production apparatus shown in FIG. 1 comprises a reaction container (for example, a quartz tube having an inner diameter of 60 mm) 1, a methane (CH 4 ) gas cylinder 2 and a hydrogen (H 2 ) gas cylinder 3 which are source gas sources, and a reaction It comprises an induction coil 4 surrounding the vessel 1, a high frequency power source 5 (for example, 13.56 MHz, 500 W), and a vacuum pump (not shown) for exhausting the inside of the reaction vessel. The gas cylinders 2 and 3 are in communication with the reaction vessel 1 through a pipe 6, and each cylinder has a rheometer (not shown) and a valve.
7,8 are provided. A pipe 9 connected to a vacuum pump is provided on the downstream side of the reaction vessel 1, and the inside of the reaction vessel can be depressurized by exhausting in the direction of arrow A. In this reaction vessel 1, a metal fibrous body (for example, a molybdenum wire state having a thickness of about 50 μm) 12 mounted on a boat (for example, a quartz boat) 11 can be inserted and taken out. As shown in FIG. 1, the boat 11 is arranged inside the induction coil 4.
上述した装置でモリブデン繊維状体12を反応容器１内に
配置したところで、次のような条件にて炭化水素のプラ
ズマCVDによるダイヤモンド微粒子の製造（合成）を行
なった。When the molybdenum fibrous body 12 was placed in the reaction vessel 1 by the above-described apparatus, diamond fine particles were produced (synthesized) by plasma CVD of hydrocarbon under the following conditions.
モリブデン繊維状体：太さ約50μm, 重量40g, 合計長さ2000m, 表面積30cm2 反応容器内圧力:10Torr 反応温度（モリブデンの加熱温度）:800℃ 原料ガス:1vo″％CH4＋99vo″％H2 ガス流量:100SCCM 反応時間:50時間 高周波出力:500W（13.56MHz） この結果として、モリブデン繊維状体12の表面にダイヤ
モンド微粒子が析出し、その粒径は平均20μｍであっ
た。次に、モリブデン繊維状体を塩酸で溶解することに
よってダイヤモンド微粒子を回収したならば、その量は
約5gであった。Molybdenum fibrous material: Thickness about 50 μm, weight 40 g, total length 2000 m, surface area 30 cm 2 Reaction vessel pressure: 10 Torr Reaction temperature (heating temperature of molybdenum): 800 ° C Source gas: 1 vo ″% CH 4 +99 vo ″% H 2 Gas flow rate: 100 SCCM Reaction time: 50 hours High frequency output: 500 W (13.56 MHz) As a result, fine diamond particles were deposited on the surface of the molybdenum fibrous body 12, and the average particle size was 20 μm. Next, if the fine diamond particles were recovered by dissolving the molybdenum fibrous body with hydrochloric acid, the amount was about 5 g.
上述した実施例でのモリブデン繊維状体12の代りに正方
形（5cm×5cm）のモリブデン板を配置して、上述した製
造条件と同一条件でモリブデン板上にダイヤモンド微粒
子を析出させた。モリブデン板の溶解によってダイヤモ
ンド微粒子を回収したところ、その量は約0.02gであっ
た。A square (5 cm × 5 cm) molybdenum plate was placed in place of the molybdenum fibrous body 12 in the above-mentioned examples, and diamond fine particles were deposited on the molybdenum plate under the same manufacturing conditions as described above. When the fine diamond particles were recovered by melting the molybdenum plate, the amount was about 0.02 g.
本発明のダイヤモンド微粒子の製造方法によれば、ダイ
ヤモンド微粒子の核生成場所を金属板から金属繊維状体
にして大幅に増やすことができるので、ダイヤモンドの
析出量（生産量）を大幅に増やすことができる。このこ
とが、ダイヤモンド微粒子の製造コストを下げることに
なる。According to the method for producing diamond fine particles of the present invention, it is possible to significantly increase the nucleation site of diamond fine particles from a metal plate to a metal fibrous body, and thus it is possible to significantly increase the precipitation amount (production amount) of diamond. it can. This reduces the manufacturing cost of the diamond fine particles.
第１図はダイヤモンド微粒子の製造装置の概略図であ
る。 １……反応容器、５……高周波電源、 ２……CH4ガスボンベ、11……ボート、 ３……H2ガスボンベ、12……モリブデン繊維状体。 ４……誘導コイル、FIG. 1 is a schematic view of an apparatus for producing diamond fine particles. 1 ...... reaction vessel, 5 ...... high frequency power source, 2 ...... CH 4 gas cylinder, 11 ...... boat, 3 ...... H 2 gas cylinder, 12 ...... molybdenum fibrous bodies. 4 ... Induction coil,
Claims (2)
によって、減圧反応容器内に配置しかつ加熱したMo、
Ｗ、Nb、またはTiのようなダイヤモンドの核生成しやす
い金属繊維状体の表面上にダイヤモンド微粒子を析出さ
せることを特徴とするダイヤモンド微粒子の製造方法。1. Mo placed and heated in a reduced pressure reaction vessel by a plasma CVD method using a hydrocarbon gas as a raw material,
A method for producing fine diamond particles, which comprises depositing fine diamond particles on the surface of a metal fibrous body, such as W, Nb, or Ti, which easily nucleates diamond.
導コイルによって前記金属繊維状体を加熱しかつ炭化水
素のプラズマを発生させることを特徴とする特許請求の
範囲第１項記載の方法。2. The method according to claim 1, wherein the metal fibrous body is heated and a plasma of hydrocarbon is generated by a high frequency induction coil provided around the reduced pressure reaction vessel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61124638A JPH0725637B2 (en) | 1986-05-31 | 1986-05-31 | Method for producing diamond fine particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61124638A JPH0725637B2 (en) | 1986-05-31 | 1986-05-31 | Method for producing diamond fine particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62283898A JPS62283898A (en) | 1987-12-09 |
| JPH0725637B2 true JPH0725637B2 (en) | 1995-03-22 |
Family
ID=14890363
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61124638A Expired - Lifetime JPH0725637B2 (en) | 1986-05-31 | 1986-05-31 | Method for producing diamond fine particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0725637B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2534094A2 (en) * | 2010-02-13 | 2012-12-19 | McAlister Technologies, LLC | Induction for thermochemical processes, and associated systems and methods |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59184792A (en) * | 1983-04-01 | 1984-10-20 | Mitsubishi Metal Corp | Vapor phase synthesis of diamond |
-
1986
- 1986-05-31 JP JP61124638A patent/JPH0725637B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2534094A2 (en) * | 2010-02-13 | 2012-12-19 | McAlister Technologies, LLC | Induction for thermochemical processes, and associated systems and methods |
| EP2534094A4 (en) * | 2010-02-13 | 2014-01-01 | Mcalister Technologies Llc | Induction for thermochemical processes, and associated systems and methods |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62283898A (en) | 1987-12-09 |
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