JPS63236791A - Production of diamond - Google Patents
Production of diamondInfo
- Publication number
- JPS63236791A JPS63236791A JP6934287A JP6934287A JPS63236791A JP S63236791 A JPS63236791 A JP S63236791A JP 6934287 A JP6934287 A JP 6934287A JP 6934287 A JP6934287 A JP 6934287A JP S63236791 A JPS63236791 A JP S63236791A
- Authority
- JP
- Japan
- Prior art keywords
- substrate
- diamond
- diamond according
- microwave
- vacuum chamber
- 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
Links
- 239000010432 diamond Substances 0.000 title claims abstract description 72
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 56
- 238000004519 manufacturing process Methods 0.000 title claims description 24
- 239000000758 substrate Substances 0.000 claims abstract description 56
- 239000007789 gas Substances 0.000 claims abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012495 reaction gas Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 230000005684 electric field Effects 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 239000004809 Teflon Substances 0.000 claims description 2
- 229920006362 Teflon® Polymers 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims 2
- 239000007924 injection Substances 0.000 claims 2
- 239000004215 Carbon black (E152) Substances 0.000 claims 1
- 238000005498 polishing Methods 0.000 claims 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 6
- 239000001257 hydrogen Substances 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000010408 film Substances 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- -1 alicyclic hydrocarbons Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910001179 chromel Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- FHTQCUNSKSWOHF-UHFFFAOYSA-N ethyl carbamate;silicon Chemical compound [Si].CCOC(N)=O FHTQCUNSKSWOHF-UHFFFAOYSA-N 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、マイクロ波プラズマの利用によるダイヤモン
ド薄膜の製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method of manufacturing a diamond thin film using microwave plasma.
従来の技術
ダイヤモンドは、硬度及び耐摩耗性に優れていることか
ら従来切削部材や耐摩耗部材としての用途があった。近
年では、ダイヤモンドの優れた電気絶縁性、熱伝導性を
活かし、半導体の高集積化に伴って１．熱伝導性の良い
絶縁膜、表面保護膜またバンドギャップの大きい半導体
といった電子材料としても注目され低圧下でのダイヤモ
ンドの形成の試みが成されている。BACKGROUND OF THE INVENTION Diamond has conventionally been used as cutting members and wear-resistant members because of its excellent hardness and wear resistance. In recent years, taking advantage of diamond's excellent electrical insulation and thermal conductivity, 1. Diamond is attracting attention as an electronic material such as an insulating film with good thermal conductivity, a surface protection film, and a semiconductor with a large band gap, and attempts have been made to form diamond under low pressure.
従来ダイヤモンドの製造方法としては、マイクロ波プラ
ズマ放電を用いる方法が主として研究されている。第３
図に従来の装置の代表例を示した。Conventionally, as a method for manufacturing diamond, a method using microwave plasma discharge has been mainly studied. Third
The figure shows a typical example of a conventional device.
３１は石英管、３２は導波管、３５は基体、３６は基体
ホルダーである。石英管３１内に基体４の上方にあるガ
ス導入部からメタンと水素の混合ガ五を、混合比１：１
００となるようにして導入し、排気を行うことで、石英
管３１内を所要の圧力（数十〜数百Ｔｏｒｒ）に維持す
る。導入した混合ガスを基体、４の側方にある導波管３
２から導入したマイクロ波（２４５ＧＨｚ ）を用いて
プラズマ放電によシ、８００ ”Ｃ〜１ ｏｏｏ’ｃｏ
基体３６上ニタイヤモンドを形成する。（特開昭６０−
６４９９６号「ダイヤモンドの合成法」）
発明が解決しようとする問題点
このような従来の技術では、ダイヤモンドの形成速度が
非常に遅いという問題点を有していた。31 is a quartz tube, 32 is a waveguide, 35 is a substrate, and 36 is a substrate holder. A mixture of methane and hydrogen is introduced into the quartz tube 31 from the gas introduction part above the base 4 at a mixing ratio of 1:1.
By introducing the quartz tube so that the pressure becomes 0.00 and exhausting the air, the inside of the quartz tube 31 is maintained at a required pressure (several tens to hundreds of Torr). The introduced mixed gas is passed through the waveguide 3 on the side of the base and 4.
Plasma discharge was generated using the microwave (245 GHz) introduced from 2, 800 ”C ~ 1 ooo'co
A diamond is formed on the substrate 36. (Unexamined Japanese Patent Publication 1986-
No. 64996 "Diamond Synthesis Method") Problems to be Solved by the Invention These conventional techniques had the problem that the rate of diamond formation was very slow.
これに対して本発明者らが実験を行った結果、ダイヤモ
ンドの形成速度はメタン律速となっていることを発見し
た。しかし、従来の技術では、良質のダイヤモンドが形
成されるのは、メタンと水素の混合比が、メタン／水素
が１％以下という極めてメタンの少ない領域だけに限定
されており、１チを越えると、グラファイト等のダイヤ
モンド構造をとらない部分と多く含む膜が形成されてし
まう。従って１％の混合比のまま、メタンを増やすには
、真空槽内のガス圧を上げなければならないが、実験の
結果ガス圧を高くすると放電は不安定となシ、さらに数
百Ｔｏｒｒを超えると放電しないことがわかった。加え
て、従来の形成条件は基板温度等に大きく影響されやす
いものであシ、再現性に乏しいものであった。As a result of experiments conducted by the present inventors, it was discovered that the rate of diamond formation is determined by methane. However, with conventional technology, high-quality diamonds are formed only in areas where the mixing ratio of methane and hydrogen is extremely low, with a methane/hydrogen ratio of 1% or less; , a film is formed that contains many parts that do not have a diamond structure, such as graphite. Therefore, in order to increase the amount of methane while keeping the mixing ratio at 1%, it is necessary to increase the gas pressure in the vacuum chamber, but as a result of experiments, the discharge becomes unstable when the gas pressure is increased, and the discharge exceeds several hundred Torr. It was found that there was no discharge. In addition, conventional forming conditions are easily influenced by substrate temperature and the like, and have poor reproducibility.
問題点を解決するための手段
前記問題点を解決するために本発明は、真空槽内に基体
を設けてプラズマ生成とダイヤモンド形成とを一体化し
て行うとともに、真空槽を空洞共振器状構造にしたもの
である。Means for Solving the Problems In order to solve the above-mentioned problems, the present invention provides a substrate in a vacuum chamber to integrate plasma generation and diamond formation, and also constructs the vacuum chamber into a cavity resonator-like structure. This is what I did.
作 用
本発明は上記した構成によシ、マイクロ波のパワーが効
率的にプラズマに寄与し、真空槽内の反応生成ガスが高
励起されて、そのまま真空槽内の基体に到達するので、
結晶性の良いダイヤモンドを再現性良く形成することが
出来た。Operation The present invention has the above-described configuration, and the power of the microwave efficiently contributes to the plasma, and the reaction product gas in the vacuum chamber is highly excited and reaches the substrate in the vacuum chamber as it is.
Diamonds with good crystallinity could be formed with good reproducibility.
さらにメタンと水素の混合比が１０％以上でも良質のダ
イヤモンドを形成することが出来た。この値は従来に比
べ１桁大きい値であり、混合比を変えてメタンを増やす
ことが出来、メタン律速であったダイヤモンドの形成速
度を高く保つことが出来た。Furthermore, high quality diamonds could be formed even when the mixing ratio of methane and hydrogen was 10% or more. This value is an order of magnitude larger than the conventional value, and it was possible to increase methane by changing the mixing ratio, and it was possible to maintain a high diamond formation rate, which was rate-limiting with methane.
本発明によシ上記問題が完全に解決できることを発見し
た。It has been discovered that the above problems can be completely solved by the present invention.
実施例 以下本発明について実施例とともに説明する。Example The present invention will be explained below along with examples.
第１図に本発明のダイヤモンドを形成するためのプラズ
マ装置の一実施例の概略図である。１１は真空槽、１２
はマイクロ波導波管、１３はマグネトロン、１４はガス
導入部、１５は基体、１６は基体ホルダー、１７は窓で
ある。真空槽１１は内径８５ｊｆｆ、長さ約１３６Ｎで
、円筒空洞型共振器のＴＥ１１１モードが立つような寸
法とした。マイクロ波導入部は、γマイクロ波導波管１
２を介してマグネトロン１３につながっている。マイク
ロ波導波管１２と真空槽１１は、石英ガラスの窓１７で
仕切っである。ガス導入部１４は、反応ガスｑ０と炭素
を含む原料ｑ、とを混合あるいは個別に導入出来るよう
にしである。基体ホルダー１６は、Ｔａ、Ｗ等の補助ヒ
ーターを用いて、基体１５を加熱出来る構造にし、基体
温度については、クロメルマルメル等の熱電対の出力に
応じて、ヒーター電流の制御を行うことで、±１°Ｃ以
内に温度制御を行った。FIG. 1 is a schematic diagram of an embodiment of a plasma apparatus for forming diamond according to the present invention. 11 is a vacuum chamber, 12
13 is a microwave waveguide, 13 is a magnetron, 14 is a gas introduction section, 15 is a substrate, 16 is a substrate holder, and 17 is a window. The vacuum chamber 11 had an inner diameter of 85jff and a length of about 136N, and was dimensioned to allow the TE111 mode of the cylindrical cavity resonator to stand. The microwave introduction section includes a γ microwave waveguide 1
It is connected to the magnetron 13 via 2. The microwave waveguide 12 and the vacuum chamber 11 are separated by a quartz glass window 17. The gas introduction section 14 is configured to allow the reaction gas q0 and the carbon-containing raw material q to be mixed or introduced individually. The substrate holder 16 has a structure that can heat the substrate 15 using an auxiliary heater such as Ta or W, and the substrate temperature is controlled by controlling the heater current according to the output of a thermocouple such as Chromel Marmel. , temperature was controlled within ±1°C.
まず真空槽１１内を油回転ポンプと拡散ポンプを用いて
１０＝ 〜１０−８Ｔｏｘｒ ｉ テ排気しり後、ガス
導入部１４から炭素を含む原料ｑ、を所要の圧力まで導
入した後同じく反応ガスｑ０を導入して、真空槽内を所
要のガス圧に維持した。ガス圧は水銀マノメーターによ
って測定した。ヒーターに電流を流して基体温度の設定
を行い、マイクロ波溝制御を行いながら、真空槽１１内
に設置した基体１６上にダイヤモンドを形成した。First, the inside of the vacuum chamber 11 is evacuated to 10 = ~10-8Toxr i using an oil rotary pump and a diffusion pump, and after that, carbon-containing raw material q is introduced from the gas introduction part 14 to the required pressure, and then the reaction gas q0 is also introduced. was introduced to maintain the required gas pressure inside the vacuum chamber. Gas pressure was measured by a mercury manometer. A current was applied to the heater to set the temperature of the substrate, and diamond was formed on the substrate 16 placed in the vacuum chamber 11 while controlling the microwave groove.
実際には、反応ガスｑ０として水素、炭素を含む原料ｑ
１ としてメタンを用い、メタンの分圧比を１％〜６０
％；ガス圧０．１〜５０ Ｔｏｒｒ 、 ？イクロ波電
力ｓｏＷ 〜ｅｏｏｗ；基体温度６基体温度６塊０
基体には、シリコンウェハーを用い、予め０．１〜１μ
ｍのダイヤモンドペーストで表面の研摩処理を施した後
トリクロロエタンとア七トンで洗浄シたものを使用した
。In reality, raw material q containing hydrogen and carbon as reaction gas q0
Using methane as 1, the partial pressure ratio of methane is 1% to 60.
%; Gas pressure 0.1-50 Torr, ? Microwave power soW ~ eoow; Substrate temperature 6 Substrate temperature 6 lumps 0 A silicon wafer is used as the substrate, and 0.1 to 1μ
The surface was polished with a diamond paste of No. 1, and then washed with trichloroethane and amethane.
このようにして得られたダイヤモンドの走査型電子顕微
鏡写真を第２図に示した。１ｏｏはダイヤモンド結晶を
示す。これらダイヤモンドについてラマン分光分析を行
うと、いずれも１３３３３に半値巾１００１１ 以下
のダイヤモンドとはっきシ同定出来るピークが得られた
。電子線回折でも同様な結果が得られた。またビッカー
ス硬度及び電気抵抗を測定したところ、ビッカース硬度
１００００１１Ｐ／−及び抵抗１０９Ω１以上を確認し
た。成長速度は従来の信販上となった。A scanning electron micrograph of the diamond thus obtained is shown in FIG. 1oo indicates a diamond crystal. When these diamonds were subjected to Raman spectroscopy, a peak at 13333 with a half width of 10011 or less was clearly identified as diamond. Similar results were obtained using electron diffraction. Further, when the Vickers hardness and electrical resistance were measured, it was confirmed that the Vickers hardness was 1000011P/- and the resistance was 109Ω1 or more. The growth rate was higher than that of conventional credit sales.
なお、炭素を含む原料ｑ１ としてはメタンを用いたが
、これに限らず、飽和系または不飽和系炭化水素，芳香
族炭化水素，脂環式炭化水素，多核炭化水素の少くとも
一つを用いることで、高速化が図られる。Although methane was used as the raw material q1 containing carbon, it is not limited to this, and at least one of saturated or unsaturated hydrocarbons, aromatic hydrocarbons, alicyclic hydrocarbons, and polynuclear hydrocarbons may be used. By doing so, the speed can be increased.
真空槽内のガス圧は０，Ｉ Ｔｏｒｒ以上５０Ｔｏｒｒ
以下で良質のダイヤモンドが得られる。０，Ｉ Ｔｏｒ
ｒよシ低いガス圧では、ダイヤモンドはほとんど得られ
ず、５０Ｔｏｒｒを超えると放電が不安定となる。The gas pressure in the vacuum chamber is 0.1 Torr or more and 50 Torr
You can get good quality diamonds below. 0, I Tor
At a gas pressure lower than r, hardly any diamond is obtained, and at a gas pressure exceeding 50 Torr, the discharge becomes unstable.
最適ガス圧は５ Ｔｏｒｒ〜２０Ｔｏｒｒが望ましい。The optimum gas pressure is preferably 5 Torr to 20 Torr.
基体温度は６００°Ｃから１０００°Ｃの範囲で良好な
ダイヤモンドを得た。ｅ ｏ ｏ ”Ｃ未満でも１００
０°Ｃを超えてもダイヤモンドは得られなかった。特に
望ましいのは８００℃±５０″Ｃであることがわかった
。Good diamonds were obtained when the substrate temperature ranged from 600°C to 1000°C. e o o “100 even if it is less than C
Diamonds were not obtained even at temperatures exceeding 0°C. A temperature of 800°C ± 50″C has been found to be particularly desirable.
マイクロ波の出力は４００Ｗ以下が適切で４００Ｗを超
えると基体の損傷が大きくダイヤモンド形成が出来ない
。特に３００Ｗ前後が好ましい。The appropriate microwave output is 400 W or less; if it exceeds 400 W, the substrate will be severely damaged and diamond formation will not be possible. In particular, around 300W is preferable.
炭素を含む原料の混合比は１％〜５０％の範囲で良質の
ダイヤモンドが得られる。１チ未満ではダイヤモンドの
形成はほとんど出来ず、６０％を超えるとグラファイト
等の混入が見られる。Good quality diamonds can be obtained when the mixing ratio of raw materials containing carbon is in the range of 1% to 50%. If it is less than 1%, hardly any diamond can be formed, and if it exceeds 60%, graphite etc. will be mixed in.
マイクロ波導波管と真空槽とは石英ガラスで仕切ったが
、テフロンまたはセラミック等で仕切っても同様にマイ
クロ波を良く透過するとともに真空槽内の排気速度を速
めることが出来る。Although the microwave waveguide and the vacuum chamber were partitioned with quartz glass, partitioning with Teflon, ceramic, or the like would also allow microwaves to pass through the tube well and increase the pumping speed in the vacuum chamber.
反応ガスを基体表面に噴射すると、反応ガスのグラファ
イト等の除去効果が高まりよ多結晶性の良いダイヤモン
ドが得られる。When the reactive gas is injected onto the surface of the substrate, the effectiveness of the reactive gas in removing graphite, etc. increases, and diamond with good polycrystallinity can be obtained.
炭素を含む原料を基体表面に噴射すると、７リツトがな
いので、欠陥の少ないダイヤモンドが得られる。When a raw material containing carbon is injected onto the surface of a substrate, diamonds with fewer defects can be obtained since there are no diamonds.
基体Ｄ、マイクロ波の電界に対して垂直に設置したが反
応生成ガスがマイクロ波の電界で加速されて基体表面に
到達するので緻密なダイヤモンドが得られる。Although the substrate D was placed perpendicular to the microwave electric field, a dense diamond was obtained because the reaction product gas was accelerated by the microwave electric field and reached the substrate surface.
なお、基体をマイクロ波の電界に対し平行に設置しても
良質のダイヤモンドが得られた。これは基体に電界がか
かって発熱し結晶化が促進されるためではないかと考え
られる。Note that even when the substrate was placed parallel to the microwave electric field, high-quality diamonds were obtained. This is thought to be because an electric field is applied to the substrate, which generates heat and promotes crystallization.
また基体を下側を表面に設値すると、真空槽内で発生す
るフリットなどの堆積が少ないダイヤモンドが得られた
。Furthermore, when the lower side of the substrate was placed on the surface, diamonds with less frit and other deposits generated in the vacuum chamber were obtained.
反応ガスまたは炭素を含む原料の導入については、基体
に対し前方から導入したが、これによシ基板表面に集中
的に反応ガスまたは炭素を含む原料を供給することが出
来、反応効率が良い。Regarding the introduction of the raw material containing the reactive gas or carbon, it was introduced from the front of the substrate, but this allows the reactive gas or the raw material containing carbon to be supplied intensively to the surface of the substrate, resulting in good reaction efficiency.
また基体に対し、後方から導入すると、真空槽内に均一
なプラズマを発生させることが出来、良質のダイヤモン
ドが得られる。Furthermore, when introduced from the rear of the substrate, uniform plasma can be generated in the vacuum chamber, and high quality diamond can be obtained.
また基体に対し、側方から導入してもよいが、その際反
応ガスまたは炭素を含む原料の流出方向を基体表面に対
しある角度を持たしてやると、基体表面で粘性流が出来
、基体表面上に均一な分布の少ないダイヤモンドが得ら
れる。角度は５°〜３０’が最も望ましい。The substrate may also be introduced from the side, but if the outflow direction of the reactant gas or carbon-containing raw material is at a certain angle to the substrate surface, a viscous flow will be created on the substrate surface. A less uniform distribution of diamonds is obtained. The most desirable angle is 5° to 30'.
基体１６にはシリコンウエノ・−を用いたが、この場合
界面にＳｉＣが出来て一基体上にダイヤモンドを形成し
やすくなると考えられる。Although silicon urethane was used for the substrate 16, it is thought that in this case, SiC is formed at the interface, making it easier to form diamond on one substrate.
また、反応前に基体表面の研摩処理を行ったが、研摩し
ない基体よシ倍以上の速度でダイヤモンドが形成された
。これは基体表面の傷がダイヤモンドの結晶の核となっ
て結晶成長を高めていると考えられる。Furthermore, although the surface of the substrate was polished before the reaction, diamonds were formed at a rate more than twice that of the substrate that was not polished. This is thought to be because scratches on the substrate surface act as nuclei for diamond crystals, increasing crystal growth.
さらに真空槽に磁界を印加すると、特に低ガス圧領域で
よシ安定した放電が得られた。Furthermore, when a magnetic field was applied to the vacuum chamber, a more stable discharge was obtained, especially in the low gas pressure region.
発明の効果
本発明は、真空槽内に基体を設置してプラズマ生成とダ
イヤモンド形成を一体化して行うとともに、真空槽を空
洞共振器状構造にすることによシ、マイクロ波が効率良
くプラズマに寄与し、よシ膜質の良いダイヤモンドを再
現性良く、高速で形成することが出来、これら産業上の
利用分野に与える効果は極めて大きい。Effects of the Invention The present invention integrates plasma generation and diamond formation by installing a substrate in a vacuum chamber, and also uses a cavity resonator-like structure in the vacuum chamber to efficiently generate plasma using microwaves. This makes it possible to form diamonds with good film quality and good reproducibility at high speed, which has an extremely large effect on these industrial fields of application.
第１図は本発明のダイヤモンドの形成に用いた真（２万
倍）、第３図は従来の装置図である。
１１・・・・・・真空槽、１２・・・・・・マイクロ波
導波管、１３・・・・・・マグネトロン、１４・・・・
・・ガス導入部、１６・・・・・・基体、１６・・・・
・・基体ホルダー、１７・・・・・・窓。
代理人の氏名 弁理士 中 尾 敏 男 ほか１名第１
図
第２図
第３図
Ｈ２十Ｃ）（４
↓
ンプFIG. 1 is a diagram (20,000 times magnified) used to form the diamond of the present invention, and FIG. 3 is a diagram of a conventional apparatus. 11... Vacuum chamber, 12... Microwave waveguide, 13... Magnetron, 14...
...Gas introduction part, 16...Base, 16...
...Base holder, 17...Window. Name of agent: Patent attorney Toshio Nakao and 1 other person No. 1
Figure 2 Figure 3 H20C) (4 ↓
Claims (20)
くとも炭素を含む原料と、マイクロ波とを導入し、マイ
クロ波プラズマを発生させ、得られた反応生成ガスを基
体に到達させてダイヤモンドを形成する方法において、
前記真空槽内に基体を設置するとともに前記真空槽を空
洞共振器状構造にしたことを特徴とするダイヤモンドの
製造方法。(1) At least one type of reaction gas, a raw material containing at least carbon, and microwave are introduced into a vacuum chamber to generate microwave plasma, and the resulting reaction product gas is allowed to reach the substrate to form a diamond. In the method of forming,
A method for producing diamond, characterized in that a substrate is placed in the vacuum chamber, and the vacuum chamber has a cavity resonator-like structure.
１＿１が立つ空洞共振器構造にしたことを特徴とする特
許請求の範囲第１項記載のダイヤモンドの製造方法。(2) Microwave fundamental resonance mode TE_1_ inside the vacuum chamber
1. The method of manufacturing diamond according to claim 1, wherein the diamond has a cavity structure in which 1_1 stands.
請求の範囲第１項記載のダイヤモンドの製造方法。(3) The method for producing diamond according to claim 1, wherein the reactive gas is hydrogen gas.
る特許請求の範囲第１項記載のダイヤモンドの製造方法
。(4) The method for producing diamond according to claim 1, wherein the carbon-containing raw material is a hydrocarbon.
ｒｒ以下にしたことを特徴とする特許請求の範囲第１項
記載のダイヤモンドの製造方法。(5) Increase the gas pressure in the vacuum chamber to 0.1 Torr or more and 50 To
2. The method for manufacturing diamond according to claim 1, wherein the diamond manufacturing method is made to be less than or equal to rr.
イヤモンドを形成することを特徴とする特許請求の範囲
第１項記載のダイヤモンドの製造方法。(6) A method for manufacturing diamond according to claim 1, characterized in that the diamond is formed by keeping the substrate temperature at 600°C to 1000°C.
にしたことを特徴とする特許請求の範囲第１項記載のダ
イヤモンドの製造方法。(7) The diamond manufacturing method according to claim 1, characterized in that the output of the microwave at 2.46 GHz is 400 W or less.
フロンまたはセラミックで仕切ったことを特徴とする特
許請求の範囲第１項記載のダイヤモンドの製造方法。(8) The method for producing diamond according to claim 1, characterized in that the microwave waveguide and the vacuum chamber are partitioned by quartz glass, Teflon, or ceramic.
することを特徴とする特許請求の範囲第１項記載のダイ
ヤモンドの製造方法。(9) The method for producing diamond according to claim 1, characterized in that the partial pressure ratio of the carbon-containing raw material is set to 1% or more and 50% or less.
ことを特徴とする特許請求の範囲第１項記載のダイヤモ
ンドの製造方法。(10) A method for producing diamond according to claim 1, characterized in that a raw material containing carbon is supplied by injection onto the surface of the substrate.
特徴とする特許請求の範囲第１項記載のダイヤモンドの
製造方法。(11) The method for producing diamond according to claim 1, characterized in that the reaction gas is supplied by injection onto the surface of the substrate.
ことを特徴とする特許請求の範囲第１項記載のダイヤモ
ンドの製造方法。(12) The method for producing diamond according to claim 1, wherein the substrate is placed perpendicular to the electric field of the microwave.
ことを特徴とする特許請求の範囲第１項記載のダイヤモ
ンドの製造方法。(13) A method for manufacturing diamond according to claim 1, characterized in that the substrate is placed parallel to the electric field of the microwave.
する特許請求の範囲第１項記載のダイヤモンドの製造方
法。(14) The method for manufacturing diamond according to claim 1, characterized in that the substrate is placed with its surface facing downward.
方から導入することを特徴とする特許請求の範囲第１項
記載のダイヤモンドの製造方法。(15) The method for producing diamond according to claim 1, characterized in that the reactant gas or the raw material containing carbon is introduced into the substrate from the front.
後方から導入することを特徴とする特許請求の範囲第１
項記載のダイヤモンドの製造方法。(16) Claim 1, characterized in that the reactant gas or the raw material containing carbon is introduced from the rear into the substrate.
Method for producing diamonds as described in Section 1.
方から導入し、基体に対して角度を持たせることを特徴
とする特許請求の範囲第１項記載のダイヤモンドの製造
方法。(17) A method for producing diamond according to claim 1, characterized in that the reactant gas or the raw material containing carbon is introduced from the side to the substrate so as to form an angle with the substrate.
求の範囲第１項記載のダイヤモンドの製造方法。(18) The method for producing diamond according to claim 1, wherein the substrate is silicon.
とする特許請求の範囲第１項記載のダイヤモンドの製造
方法。(19) The method for producing diamond according to claim 1, characterized in that the surface of the substrate is subjected to a polishing treatment before the reaction.
請求の範囲第１項記載のダイヤモンドの製造方法。(20) The method for producing diamond according to claim 1, characterized in that a magnetic field is applied to the vacuum chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6934287A JPS63236791A (en) | 1987-03-24 | 1987-03-24 | Production of diamond |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6934287A JPS63236791A (en) | 1987-03-24 | 1987-03-24 | Production of diamond |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63236791A true JPS63236791A (en) | 1988-10-03 |
Family
ID=13399777
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6934287A Pending JPS63236791A (en) | 1987-03-24 | 1987-03-24 | Production of diamond |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63236791A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017521556A (en) * | 2014-06-16 | 2017-08-03 | エレメント シックス テクノロジーズ リミテッド | Microwave plasma reactor for producing synthetic diamond materials |
| CN111511090A (en) * | 2020-04-13 | 2020-08-07 | 北京工业大学 | Microwave plasma reactor |
-
1987
- 1987-03-24 JP JP6934287A patent/JPS63236791A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017521556A (en) * | 2014-06-16 | 2017-08-03 | エレメント シックス テクノロジーズ リミテッド | Microwave plasma reactor for producing synthetic diamond materials |
| JP2019077951A (en) * | 2014-06-16 | 2019-05-23 | エレメント シックス テクノロジーズ リミテッド | Microwave plasma reactor for manufacturing synthetic diamond material |
| US10734198B2 (en) | 2014-06-16 | 2020-08-04 | Element Six Technologies Limited | Microwave plasma reactor for manufacturing synthetic diamond material |
| CN111511090A (en) * | 2020-04-13 | 2020-08-07 | 北京工业大学 | Microwave plasma reactor |
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