JPH0135799B2 - - Google Patents
Info
- Publication number
- JPH0135799B2 JPH0135799B2 JP58236564A JP23656483A JPH0135799B2 JP H0135799 B2 JPH0135799 B2 JP H0135799B2 JP 58236564 A JP58236564 A JP 58236564A JP 23656483 A JP23656483 A JP 23656483A JP H0135799 B2 JPH0135799 B2 JP H0135799B2
- Authority
- JP
- Japan
- Prior art keywords
- diamond
- vapor phase
- gun
- phase synthesis
- plasma
- 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
Links
- 239000010432 diamond Substances 0.000 claims description 27
- 229910003460 diamond Inorganic materials 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 16
- 230000015572 biosynthetic process Effects 0.000 claims description 11
- 239000000758 substrate Substances 0.000 claims description 11
- 238000003786 synthesis reaction Methods 0.000 claims description 11
- 239000012808 vapor phase Substances 0.000 claims description 10
- 229930195733 hydrocarbon Natural products 0.000 claims description 9
- 150000002430 hydrocarbons Chemical class 0.000 claims description 9
- 239000004215 Carbon black (E152) Substances 0.000 claims description 7
- 238000010884 ion-beam technique Methods 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 238000010894 electron beam technology Methods 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims 1
- 238000001308 synthesis method Methods 0.000 claims 1
- 239000010408 film Substances 0.000 description 13
- 229910052799 carbon Inorganic materials 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 239000007789 gas Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 5
- 238000000151 deposition Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- YZCKVEUIGOORGS-UHFFFAOYSA-N Hydrogen atom Chemical compound [H] YZCKVEUIGOORGS-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- -1 carbon ions Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】
(イ) 技術分野
本発明は気相合成法によるダイヤモンド薄膜の
製造法に関するものである。[Detailed Description of the Invention] (a) Technical Field The present invention relates to a method for producing a diamond thin film by vapor phase synthesis.
(ロ) 技術の背景
ダイヤモンド又はダイヤモンドと凝似の特性を
示すカーボンの気相合成法として世人に確かな方
法として認められているものには下記の２大別さ
れる方法がある。(b) Background of the technology There are two general methods that are recognized as reliable methods for the vapor phase synthesis of diamond or carbon that exhibits properties similar to those of diamond.
CVD法：メタン等の炭化水素ガスに水素ガ
スを混じて、この混合ガスを加熱及び又はガス
放電を利用して分解し、やはり加熱された基材
の表面に、SP3結合を有するカーボンを選択的
に蒸着させ、粒子状又は膜状のダイヤモンドを
気相合成する方法。 CVD method: Hydrocarbon gas such as methane is mixed with hydrogen gas, and this mixed gas is decomposed using heating and/or gas discharge. Carbon having SP3 bonds is selectively deposited on the surface of the heated base material. A method of vapor phase synthesis of particulate or film diamond by vapor deposition.
PVD法：所謂イオンビーム蒸着法を用い、
カーボンをArイオンでスパツターし、スパツ
ターされたカーボンとArイオンを磁場内でプ
ラズマ励起し、その后カーボンイオンを選択的
に電界印加引出しを行い、加速を与えた状態で
高真空雰囲気に置かれた基材にタタキつける状
態にてダイヤモンドと凝似の特性を有するカー
ボン膜の蒸着を行う方法。 PVD method: Using the so-called ion beam evaporation method,
Carbon was sputtered with Ar ions, the sputtered carbon and Ar ions were plasma excited in a magnetic field, and then the carbon ions were selectively drawn out by applying an electric field, and placed in a high vacuum atmosphere while being accelerated. A method of vapor-depositing a carbon film that has properties similar to diamond by tapping it onto a base material.
これ等の方法は夫々に短所がある。 Each of these methods has its own shortcomings.
例えば前者の方法はダイヤモンド合成の原料と
なるカーボンを供給する炭化水素ガスを水素にて
100倍近くに希釈せねばならず、従つて大面積の
薄膜形成の為には多量の水素を消費せねばならな
いこと、また基材を加熱することが前提となつて
いるため、融点の低いものには蒸着させることが
出来ない問題を有している。 For example, in the former method, hydrogen is used to replace hydrocarbon gas that supplies carbon, which is the raw material for diamond synthesis.
It must be diluted nearly 100 times, and therefore a large amount of hydrogen must be consumed to form a thin film over a large area, and the base material must be heated, so it has a low melting point. has the problem that it cannot be vapor deposited.
また後者の方法は硬質で絶縁性が大きい膜の形
成が可能となるが、その特性は飽く迄凝似ダイヤ
モンドであり硬度もHV＝5000（Kg／mm2）程度で
あり、密度も天然ダイヤモンドの70％前后と低
く、結晶性も悪く、アモルフアス状の部分が大勢
を占め、従つて熱伝導率や電子移動度なども天然
ダイヤ−ａ型に比べて相当小さい。 In addition, the latter method makes it possible to form a film that is hard and has high insulating properties, but its characteristics are that of condensed diamond, with a hardness of approximately HV=5000 (Kg/mm 2 ) and a density of 70% that of natural diamond. %, the crystallinity is poor, the amorphous portion predominates, and the thermal conductivity and electron mobility are considerably lower than that of natural diamond type A.
(ハ) 発明の開示
本発明は上記の問題を解決する為のもので、上
記のCVD法とPVD法が夫々に有する欠点を解消
したものである。即ち、ダイヤモンドを気相合成
する方法において、原料の炭化水素ガスを冷陰極
または熱陰極PIG型ガン、もしくは電子振動式ガ
ン等のイオンガンで分解せしめ、さらにガンの中
で磁界等によりプラズマ励起させ、該プラズマに
電界を印加し、加速して高真空の蒸着室にビーム
状態で引き出し、同室に設置された熱電子放射銃
により電子照射された引き出されたビームを加熱
された基材に当ててダイヤモンドを合成すること
を特徴とするダイヤモンドの気相合成法を提供す
るものである。加熱された基材は最高1000℃まで
の範囲で制御可能である。また基材にはバイアス
電圧として3KVまで印加可能である。また蒸着
室に設置された熱電子放射銃はＷフイラメントま
たはLaB6フイラメントであることが望ましい。(C) Disclosure of the Invention The present invention is intended to solve the above-mentioned problems, and eliminates the drawbacks of the above-mentioned CVD method and PVD method. That is, in a method for vapor phase synthesis of diamond, hydrocarbon gas as a raw material is decomposed with an ion gun such as a cold cathode or hot cathode PIG type gun, or an electronic vibration type gun, and then plasma is excited in the gun by a magnetic field or the like. An electric field is applied to the plasma, the plasma is accelerated and drawn out in a beam state into a high vacuum deposition chamber, and the drawn beam, which is irradiated with electrons by a thermionic emission gun installed in the same chamber, is applied to a heated substrate to form diamonds. The present invention provides a method for vapor phase synthesis of diamond, which is characterized by synthesizing diamond. The heated substrate can be controlled up to 1000°C. Furthermore, it is possible to apply up to 3KV as a bias voltage to the base material. Further, the thermionic radiation gun installed in the deposition chamber is preferably a W filament or a LaB 6 filament.
イオンビームの加速電圧は5KV以下ではカー
ボン膜しか得られず、3KV以上ではスパツタリ
ングが起つて堆積しない。又基板は５×
10-4Torr以下の高真空度室に設置しないとイオ
ンビームが基板に到達する以前にガス分子と衝突
してエネルギーを損失する確率が高くなる。 If the ion beam acceleration voltage is less than 5KV, only a carbon film will be obtained, and if it is more than 3KV, sputtering will occur and no deposition will occur. Also, the board is 5x
If the ion beam is not installed in a high vacuum chamber below 10 -4 Torr, there is a high probability that the ion beam will collide with gas molecules and lose energy before reaching the substrate.
本発明の特徴は、カーボン原子の発生を炭化水
素ガスもしくは少量のアルゴンと混ぜた炭化水素
ガスの直流放電により達成し、ガンの中に設けら
れた磁界等によりプラズマ励起し、更にこの際に
発生した解離炭化水素、水素、炭素を高真空室へ
導き熱電子放射フイラメントより放出される電子
により原子状水素に10％以上の比率で解離させ、
その結果として炭素の原子結合はSP3を示し硬
度、密度共に天然或いは超高圧合成で得られるダ
イヤモンドと有意差のない蒸着膜が得られる方法
を提供するものである。 A feature of the present invention is that carbon atoms are generated by direct current discharge of hydrocarbon gas or hydrocarbon gas mixed with a small amount of argon, plasma is excited by a magnetic field provided in a gun, and carbon atoms are generated at this time. The dissociated hydrocarbons, hydrogen, and carbon are introduced into a high vacuum chamber and dissociated into atomic hydrogen at a ratio of 10% or more by the electrons emitted from the thermionic filament.
As a result, the atomic bond of carbon exhibits SP 3 , and a method is provided in which a deposited film is obtained that has no significant difference in hardness and density from diamond obtained by natural or ultra-high pressure synthesis.
本方法は多段にわたるプラズマの励起により蒸
着層がSP3結合を有するダイヤモンドを気相合成
する方法を提供するものであるが、さらに本願の
別の特徴は基板の温度を最高1000℃まで加熱する
ことによつて、無定形結晶状から結晶性の良い状
態までの巾広い特性のダイヤモンドを大面積の基
材に均一につけることに適している。さらには低
温に保持した基板にもダイヤコート出来ることに
特徴がある。このことは炭化水素のプラズマが高
いレベルに励起されている結果可能となるもので
ある。 This method provides a method for vapor phase synthesis of diamond in which the deposited layer has SP 3 bonds by excitation of plasma in multiple stages, and another feature of the present application is that the temperature of the substrate is heated to a maximum of 1000°C. Accordingly, it is suitable for uniformly applying diamonds with a wide range of characteristics, from amorphous crystalline to well-crystalline states, to a large area of a base material. Another feature is that it can be coated with diamond even on substrates kept at low temperatures. This is possible as a result of the high level of excitation of the hydrocarbon plasma.
かくの如くして得られたダイヤモンドは例えば
耐摩、耐蝕等のための表面処理、また光学系、半
導体、IC、LSI等の分野で使用することができ
る。 The diamond thus obtained can be used, for example, in surface treatments for wear resistance, corrosion resistance, etc., and in fields such as optical systems, semiconductors, ICs, and LSIs.
(ニ) 実施例
第１図に示す冷陰極PIG型ガンを装着した装置
を用いて、下記の条件でシリコン基板上に8000Å
の蒸着膜を得た。その条件としては、原料ガスと
してCH4を用い、冷陰極PIGガンに導入する。
50Vに印加した直流放電でこのCH4ガスをプラズ
マ分解し200Gの外部磁場でこのプラズマの励起
を強化し、1KVの引き出し電圧で引出した。蒸
着室は１×10-4Torrとなつており、ここに、700
℃に加熱した基板を設置した。イオンビームと基
板の間に第１図の如くＷフイラメント１からの電
子ビームが当るようにした。この時Ｗフイラメン
トの温度は2150℃であつた。(D) Example Using a device equipped with a cold cathode PIG type gun shown in Figure 1, a film of 8000 Å was deposited on a silicon substrate under the following conditions.
A deposited film was obtained. The conditions are that CH 4 is used as the source gas and introduced into a cold cathode PIG gun.
This CH 4 gas was plasma decomposed by a DC discharge applied to 50V, the excitation of this plasma was strengthened by an external magnetic field of 200G, and it was extracted with an extraction voltage of 1KV. The deposition chamber has a pressure of 1 × 10 -4 Torr, where 700
A substrate heated to ℃ was installed. An electron beam from a W filament 1 was made to strike between the ion beam and the substrate as shown in FIG. At this time, the temperature of the W filament was 2150°C.
得られた膜は電子線回折によりダイヤモンド構
造でその格子定数は3.568Åと天然ダイヤモンド
と近いものであつた。又、ラマン分光法によつて
1330cm-1付近にダイヤモンドの特徴的なスペクト
ルが観察された。 The obtained film was found to have a diamond structure by electron beam diffraction, and its lattice constant was 3.568 Å, which is close to that of natural diamond. Also, by Raman spectroscopy
A characteristic spectrum of diamond was observed near 1330 cm -1 .
比較例として、Ｗフイラメントからの電子照射
をなくした場合、電子線回折では何の回折線も見
られず、ラマン分光法によつては1550cm-1や1400
cm-1のダイヤモンド状炭素膜の特徴を示すピーク
が見られた。 As a comparative example, when the electron irradiation from the W filament was eliminated, no diffraction lines were observed in electron diffraction, and Raman spectroscopy showed only 1550 cm -1 or 1400 cm -1.
A peak characteristic of a diamond-like carbon film at cm -1 was observed.
なお本発明の方法で得た膜が３×1011Ωcmの電
気抵抗であつたのに対し比較例は２×107Ωcmと
低抵抗であつた。更に、第１図の冷陰極PIG型ガ
ンの代りに、熱陰極PIG型ガン又は電子振動式ガ
ンを装着した装置を用いて、前記同様の条件でシ
リコン基板上に蒸着膜を生成させ、得られた膜を
電子線回折で観察したところ、ダイヤモンドの構
造を示す回折線が得られ、ダイヤモンド膜である
ことが確認された。 The film obtained by the method of the present invention had an electrical resistance of 3×10 11 Ωcm, whereas the comparative example had a low resistance of 2×10 7 Ωcm. Further, in place of the cold cathode PIG type gun shown in Fig. 1, a device equipped with a hot cathode PIG type gun or an electronic vibration type gun was used to generate a vapor deposited film on a silicon substrate under the same conditions as described above. When the film was observed by electron diffraction, diffraction lines showing the structure of diamond were obtained, confirming that it was a diamond film.
第１図は本願発明で用いられたダイヤモンドの
気相合成装置を示す。
１……Ｗフイラメント、２……イオン源、３…
…基板、４……CH4導入口、５……排気口。
FIG. 1 shows a diamond vapor phase synthesis apparatus used in the present invention. 1... W filament, 2... ion source, 3...
... Board, 4... CH 4 inlet, 5... Exhaust port.
Claims (1)
炭化水素ガスを主原料とし、50V〜3KVの印加電
圧で加速したイオンビームを、５×10-4Torr以
下の真空度に保つた高真空室に設置され加熱され
た基板に衝突以前、もしくは衝突と同時に熱電子
放射銃からの電子ビームを照射することを特徴と
し、かつ、該イオン源が熱陰極または冷陰極PIG
型ガンもしくは電子振動式ガンであり、直流プラ
ズマで炭化水素を分解せしめ、このプラズマに磁
界を与えることによつて分解したイオンやラジカ
ルを一層励起することを特徴とするダイヤモンド
の気相合成法。 ２ 該基板を300℃以上1000℃までの範囲で加熱
することを特徴とする特許請求の範囲第１項記載
のダイヤモンドの気相合成法。[Claims] 1. In a method for vapor phase synthesis of diamond,
The ion beam, which is mainly made of hydrocarbon gas and accelerated with an applied voltage of 50 V to 3 KV, is placed in a high vacuum chamber maintained at a vacuum level of 5 × 10 -4 Torr or less and hits a heated substrate before or after impact. It is characterized by simultaneously irradiating an electron beam from a thermionic emission gun, and the ion source is a hot cathode or a cold cathode PIG.
A diamond vapor phase synthesis method that uses a type gun or an electronic vibration gun to decompose hydrocarbons using direct current plasma, and further excites the decomposed ions and radicals by applying a magnetic field to this plasma. 2. The method for vapor phase synthesis of diamond according to claim 1, characterized in that the substrate is heated in a range of 300°C to 1000°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58236564A JPS60127299A (en) | 1983-12-14 | 1983-12-14 | Diamond vapor phase synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58236564A JPS60127299A (en) | 1983-12-14 | 1983-12-14 | Diamond vapor phase synthesis method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60127299A JPS60127299A (en) | 1985-07-06 |
| JPH0135799B2 true JPH0135799B2 (en) | 1989-07-27 |
Family
ID=17002502
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58236564A Granted JPS60127299A (en) | 1983-12-14 | 1983-12-14 | Diamond vapor phase synthesis method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60127299A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6433096A (en) * | 1987-04-03 | 1989-02-02 | Fujitsu Ltd | Gaseous phase synthesis for diamond |
| US4981568A (en) * | 1988-09-20 | 1991-01-01 | International Business Machines Corp. | Apparatus and method for producing high purity diamond films at low temperatures |
| DE202008006069U1 (en) * | 2008-03-10 | 2008-07-17 | Becker Marine Systems Gmbh & Co. Kg | Device for reducing the power requirement of a ship |
-
1983
- 1983-12-14 JP JP58236564A patent/JPS60127299A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60127299A (en) | 1985-07-06 |
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