JPH01275498A - Production of diamond film - Google Patents
Production of diamond filmInfo
- Publication number
- JPH01275498A JPH01275498A JP10189888A JP10189888A JPH01275498A JP H01275498 A JPH01275498 A JP H01275498A JP 10189888 A JP10189888 A JP 10189888A JP 10189888 A JP10189888 A JP 10189888A JP H01275498 A JPH01275498 A JP H01275498A
- Authority
- JP
- Japan
- Prior art keywords
- substrate
- diamond film
- thermionic
- temperature
- hydrogen
- 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 26
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000000463 material Substances 0.000 claims abstract description 44
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 7
- 230000005284 excitation Effects 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- 229930195733 hydrocarbon Natural products 0.000 abstract description 4
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000007858 starting material Substances 0.000 abstract 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000005520 cutting process Methods 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 229910052715 tantalum Inorganic materials 0.000 description 4
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- JFIOVJDNOJYLKP-UHFFFAOYSA-N bithionol Chemical compound OC1=C(Cl)C=C(Cl)C=C1SC1=CC(Cl)=CC(Cl)=C1O JFIOVJDNOJYLKP-UHFFFAOYSA-N 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
この発明は硬度、熱伝導率、耐腐食性に非常にすぐれた
特性を有し、切削工具や放熱基板として有効であるダイ
ヤモンドを気相合成法にて基板上に析出させるダイヤモ
ンド膜の製造方法の改良に関するものである。[Detailed Description of the Invention] <Industrial Application Field> This invention utilizes vapor phase synthesis of diamond, which has excellent properties in hardness, thermal conductivity, and corrosion resistance, and is effective as a cutting tool and heat dissipation substrate. This invention relates to an improvement in a method for producing a diamond film deposited on a substrate by a method.
〈従来の技術〉
従来、ダイヤモンドの合成方法としては炭化水素と水素
との混合ガスを熱電子放射材により加熱した後、５００
〜１３００℃に加熱した基板表面に導入して基材上にダ
イヤモンドを析出せしめる技術が特開昭５８−９１１０
０号により知られている。<Conventional technology> Conventionally, the method of synthesizing diamond is to heat a mixed gas of hydrocarbon and hydrogen with a thermionic emitter, and then
Japanese Patent Laid-Open No. 58-9110 describes a technique for depositing diamond on the substrate surface heated to ~1300°C.
Known by No. 0.
〈発明が解決しようとする課題〉
上記した公知技術においては、基材と熱電子放射材の距
離は１０ｍｍ程度であるため（即ち、この距離が１ｏｎ
＋ｍをこえると成膜速度が極度に低下する）、熱電子放
射材の温度は２１００℃までしか上げることができない
という問題があった。なぜならば、熱電子放射材の温度
を２１００℃以上に上げると、基材温度が上りすぎてダ
イヤモンド析出温度（５００〜１３００℃）から外れて
しまい、ダイヤモンドが成膜しなくなる。従って、熱電
子放射材の温度は２１００℃以下に抑えなければならな
いが、その際原料源である炭化水素および水素の活性を
促進するには原料ガスの加熱が充分とはいえず、ダイヤ
モンドと同時に無定形炭素やグラファイトが生成すると
いう問題がある。<Problem to be solved by the invention> In the above-mentioned known technology, since the distance between the base material and the thermionic emitting material is about 10 mm (that is, this distance is 1 on
(If the temperature exceeds +m, the film formation rate is extremely reduced), and the temperature of the thermionic emitting material can only be raised to 2100°C. This is because if the temperature of the thermionic emission material is raised to 2100° C. or higher, the base material temperature rises too much and deviates from the diamond precipitation temperature (500 to 1300° C.), making it impossible to form a diamond film. Therefore, the temperature of the thermionic emissive material must be kept below 2100°C, but the heating of the raw material gas is not sufficient to promote the activity of the hydrocarbons and hydrogen that are the raw material sources, There is a problem that amorphous carbon and graphite are generated.
く課題を解決するための手段〉
本発明者らは上記従来のダイヤモンド合成方法における
問題を解消することができるダイヤモンド膜の製造方法
を得るべく検討の結果この発明に至ったものである。Means for Solving the Problems> The present inventors have arrived at the present invention as a result of their studies to obtain a method for manufacturing a diamond film that can solve the problems in the conventional diamond synthesis methods described above.
即ち、この発明は炭化水素化合物および水素を２３００
℃以上の高温に加熱した熱電子放射材を通過せしめ、基
材上にダイヤモンド膜を析出せしめる際に、熱電子放射
材と基材の間隔を３０１Ｔ１ｍ以上とすることを特徴と
するダイヤモンド膜の製造方法を提供するものである。That is, this invention can convert hydrocarbon compounds and hydrogen into 2300
Production of a diamond film, characterized in that the distance between the thermionic emissive material and the base material is 301 T1 m or more when the thermionic emissive material heated to a high temperature of ℃ or higher is passed through and the diamond film is deposited on the base material. The present invention provides a method.
く作用〉
従来の熱電子放射材を使用したダイヤモンド膜の製造方
法においては、上述したように基材と熱電子放射材との
距離は１０１１ｍ以下と短かく、また熱電子放射材の温
度は２１００℃までしかあげることはできない。この温
度を２１００℃以上に上げると、基材温度が１３００℃
以上になり、その場合にはダイヤモンドは析出しなくな
る。In the conventional method for producing a diamond film using a thermionic emitter, the distance between the base material and the thermionic emitter is as short as 1011 m or less, and the temperature of the thermionic emitter is 2100 m or less, as described above. It can only be raised up to ℃. When this temperature is increased to 2100°C or higher, the base material temperature increases to 1300°C.
In this case, diamond will no longer precipitate.
これに対してこの発明では熱電子放射材と基板との距離
を３０１１ｍ以上離すことにより、熱電子放射材の温度
を２３００℃以上にすることができるのである。On the other hand, in the present invention, the temperature of the thermionic emitter can be increased to 2,300° C. or more by separating the thermionic emitter and the substrate at a distance of 3,011 m or more.
また、２３００℃以上に熱電子放射材の温度を上げるこ
とにより、高活性な炭素種を生成することができ、基材
上により結晶度の高いダイヤモンド膜を析出させること
ができるのである。Furthermore, by raising the temperature of the thermionic emitter to 2300° C. or higher, highly active carbon species can be generated, and a diamond film with higher crystallinity can be deposited on the substrate.
この発明で２３００℃以上の高温に耐えられる熱電子放
射材の材質としては炭素フィラメント、タンタルフィラ
メントが好ましい。In this invention, carbon filaments and tantalum filaments are preferable as materials for the thermionic radiation material that can withstand high temperatures of 2300° C. or higher.
炭化水素化合物としてはメタン、エタンなどの炭化水素
やメチルアルコール、アセトンなどのアルコール、ケト
ン類が挙げられる。また水素にはアルゴン等の不活性ガ
スを加えてもよい。Examples of hydrocarbon compounds include hydrocarbons such as methane and ethane, alcohols such as methyl alcohol and acetone, and ketones. Further, an inert gas such as argon may be added to hydrogen.
炭化水素化合物と水素の流量比は炭化水素化合物／水素
＝１１５〜１／１０００が好ましく、この比が１１５以
下ではグラファイトの析出が問題であり、１／１０００
以上では成膜速度が小さすぎて好ましくない。The flow rate ratio of hydrocarbon compound and hydrogen is preferably hydrocarbon compound/hydrogen = 115 to 1/1000. If this ratio is less than 115, precipitation of graphite becomes a problem, and 1/1000
Above this value, the film formation rate is too low, which is not preferable.
基材温度は８００℃以下では無定形炭素を生じ、１３０
０℃以上ではダイヤモンドが析出しないので８００〜１
３００℃の範囲が適当である。When the substrate temperature is below 800°C, amorphous carbon is formed, and 130
Diamonds do not precipitate at temperatures above 0°C, so the temperature is 800-1.
A range of 300°C is suitable.
次にこの発明の方法を実施するに使用する装置の一例を
第１図に示した。同図において、１は反応室であり、該
反応室１内には基材２、基材支持台３および熱電子放射
材４が内蔵されている。５は炭化水素化合物供給装置、
６は水素供給装置であって夫々から所要量がバイブ７に
より反応室１へ供給される。８は熱電子放射材用加熱電
源であって、これによって反応室１内の熱電子放射材４
の温度がコントロールされる。９は排気装置、１０は排
気口である。Next, an example of the apparatus used to carry out the method of this invention is shown in FIG. In the figure, 1 is a reaction chamber, and the reaction chamber 1 contains a base material 2, a base material support 3, and a thermionic radiation material 4. 5 is a hydrocarbon compound supply device;
Reference numeral 6 denotes a hydrogen supply device, from which the required amount is supplied to the reaction chamber 1 via a vibrator 7. Reference numeral 8 denotes a heating power source for the thermionic emitting material, which heats the thermionic emitting material 4 in the reaction chamber 1.
temperature is controlled. 9 is an exhaust device, and 10 is an exhaust port.
〈実施例〉 以下、実施例によりこの発明の詳細な説明する。<Example> Hereinafter, this invention will be explained in detail with reference to Examples.
実施例１
第１図に示すダイヤモンド膜作製装置を用い、基材２と
して市を使用した。原料としてメタン、水素を夫々１ｃ
ｃ／ｎｉｎ、 １００ｃｃ／ｌｉｎ反応室１に供給し
た。Example 1 The diamond film production apparatus shown in FIG. 1 was used, and diamond was used as the base material 2. 1 c each of methane and hydrogen as raw materials
c/nin, 100 cc/lin was supplied to the reaction chamber 1.
熱電子放射材４としてタンタルフィラメントを使用し、
その温度を２４００℃、フィラメントと基材間の距離を
３５＋ｎｍとし、基材温度８７０℃、反応室内の圧力を
２０Ｔｏｒｒに調整して４時間の成膜を行なった。A tantalum filament is used as the thermionic radiation material 4,
Film formation was carried out for 4 hours at a temperature of 2400° C., a distance between the filament and the substrate of 35+ nm, a substrate temperature of 870° C., and a pressure in the reaction chamber of 20 Torr.
その結果、基材２上に５μｍ厚の炭素膜を析出した。こ
の膜の評価方法として（ａ−Ｋｃｔ、線によるＸ線回折
を行なったところ、２θ＝４３．９°付近に鋭いピーク
を検出し、この膜がダイヤモンド膜であると同定できた
。As a result, a 5 μm thick carbon film was deposited on the base material 2. As a method for evaluating this film, (a-Kct) X-ray diffraction was performed, and a sharp peak was detected near 2θ=43.9°, and this film was identified as a diamond film.
実施例２
第１図の装置を使用し、エタノールと水素を原料として
使用した。そして水素を２００ｃｃ／ ｎｉｎ １エタ
ノールを１０ ｖｏ１％（ｉｎＨ２）反応室内に供給し
た。Example 2 The apparatus shown in FIG. 1 was used, and ethanol and hydrogen were used as raw materials. Then, 200 cc/nin of hydrogen and 10 vol 1% (inH2) of ethanol were supplied into the reaction chamber.
熱電子放射材としてタンタルフィラメントを使用し、そ
の温度を２４４０℃とした。基材としてＣ−８，を使用
し、基材とフィラメント間の距離を４（Ｌｎｍ、基材温
度８５０℃、圧力１０Ｔｏｒｒで８時間の成膜を行なっ
た。A tantalum filament was used as the thermionic emitting material, and its temperature was set at 2440°C. C-8 was used as the base material, and the film was formed for 8 hours at a distance between the base material and the filament of 4 (L nm), a base material temperature of 850° C., and a pressure of 10 Torr.
その結果、１０μ汎の炭素膜を得た。As a result, a 10μ wide carbon film was obtained.
得られた膜の評価方法としてレーダーラーマン分光法を
使用したところ、１３３３ｃｘ１−１付近に鋭いピーク
を検出し、ダイヤモンド膜と同定できた。When radar Raman spectroscopy was used to evaluate the obtained film, a sharp peak was detected near 1333cx1-1, and it was identified as a diamond film.
実施例３
第１図の装置を使用し、原料どしてメタン、水素を夫々
１ｃｃ／ｌｉｎ 、 ２００ｃｃ／ｉｉｎ供給した。Example 3 Using the apparatus shown in FIG. 1, methane and hydrogen were supplied as raw materials at a rate of 1 cc/lin and 200 cc/iin, respectively.
熱電子放射材としてタンタルフィラメントを使用し、そ
の温度を２４２０℃とした。またフィラメントと基材間
の距離は１５ｍｍとし、基材としては−を使用した。そ
して基材温度１０００℃、２５Ｔｏｒｒの圧力で３時間
の成膜を行なった。A tantalum filament was used as the thermionic emitting material, and its temperature was set at 2420°C. Further, the distance between the filament and the base material was 15 mm, and - was used as the base material. Then, film formation was performed for 3 hours at a substrate temperature of 1000° C. and a pressure of 25 Torr.
その結果、膜厚２μ汎の炭素膜を析出した。この炭素膜
をラマン分光法にて調べたところ、１３７０α−１およ
び１５１０■−１付近に緩やかなピークを検出し、グラ
フ１イト膜であると同定できた。As a result, a carbon film with a thickness of about 2 μm was deposited. When this carbon film was examined by Raman spectroscopy, gentle peaks were detected near 1370α-1 and 1510■-1, and it was identified as a graphite film.
以上実施例１乃至３によって得た炭素膜を切削工具に被
覆して切削テストを行なった。A cutting test was conducted by coating cutting tools with the carbon films obtained in Examples 1 to 3 above.
被覆層厚は何れも４μｍとし、切削チップとしては５Ｎ
ＨＮ １２０４０８を使用した。The coating layer thickness was 4μm in both cases, and the cutting tip was 5N.
HN 120408 was used.
また比較としてＣＶＤ法を用いて〃２０．コーティング
を行なったチップおよびコーティング無しのチップを使
用した。In addition, for comparison, using the CVD method, 20. Coated and uncoated chips were used.
その結果は第１表に示した。The results are shown in Table 1.
なお、切削条件′は次の通りである。Note that the cutting conditions' are as follows.
被剛材 ＡＣ８Ａ−Ｔ６ （１２％ＳＬ −＃合金）切
削速度 ８００ｍ ／１ａｉｎ
送 リ ０．１ｍｍ／ｒｅＶ切り込
み ０．２ｍｍ
第 １ 表
上表からこの発明の方法による実施例１および２がすぐ
れていることが認められた。Rigid material AC8A-T6 (12%SL-# alloy) Cutting speed 800m/1ain Feed 0.1mm/reV depth of cut 0.2mm From the table above, Examples 1 and 2 using the method of this invention are superior. This was recognized.
また、実施例１の方法で得られるダイヤモンド膜を被覆
した耐摩工具およびＴ、Ｃコーティングを行なったもの
、コーティング無しのものによって被剛材 １８ＳＬ
−＃合金
チップ ５ＥＧＮ １２０３０４
切削速度 １２００ｍ ／１ａｉｎ乾式％式％
の切削条件でアルミニウム合金旋削における耐摩耗特性
を調べたところ第２図に示す結果が得られ、この発明の
方法によるものは非常にすぐれた耐摩耗性を示すことが
認められた。In addition, a wear-resistant tool coated with a diamond film obtained by the method of Example 1, a tool with T and C coatings, and a tool without coating were used to improve the rigidity of the 18SL material.
-#Alloy tip 5EGN 120304 Cutting speed: 1200m/1ain Dry type % We investigated the wear resistance properties in aluminum alloy turning under the cutting conditions of It was observed that the material exhibited excellent abrasion resistance.
・ 第１図はこの発明の方法を実施するに使用する装置
の１例を示す態様図、第２図は耐摩耗特性を示す線図で
ある。
１・・・反応室 ２・・・基材３・・・
基材支持台 ４・・・熱電子放射材５・・・
炭化水素化合物供給装置
６・・・水素供給装置 ７・・・バイブ８・・
・熱電子放射材用加熱電源
９・・・排気装置１０・・・排気口
出願人代理人 弁理士 和 １） 昭逃１ｆ面
摩耗量Ｖｓ（ｍｍ）- Fig. 1 is a diagram showing an example of an apparatus used to carry out the method of the present invention, and Fig. 2 is a diagram showing wear resistance characteristics. 1... Reaction chamber 2... Base material 3...
Base material support stand 4... Thermionic emission material 5...
Hydrocarbon compound supply device 6...Hydrogen supply device 7...Vibe 8...
・Heating power source for thermionic radiation material 9...Exhaust device 10...Exhaust port applicant's agent Patent attorney Kazu 1) Showa 1f surface wear amount Vs (mm)
Claims (2)
上に加熱した熱電子放射材を通過させて加熱励起するこ
とにより基板上にダイヤモンドを生成するダイヤモンド
膜の製造に際し、前記熱電子放射材と基板との間隔を３
０ｍｍ以上としたことを特徴とするダイヤモンド膜の製
造方法。(1) When manufacturing a diamond film in which diamond is produced on a substrate by passing a thermionic emitting material heated to 2300° C. or higher through the raw material hydrocarbon compound and hydrogen and excitation by heating, the above-mentioned thermionic emitting material and the substrate are heated and excited. The distance between
A method for producing a diamond film, characterized in that the thickness is 0 mm or more.
５〜１／１０００であることを特徴とする請求項（１）
記載のダイヤモンド膜の製造方法。(2) The flow rate ratio of the raw material hydrocarbon compound and hydrogen is 1/
Claim (1) characterized in that the ratio is 5 to 1/1000.
A method of manufacturing the described diamond film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10189888A JPH01275498A (en) | 1988-04-25 | 1988-04-25 | Production of diamond film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10189888A JPH01275498A (en) | 1988-04-25 | 1988-04-25 | Production of diamond film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01275498A true JPH01275498A (en) | 1989-11-06 |
Family
ID=14312738
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10189888A Pending JPH01275498A (en) | 1988-04-25 | 1988-04-25 | Production of diamond film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01275498A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006056744A (en) * | 2004-08-19 | 2006-03-02 | Tokyo Univ Of Agriculture & Technology | Diamond synthesis method and device |
-
1988
- 1988-04-25 JP JP10189888A patent/JPH01275498A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006056744A (en) * | 2004-08-19 | 2006-03-02 | Tokyo Univ Of Agriculture & Technology | Diamond synthesis method and device |
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