JPS6134506B2 - - Google Patents
Info
- Publication number
- JPS6134506B2 JPS6134506B2 JP4571382A JP4571382A JPS6134506B2 JP S6134506 B2 JPS6134506 B2 JP S6134506B2 JP 4571382 A JP4571382 A JP 4571382A JP 4571382 A JP4571382 A JP 4571382A JP S6134506 B2 JPS6134506 B2 JP S6134506B2
- Authority
- JP
- Japan
- Prior art keywords
- cathode
- shielding member
- glow discharge
- cathode body
- treatment apparatus
- 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
- 239000000758 substrate Substances 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000615 nonconductor Substances 0.000 claims 1
- 238000000034 method Methods 0.000 description 11
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 150000002736 metal compounds Chemical class 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000010891 electric arc Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000012993 chemical processing Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
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
- C23C16/50—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 electric discharges
- C23C16/503—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 electric discharges using dc or ac discharges
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
- Chemical Vapour Deposition (AREA)
Description
【発明の詳細な説明】
〔発明の技術分野〕
本発明は、金属、セラミツクス等からなる基体
表面に窒化チタン等の耐摩耗性装飾性に優れた金
属化合物の被膜を形成するために用いるグロー放
電化学処理装置に係わり、特に被膜形成を妨害す
るアーク放電現象の発生を防止したグロー放電化
学処理装置に関する。Detailed Description of the Invention [Technical Field of the Invention] The present invention relates to a glow discharge method used to form a coating of a metal compound such as titanium nitride with excellent wear resistance and decorative properties on the surface of a substrate made of metal, ceramics, etc. The present invention relates to chemical processing equipment, and particularly to a glow discharge chemical processing equipment that prevents the occurrence of arc discharge phenomena that interfere with film formation.
従来より、金属、セラミツクス等からなる基体
表面に、耐摩耗性にすぐれる。たとえば窒化チタ
ン、炭化チタン等の高融点化合物の被膜を形成す
る方法として化学蒸着法が知られている。この方
法では、高融点化合物の被膜の形成が900〜1200
℃で行われるため基体が薄物あるいは細物等の変
形を起こしやすい形状のものが融点の低い材質の
ものでは適用できないという制限があつた。また
得られる被膜の表面状態が粗雑であり、装飾用と
しては不適当であるという欠点があつた。
Conventionally, substrate surfaces made of metals, ceramics, etc. have excellent wear resistance. For example, chemical vapor deposition is known as a method for forming a film of a high melting point compound such as titanium nitride or titanium carbide. In this method, the formation of a film of high melting point compound is 900 to 1200
Since the process is carried out at ℃, there is a limitation that it cannot be applied to thin or thin substrates that are easily deformed or made of materials with a low melting point. Another disadvantage was that the surface of the resulting coating was rough, making it unsuitable for decorative purposes.
このため腕時計等の外側として用いた場合、耐
摩耗性向上と装飾性付与の目的の為に、上述の金
属化合物を被覆する場合にグロー放電空間を基体
近傍に形成させて、放電エネルギーにより、化学
反応を起こさせ、被覆に要するする加熱温度を
400〜600℃と低くして行なうグロー放電化学蒸着
法が検討されている。 For this reason, when used as the outside of a wristwatch, etc., a glow discharge space is formed near the base when coating with the above-mentioned metal compound in order to improve wear resistance and add decorative properties. The heating temperature required to cause the reaction and coating is
A glow discharge chemical vapor deposition method that is carried out at a low temperature of 400 to 600°C is being considered.
この方法を例えば基体表面に金属窒化物を被覆
する場合について第１図を参照して説明すると、
まず初めに真空ポンプに接続された排気口１より
排気して真空容器２内を10-3Torr以下の真空度
まで排気した後、ガス供給口３から金属ハロゲン
化物と窒素と水素との混合ガスを、真空容器２内
が0.1〜10Torrの圧になるよう真空容器２内に導
入する。真空容器２内には、被処理基体４を電気
的に導通した状態で設置しうる陰極体５と陰極体
５の上方に所定の間隔をおいて支持される陽極体
６とが配置されている。この電極間で200〜
8000Vの直流電圧を印加し、かつ陰極体５の裏面
に設けられた加熱板７を加熱して被処理基体を
200〜1000℃，好ましくは400〜60℃にすることに
より、被処理基体近傍にグロー放電空間が形成さ
れ、基体表面で混合ガスが反応して金属窒化物の
被膜が形成される。なお、図中各電極は配線９に
より直流電源１０のしかるべき端子に接続され、
陽極側はアース１１により接地されている。 This method will be explained with reference to FIG. 1 for the case where the surface of the substrate is coated with metal nitride, for example.
First, the inside of the vacuum container 2 is evacuated to a degree of vacuum of 10 -3 Torr or less by evacuating through the exhaust port 1 connected to the vacuum pump, and then a mixed gas of metal halide, nitrogen, and hydrogen is supplied from the gas supply port 3. is introduced into the vacuum container 2 so that the pressure inside the vacuum container 2 is 0.1 to 10 Torr. Disposed within the vacuum container 2 are a cathode body 5 that can be placed in electrical continuity with the substrate 4 to be processed, and an anode body 6 supported at a predetermined distance above the cathode body 5. . 200~ between this electrode
The substrate to be processed is heated by applying a DC voltage of 8000 V and heating the heating plate 7 provided on the back surface of the cathode body 5.
By heating the temperature to 200 to 1000°C, preferably 400 to 60°C, a glow discharge space is formed near the substrate to be processed, and the mixed gas reacts on the surface of the substrate to form a metal nitride film. In addition, each electrode in the figure is connected to the appropriate terminal of the DC power supply 10 by wiring 9,
The anode side is grounded by earth 11.
しかしながら、この方法においては、陰極体５
の陽極側に形成されるグローが、陰極の縁部を越
えて陰極導入部材８側に延びてきて矢印に示すよ
うに真空容器２の底部（陽極）にまで達し、この
部分で主放電が生じるようになり、遂にはアーク
放電へと移行して基体表面の被膜形成が妨害され
るという問題があつた。 However, in this method, the cathode body 5
The glow formed on the anode side extends beyond the edge of the cathode to the cathode introduction member 8 side, reaching the bottom (anode) of the vacuum container 2 as shown by the arrow, and a main discharge occurs in this part. There was a problem in that the process eventually shifted to arc discharge and the formation of a film on the surface of the substrate was obstructed.
本発明は上述の問題を解消するもので、陰極導
入部材８表面への金属化合物被膜の形成を防止し
て、アーク放電現象の発生を防いだグロー放電化
学処理装置を提供することを目的とする。
The present invention solves the above-mentioned problems, and aims to provide a glow discharge chemical treatment device that prevents the formation of a metal compound film on the surface of the cathode introduction member 8 and prevents the occurrence of arc discharge phenomena. .
すなわ本発明は、真空容器２内の陰極体５の端
縁の外周もしくは陰極導入部材８との接合部にキ
グローが侵入しない間隙Ａを形成するための遮蔽
部材１２を設けたことを特徴とする。
That is, the present invention is characterized in that a shielding member 12 is provided at the outer periphery of the edge of the cathode body 5 in the vacuum container 2 or at the joint with the cathode introduction member 8 to form a gap A in which Kiglow does not enter. do.
本発明に使用する遮蔽部材は、石英等の絶縁物
で形成されるのが適切であるが、導体表面に絶縁
被覆を形成させたものも用いることができる。 The shielding member used in the present invention is suitably made of an insulating material such as quartz, but it is also possible to use a shielding member with an insulating coating formed on the surface of the conductor.
以下図面を参照して本発明装置の詳細を説明す
る。なお以下の図において第一図と共通する部分
は同一符号で示す。 The details of the apparatus of the present invention will be explained below with reference to the drawings. In the following figures, parts common to those in Figure 1 are designated by the same reference numerals.
第２図は陰極体５端縁の外周に間隙Ａが形成さ
れるよう円筒状の遮蔽部材１２が陰極体５を包囲
するよう配置した実施例である。遮蔽部材１２と
陰極体５との間隙Ａは１〜３mmが適切であり、遮
蔽部材１２の高さは陰極体５とほぼ同じかそれよ
り高いのが好ましい。 FIG. 2 shows an embodiment in which a cylindrical shielding member 12 is arranged to surround the cathode body 5 so that a gap A is formed around the outer periphery of the cathode body 5. FIG. The gap A between the shielding member 12 and the cathode body 5 is suitably 1 to 3 mm, and the height of the shielding member 12 is preferably approximately the same as or higher than the cathode body 5.
第３図は陰極体５と陰極導入部材８との接合部
にグローの侵入しない間隙Ａが形成されるよう笠
状遮蔽部材１２の基部が接合部にくるよう配置さ
れるように構成された例である。この笠状遮蔽部
材は加熱板の下に断熱板１３を設け、それを介し
て配置されるのが好ましい。また笠状遮蔽部材の
傾斜角度は20〜30゜が適切であり、大きさは陰極
体より大きいことが望ましい。 FIG. 3 shows an example in which the base of the shade-shaped shielding member 12 is arranged so as to be located at the joint between the cathode body 5 and the cathode introduction member 8 so that a gap A is formed in which no glow enters. It is. It is preferable that this shade-shaped shielding member is disposed via a heat insulating plate 13 provided below the heating plate. Further, the inclination angle of the shade-shaped shielding member is suitably 20 to 30°, and the size is preferably larger than the cathode body.
また、上述の笠状遮蔽部材の代りに第４図のよ
うに傾斜のない円盤状の遮蔽部材を陰極導入部材
に周設させることもも可能である。 Further, instead of the above-mentioned cap-shaped shielding member, it is also possible to provide a disc-shaped shielding member with no slope around the cathode introducing member as shown in FIG.
このように構成された本発明装置においては、
間隙Ａの形成によりグロー放電は陰極導入部材ま
で達することがなく遮蔽部材上を延びるが、陰極
体と電気的に導通しないためアーク放電現象を防
止することができる。 In the device of the present invention configured in this way,
Due to the formation of the gap A, the glow discharge does not reach the cathode introduction member and extends over the shielding member, but since it is not electrically conductive with the cathode body, arc discharge phenomenon can be prevented.
次に実施例について説明する。 Next, an example will be described.
実施例
第３図に示すような笠状遮蔽部材をその基部が
陰極体と陰極導入部材との接合部にくるよう断熱
板の下方に配置した処理装置を使用し、Cr38
％，Al3.8％，Ni残の組成の合金からなる25mm×
25mm×４mmの金属板を被処理基体として陰極体に
載置し、次の条件で処理を行なつたところ、陰極
導入部材表面にはTiNの被膜は形成されず反応が
スムーズに行えた。得られた基体上のTiN被膜は
均一で光択があり、装飾性に優れていた。Example A processing device was used in which a shade-shaped shielding member as shown in Fig. 3 was placed below a heat insulating plate so that its base was located at the joint between the cathode body and the cathode introducing member.
%, Al3.8%, Ni balance 25mm×
A 25 mm x 4 mm metal plate was placed on the cathode body as a substrate to be treated, and the treatment was carried out under the following conditions. No TiN film was formed on the surface of the cathode introducing member, and the reaction was carried out smoothly. The obtained TiN coating on the substrate was uniform, photo-selective, and had excellent decorative properties.
反応ガス組成 Ticl4：H2：N2
＝１：19：６（モル比）
圧 力 2Torr
電 圧 500V
電流密度 0.1mA／cm
基体の温度 550℃
処理時間 30分
一方、遮蔽部材を配置しない処理装置を使用し
あとは実施例と同様に処理を行なつたところ、途
中でTiN被膜が基体上に形成されず、陰極導入部
材表面の上部からどんどん下方に向かつて形成さ
れたので処理を中止した。 Reaction gas composition Ticl 4 :H 2 :N 2 = 1:19:6 (molar ratio) Pressure 2Torr Voltage 500V Current density 0.1mA/cm Substrate temperature 550℃ Treatment time 30 minutes On the other hand, treatment without placing a shielding member When the apparatus was used and the rest of the process was carried out in the same manner as in the example, the TiN film was not formed on the substrate during the process, but was formed from the top of the surface of the cathode introducing member downwards, so the process was stopped. .
以上の実施例からも明らかなように、本発明装
置によれば陰極導入部材表面へ金属化合物の被膜
が形成されることがないから、アーク放電現象が
発生するおそれがなく、基体表面上への金属化合
物被膜の形成がスムーズに行える。
As is clear from the above examples, according to the apparatus of the present invention, a metal compound film is not formed on the surface of the cathode introduction member, so there is no risk of arc discharge occurring, and no metal compound film is formed on the surface of the substrate. Metal compound coating can be formed smoothly.
第１図は従来の処理装置を模式的に示す概略断
面図、第２図及至第４図は本発明の処理装置の概
略断面図である。
２……真空容器、４……被処理基体、５……陰
極体、６……陽極板、７……加熱板、８……陰極
導入部材、１２……遮蔽部材。
FIG. 1 is a schematic sectional view schematically showing a conventional processing apparatus, and FIGS. 2 to 4 are schematic sectional views of the processing apparatus of the present invention. 2... Vacuum vessel, 4... Substrate to be processed, 5... Cathode body, 6... Anode plate, 7... Heat plate, 8... Cathode introduction member, 12... Shielding member.
Claims (1)
陰極導入部材により前記真空容器の底部から間隔
をおいて支持された被処理基体を載置する陰極体
と、この陰極体と陰極導入部材との間に設けたグ
ローを遮蔽する遮蔽部材と、前記陰極体を加熱す
る加熱装置と、前記陰極体と対向して設置された
陽極を具備することを特徴とするグロー放電化学
処理装置。 ２ 遮蔽部材が、陰極体を包囲する円筒状部材で
ある特許請求の範囲第１項記載のグロー放電化学
処理装置。 ３ 遮蔽部材が、基部を陰極体と陰極導入部材と
の接合部に位置させた笠状部材である特許請求の
範囲第１項記載のグロー放電化学処理装置。 ４ 遮蔽部材が、陰極導入部材に周設された円筒
状部材である特許請求の範囲第１項記載のグロー
放電化学処理装置。 ５ 遮蔽部材の表面が、電気絶縁体で構成されて
なる特許請求の範囲第１項記載のグロー放電化学
処理装置。 ６ 遮蔽部材が石英である特許請求の範囲第１項
記載のグロー放電化学処理装置。[Claims] 1. A vacuum container equipped with a gas supply port and an exhaust port;
a cathode body on which a substrate to be processed is placed and supported by a cathode introduction member at a distance from the bottom of the vacuum container; a shielding member provided between the cathode body and the cathode introduction member for shielding glow; A glow discharge chemical treatment apparatus comprising: a heating device that heats a cathode body; and an anode placed opposite the cathode body. 2. The glow discharge chemical treatment apparatus according to claim 1, wherein the shielding member is a cylindrical member surrounding the cathode body. 3. The glow discharge chemical treatment apparatus according to claim 1, wherein the shielding member is a shade-shaped member having a base located at a joint between the cathode body and the cathode introduction member. 4. The glow discharge chemical treatment apparatus according to claim 1, wherein the shielding member is a cylindrical member provided around the cathode introduction member. 5. The glow discharge chemical treatment apparatus according to claim 1, wherein the surface of the shielding member is made of an electrical insulator. 6. The glow discharge chemical treatment apparatus according to claim 1, wherein the shielding member is made of quartz.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4571382A JPS58164776A (en) | 1982-03-24 | 1982-03-24 | Chemical treatment device by glow discharge |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4571382A JPS58164776A (en) | 1982-03-24 | 1982-03-24 | Chemical treatment device by glow discharge |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58164776A JPS58164776A (en) | 1983-09-29 |
| JPS6134506B2 true JPS6134506B2 (en) | 1986-08-08 |
Family
ID=12726986
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4571382A Granted JPS58164776A (en) | 1982-03-24 | 1982-03-24 | Chemical treatment device by glow discharge |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58164776A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0581328B2 (en) * | 1987-06-29 | 1993-11-12 | Tsubakimoto Chain Co |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61187375U (en) * | 1985-05-15 | 1986-11-21 |
-
1982
- 1982-03-24 JP JP4571382A patent/JPS58164776A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0581328B2 (en) * | 1987-06-29 | 1993-11-12 | Tsubakimoto Chain Co |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS58164776A (en) | 1983-09-29 |
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