JPH01147067A - Formation of head carbon film - Google Patents
Formation of head carbon filmInfo
- Publication number
- JPH01147067A JPH01147067A JP30381187A JP30381187A JPH01147067A JP H01147067 A JPH01147067 A JP H01147067A JP 30381187 A JP30381187 A JP 30381187A JP 30381187 A JP30381187 A JP 30381187A JP H01147067 A JPH01147067 A JP H01147067A
- Authority
- JP
- Japan
- Prior art keywords
- film
- carbon film
- hard carbon
- plasma
- silicon
- 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title description 5
- 229910052799 carbon Inorganic materials 0.000 title description 5
- 230000015572 biosynthetic process Effects 0.000 title description 2
- 238000005268 plasma chemical vapour deposition Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 14
- 229910021385 hard carbon Inorganic materials 0.000 claims abstract description 13
- 239000010703 silicon Substances 0.000 claims abstract description 13
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 4
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 4
- 150000003377 silicon compounds Chemical class 0.000 claims abstract description 3
- 239000011651 chromium Substances 0.000 claims description 17
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 11
- 229910052804 chromium Inorganic materials 0.000 claims description 11
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 11
- 239000000758 substrate Substances 0.000 claims description 7
- 150000002291 germanium compounds Chemical class 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 14
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 3
- 230000008016 vaporization Effects 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 abstract 2
- 230000001070 adhesive effect Effects 0.000 abstract 2
- 239000007789 gas Substances 0.000 description 9
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- -1 cyclopentadienyl metal compound Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Landscapes
- Chemical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は各種基材の表面及び内壁に、プラズマ−ＣＶＤ
法によりカーボン硬質膜を３次元的に被覆形成するため
のクロムを主体とする中間層の形成法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention provides plasma-CVD coating on the surfaces and inner walls of various base materials.
The present invention relates to a method for forming an intermediate layer mainly composed of chromium for three-dimensionally coating a carbon hard film by a method.
ガラス、プラスチック、−ステンレスなど各種基材へ直
接カーボン硬質膜を被覆形成することは困難で、密着不
良から剥離が生ずる。このため、基材とカーボン硬質膜
との規着を取ることをねらい、クロムを主体とする下層
とシリコンまたはゲルマニウムからなる２層構造の中間
層を導入することが提案されている。（特願昭６０−２
５６４２６号）。クロムを主体とする下層の形成方法と
して。It is difficult to directly coat various base materials such as glass, plastic, and stainless steel with a carbon hard film, and peeling occurs due to poor adhesion. For this reason, it has been proposed to introduce an intermediate layer with a two-layer structure consisting of a lower layer mainly composed of chromium and a silicon or germanium layer, with the aim of improving the adhesion between the base material and the carbon hard film. (Special application 1986-2
No. 56426). As a method of forming a lower layer mainly composed of chromium.
イオンビーム蒸着法、スパッタリング法、イオンブレー
ティング法、真空蒸着法などの物理的（ＰＶＤ）法があ
る。シリコンまたはゲルマニウムを主体とする上層の形
成手法としては上記手法の他にも、プラズマ−ＣＶＤ法
がある。このプラズマ−ＣＶＤ法によるシリコンまたは
ゲルマニウムを主体とする中間層の形成法は公知であり
、内部が中空となっている基材（例えば、ノズル、ダイ
ス、シリンダー、パイプなど）の場合でも内壁への被覆
形成が可能である。しカルクロムを主体とする層の形成
法はＰ Ｖ’Ｄ法であり、プラズマ−ＣＶＤ法が確立し
ていないため、基材の砲壁に対してまわり込みに劣りク
ロム層が形成できない。そこでこのような基材に対して
は、シリコンまたはゲルマニウムを主体とする中間層だ
けを形成し、カーボン硬質膜を形成する手法を用いてい
た。There are physical (PVD) methods such as ion beam evaporation, sputtering, ion blating, and vacuum evaporation. In addition to the above-mentioned method, there is a plasma-CVD method as a method for forming the upper layer mainly made of silicon or germanium. This plasma-CVD method for forming an intermediate layer mainly made of silicon or germanium is well-known, and even in the case of hollow substrates (e.g., nozzles, dies, cylinders, pipes, etc.), it is possible to form an intermediate layer on the inner wall. Coating formation is possible. The method for forming a layer mainly composed of calchromium is the PV'D method, and since the plasma-CVD method has not been established, it is difficult to form a chromium layer on the gun wall of the base material due to poor wrapping. Therefore, for such base materials, a method has been used in which only an intermediate layer mainly made of silicon or germanium is formed to form a hard carbon film.
しかし基材とシリコンまたはゲルマニウムを主体とする
中間層の密着性が悪い場合や、基材とシリコンまたはゲ
ルマニウムが（相互あるいは一方からの）拡散により合
金あるいは金属間化合物を形成する場合など基材にシリ
コンまたはゲルマニウムを主体とする中間層を形成でき
ない場合には、カーボン硬質膜が形成できなかった。However, if the adhesion between the base material and an intermediate layer mainly composed of silicon or germanium is poor, or if the base material and silicon or germanium form an alloy or intermetallic compound due to diffusion (from each other or from one side), If an intermediate layer mainly made of silicon or germanium could not be formed, a hard carbon film could not be formed.
本発明の目的は、内部に中空状態を有する基材の表面及
び内壁などにカーボン硬質膜を密着性良く被覆すること
である。An object of the present invention is to coat the surface and inner wall of a substrate having a hollow interior with a carbon hard film with good adhesion.
上記目的のため、本発明においては基材をカソード電位
と同レベルに保ち、プラズマ−ＣＶＤ法により（Ｃ５’
Ｈ！１ ）２ Ｃｒを昇華させ気化したガス雰囲気中
でクロムを主体とする下層を形成し、さらにシリコン化
合物またはゲルマニウム化合物を含むガス雰囲気中でシ
リコンまたはゲルマニウムを主体とする上層を形成し、
次に炭化水素ガスを含むガス雰囲気中でカーボン硬質膜
を形成するようにした。For the above purpose, in the present invention, the substrate is kept at the same level as the cathode potential, and the plasma-CVD method (C5'
H! 1) Forming a lower layer mainly composed of chromium in a gas atmosphere in which 2 Cr is sublimated and vaporized, and further forming an upper layer mainly composed of silicon or germanium in a gas atmosphere containing a silicon compound or germanium compound,
Next, a hard carbon film was formed in a gas atmosphere containing hydrocarbon gas.
常温ではクロムを含むガスがほとんど存在しないため、
クロムを含む固体や液体、例えば、ＣｒＭ２．ＣｒＭ３
．ＣｒＭ、、Ｃｒｙ、Ｍ２、（ＭはＦＳＣｌ％Ｂｒなど
のハロゲン）や、Ｃｒｙｓ 、Ｃｒ２Ｏ５、Ｃｒ （Ｃ
Ｏ）ａなどを気化させてＣＶＤ反応を起こす技術が提案
されている。しかしこれらの物質は人体に有害であるた
め、取り扱いに注意を要するなどの問題点も多く、まだ
−膜化していない。Because there are almost no gases containing chromium at room temperature,
Solids and liquids containing chromium, such as CrM2. CrM3
．． CrM, Cry, M2, (M is halogen such as FSCl%Br), Crys, Cr2O5, Cr (C
A technique has been proposed in which a CVD reaction is caused by vaporizing O)a and the like. However, since these substances are harmful to the human body, there are many problems such as the need to handle them with care, and they have not yet been formed into a film.
本発明ではＣｒを含む化合物中では、人体に無害で常温
の固体の（Ｃｓ Ｈ５）２ Ｃ’を昇華させ気化させた
ものを生成源とし、プラズマ−ＣＶＤ法によるクロム膜
形成法を確立した。In the present invention, among compounds containing Cr, we have established a method for forming a chromium film by plasma-CVD using sublimated and vaporized (Cs H5) 2 C', which is a solid at room temperature and is harmless to the human body, as a generation source.
以下に本発明の実施例を図面に基づいて説明する。Embodiments of the present invention will be described below based on the drawings.
第１図はカーボン硬質膜を形成するプラズマ−ＣＶＤ装
置の一例である。FIG. 1 shows an example of a plasma-CVD apparatus for forming a hard carbon film.
金属からなる真空槽１内には、マツチングボックスを介
して高周波電源と電気的に結合されているカソード電極
２が配置され、真空槽１は接地電位を保っておりアノー
ド電極として機能するような装置構成である。A cathode electrode 2 electrically connected to a high frequency power source via a matching box is arranged inside a vacuum chamber 1 made of metal, and the vacuum chamber 1 maintains a ground potential and functions as an anode electrode. This is the device configuration.
基材６はカソード電極２から吊してもよいし、カソード
電極２上に置いてもよい。図面中では基材３は１つしか
示されていないが、多数の基材をカソード電極２から吊
してもよいし、置いてもよく、個数の制約はない。真空
槽１内を真空排気した後、ガス導入口４より（ＣａＨａ
）ｚｃｒ を昇華させて気化したガスを０．ＩＴｏｒｒ
導入し１３、５６ ＭＨｚの高周波電力を５００Ｗ程度
印加μプラズマーＣＶＤ法によりＣｒを主体とする膜を
厚さ約０．５μｍ形成する。次いでＳｉＨ４をガス導入
口４より０．ＩＴｏｒｒ導入し、１３．５６ ＭＨｚの
高周波電力を３００Ｗ程度印加し、プラズマ−ＣＶＤ法
によりシリコンを主体とする膜を膜厚約０．５μｍ形成
する。この場合ＳｉＨ４のがわりに、Ｓ １２Ｈａ 、
Ｓ ｉ、Ｈａ 、Ｓ ｉＦ４．５ｉ）（２ｃ１２、Ｓ
１Ｈｃｌ８．Ｓ ｉｃｌ、、Ｓ １２Ｃ１２、Ｓ １２
Ｃ１６、Ｓ ｒ Ｈｓ Ｆ、 Ｇｅ）（、、ＧｅＣｌ
＜などを用いてシリコンあるいはゲルマニウムを形成し
てもよい。このようにして形成した２層構造の中間層は
基材とカーボン硬質膜の間の密着強度を向上させるうえ
で重要である。The base material 6 may be suspended from the cathode electrode 2 or may be placed on the cathode electrode 2. Although only one base material 3 is shown in the drawing, a large number of base materials may be hung from the cathode electrode 2 or may be placed thereon, and there is no restriction on the number of base materials. After evacuating the vacuum chamber 1, the gas inlet 4 (CaHa
)zcr sublimed and vaporized gas to 0. ITorr
A film mainly composed of Cr is formed to a thickness of about 0.5 μm by applying high frequency power of about 500 W at 13 and 56 MHz by μ plasma-CVD method. Next, SiH4 was introduced into the gas inlet 4 at 0.00%. ITorr is introduced, a high frequency power of 13.56 MHz is applied to about 300 W, and a film mainly composed of silicon is formed to a thickness of about 0.5 μm by plasma-CVD. In this case, instead of SiH4, S 12Ha,
S i, Ha , S iF4.5i) (2c12, S
1Hcl8. S icl,, S 12C12, S 12
C16, S r Hs F, Ge) (,, GeCl
<< etc. may be used to form silicon or germanium. The intermediate layer having the two-layer structure thus formed is important for improving the adhesion strength between the base material and the hard carbon film.
次に炭化水素を含むガス、例えばＣＨ，を０． ＩＴｏ
ｒｒ導入し、１３．５６ ＭＨｚの高周波電力を３００
Ｗ程度印加し、プラズマ−ＣＶＤ法によりカーボン硬質
膜を形成させる。ＣＨ，のかゎりにＣ２Ｈ６、Ｃ５Ｈｓ
、Ｃ４ＨＩＯ％Ｃ２Ｈ４、Ｃ５Ｈａ、Ｃｔ Ｈ２、Ｃ
４Ｈ６を用いてもよい。Next, a gas containing a hydrocarbon, for example CH, is added to 0. ITo
rr was introduced and 13.56 MHz high frequency power was applied to 300 MHz.
Approximately W is applied to form a hard carbon film by plasma-CVD. CH、C2H6、C5Hs
,C4HIO%C2H4,C5Ha,Ct H2,C
4H6 may also be used.
本発明ではＣｒを含む化合物中では人体にほとんど無害
である（Ｃ５Ｈ５）２Ｃ’ をＣＶＤ反応の生成源に
選んだ。シクロペンタジェニル金属化合物である（Ｃｓ
Ｈａ）２Ｃｒ はプラズマで励起させることにより、容
易に（ｃａＨｓ） とＣｒの結合が切れ、クロム膜が
得られるという利点がある。内部に中空状態な有しシリ
コンまたはゲルマニウムと密着が悪かった基材の内壁に
も、プラズマ−ＣＶＤ法を採用したことによりクロム膜
が形成できるようになり、カーボン硬質膜の被覆形成が
可能となった。In the present invention, (C5H5)2C', which is almost harmless to the human body among Cr-containing compounds, was selected as the generation source for the CVD reaction. It is a cyclopentadienyl metal compound (Cs
Ha)2Cr has the advantage that by exciting it with plasma, the bond between (caHs) and Cr can be easily broken and a chromium film can be obtained. By adopting the plasma-CVD method, it is now possible to form a chromium film on the inner wall of a substrate that is hollow and has poor adhesion to silicon or germanium, making it possible to form a hard carbon film coating. Ta.
第１図は本発明の実施例における基材の表面や内部に中
空を有する基材の内壁に、カーボン硬質膜を被覆形成す
るための装置を示す模式図である。
１・・・・・・真空槽、
２・・・・・・カソード電極、
第１＠FIG. 1 is a schematic diagram showing an apparatus for coating the surface of a substrate and the inner wall of a substrate having a hollow interior with a hard carbon film in an embodiment of the present invention. 1... Vacuum chamber, 2... Cathode electrode, 1st @
Claims (1)
り、内部に中空状態を有する多数の基材を接地電位にあ
る金属製の真空槽内に配置し、（Ｃ＿５Ｈ＿５）＿２Ｃ
ｒを昇華させ気化させたガス雰囲気中で、プラズマ−Ｃ
ＶＤ法によりクロムを主体とする層を形成し、次にシリ
コン化合物またはゲルマニウム化合物を含むガス雰囲気
中で、プラズマ−ＣＶＤ法によりシリコンまたはゲルマ
ニウムを主体とする層を形成し、しかるのちに、これら
の２層構造からなる中間層上に炭化水素を含むガス雰囲
気中で、プラズマ−ＣＶＤ法によりカーボン硬質膜を被
覆形成することを特徴とするカーボン硬質膜の被覆方法
。A large number of substrates, which are held in electrical connection with the cathode electrode and have a hollow state inside, are placed in a metal vacuum chamber at ground potential, and (C_5H_5)_2C
Plasma-C in a gas atmosphere in which r is sublimed and vaporized.
A layer mainly composed of chromium is formed by a VD method, and then a layer mainly composed of silicon or germanium is formed by a plasma-CVD method in a gas atmosphere containing a silicon compound or germanium compound. A method for coating a hard carbon film, which comprises forming a hard carbon film on an intermediate layer having a two-layer structure by a plasma-CVD method in a gas atmosphere containing hydrocarbons.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30381187A JPH01147067A (en) | 1987-12-01 | 1987-12-01 | Formation of head carbon film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30381187A JPH01147067A (en) | 1987-12-01 | 1987-12-01 | Formation of head carbon film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01147067A true JPH01147067A (en) | 1989-06-08 |
Family
ID=17925587
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30381187A Pending JPH01147067A (en) | 1987-12-01 | 1987-12-01 | Formation of head carbon film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01147067A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5425983A (en) * | 1992-08-10 | 1995-06-20 | Santa Barbara Research Center | Infrared window protected by multilayer antireflective coating |
| US5455081A (en) * | 1990-09-25 | 1995-10-03 | Nippon Steel Corporation | Process for coating diamond-like carbon film and coated thin strip |
| US5527596A (en) * | 1990-09-27 | 1996-06-18 | Diamonex, Incorporated | Abrasion wear resistant coated substrate product |
| US5593719A (en) * | 1994-03-29 | 1997-01-14 | Southwest Research Institute | Treatments to reduce frictional wear between components made of ultra-high molecular weight polyethylene and metal alloys |
| US5605714A (en) * | 1994-03-29 | 1997-02-25 | Southwest Research Institute | Treatments to reduce thrombogeneticity in heart valves made from titanium and its alloys |
| US5637353A (en) * | 1990-09-27 | 1997-06-10 | Monsanto Company | Abrasion wear resistant coated substrate product |
| US5643423A (en) * | 1990-09-27 | 1997-07-01 | Monsanto Company | Method for producing an abrasion resistant coated substrate product |
| US5725573A (en) * | 1994-03-29 | 1998-03-10 | Southwest Research Institute | Medical implants made of metal alloys bearing cohesive diamond like carbon coatings |
| US5731045A (en) * | 1996-01-26 | 1998-03-24 | Southwest Research Institute | Application of diamond-like carbon coatings to cobalt-cemented tungsten carbide components |
| US5780119A (en) * | 1996-03-20 | 1998-07-14 | Southwest Research Institute | Treatments to reduce friction and wear on metal alloy components |
-
1987
- 1987-12-01 JP JP30381187A patent/JPH01147067A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5455081A (en) * | 1990-09-25 | 1995-10-03 | Nippon Steel Corporation | Process for coating diamond-like carbon film and coated thin strip |
| US5527596A (en) * | 1990-09-27 | 1996-06-18 | Diamonex, Incorporated | Abrasion wear resistant coated substrate product |
| US5635245A (en) * | 1990-09-27 | 1997-06-03 | Monsanto Company | Process of making abrasion wear resistant coated substrate product |
| US5637353A (en) * | 1990-09-27 | 1997-06-10 | Monsanto Company | Abrasion wear resistant coated substrate product |
| US5643423A (en) * | 1990-09-27 | 1997-07-01 | Monsanto Company | Method for producing an abrasion resistant coated substrate product |
| US5844225A (en) * | 1990-09-27 | 1998-12-01 | Monsanto Company | Abrasion wear resistant coated substrate product |
| US5425983A (en) * | 1992-08-10 | 1995-06-20 | Santa Barbara Research Center | Infrared window protected by multilayer antireflective coating |
| US5593719A (en) * | 1994-03-29 | 1997-01-14 | Southwest Research Institute | Treatments to reduce frictional wear between components made of ultra-high molecular weight polyethylene and metal alloys |
| US5605714A (en) * | 1994-03-29 | 1997-02-25 | Southwest Research Institute | Treatments to reduce thrombogeneticity in heart valves made from titanium and its alloys |
| US5725573A (en) * | 1994-03-29 | 1998-03-10 | Southwest Research Institute | Medical implants made of metal alloys bearing cohesive diamond like carbon coatings |
| US5731045A (en) * | 1996-01-26 | 1998-03-24 | Southwest Research Institute | Application of diamond-like carbon coatings to cobalt-cemented tungsten carbide components |
| US5780119A (en) * | 1996-03-20 | 1998-07-14 | Southwest Research Institute | Treatments to reduce friction and wear on metal alloy components |
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