CN107502868A - A kind of high, high resistant W doping CN films preparation method - Google Patents
A kind of high, high resistant W doping CN films preparation method Download PDFInfo
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- CN107502868A CN107502868A CN201710795449.5A CN201710795449A CN107502868A CN 107502868 A CN107502868 A CN 107502868A CN 201710795449 A CN201710795449 A CN 201710795449A CN 107502868 A CN107502868 A CN 107502868A
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- films
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- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
- C23C14/0658—Carbon nitride
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of high, high resistant W doping CN films preparation method, comprise the following steps：1）From the high glass thoroughly of ultrawhite as backing material, and ultrasonic wave cleaning is carried out, reach the purpose for removing substrate surface greasy dirt and dust；2）Backing material after cleaning is placed on specimen holder, is sent into sputtering chamber, is passed through Ar gas, makes C target build-ups of luminance, carries out pre-sputtering to remove the oxide on surface and impurity, pre-sputtering finishes, and is passed through N2Gas, first layer CN films are prepared on backing material by the reaction with C targets, disconnect N2Gas, specimen holder turn to W targets, the sputtering of W targets build-up of luminance, plated film, layer of metal W films are prepared on first layer CN films, and the technique for then repeating above-mentioned first layer CN films carries out the preparation of second of CN film, and high saturating, high resistant W doping CN films are obtained after the completion of plated film.Present invention process parameter is simple, and variable element is less, reproducible, and W incorporation further increases the lubricity of CN films, the application field of CN films is further expanded.
Description
Technical field
The present invention relates to the preparation and application field of film, is mainly used in liquid crystal display, hand-set lid field, particularly one
Kind is high thoroughly, the preparation method of high resistant W doping CN films.
Background technology
Liu in 1989 etc. is foretold first, can carry out the not existing compound of artificial synthesized nature --- carbonitride, tool
There are larger polymerization energy and mechanical stability.Then Teter etc. speculates to the structure of carbonitride, and more research shows, its
In the bulk modulus theoretical value of a type of carbonitride can be comparable with diamond, it is considered to be it is a kind of new superhard
Material, while can have the extraordinary physics such as very high resistivity, high transmittance by the change of processing performance, carbonitride
And optical property, and by W doping, the WC with favorable lubricating property on the one hand can be formed in CN films, can be further
Improve the premium properties such as the elasticity of film, abrasion, coefficient of friction.It will be obtained extensively in fields such as hand-set lid, FPD
General application.
The content of the invention
It is an object of the invention to provide a kind of preparation method of high, high resistant W doping CN films, by the doping of W elements,
The lubricity of CN films is can further improve, reduces abrasion.High saturating, high resistant CN films transmitance is had a certain upgrade simultaneously
Effect.
The purpose of the present invention is achieved by the following technical programs, a kind of high, high resistant W doping CN films system
Preparation Method, comprise the following steps：
1）From the high glass thoroughly of ultrawhite as backing material, ultrasonic wave cleaning is carried out to backing material, reaches removal substrate surface
The purpose of greasy dirt and dust；
2）Backing material after cleaning is placed on specimen holder, is sent into sputtering chamber, is opened equipment, is vacuumized, in vacuum
Reach 1.0 × 10-4When, Ar gas is passed through, makes C target build-ups of luminance, carries out pre-sputtering to remove the oxide on surface and impurity, pre-sputtering is complete
Finish, be passed through N2Gas, first layer CN films are prepared on backing material by the reaction with C targets, disconnect N2Gas, specimen holder turn to W
Target, the sputtering of W targets build-up of luminance, plated film, layer of metal W films are prepared on first layer CN films, it is thin then to repeat above-mentioned first layer CN
The technique of film carries out the preparation of second of CN film, and high saturating, high resistant W doping CN films are obtained after the completion of plated film.
The present invention also has following technical characteristic：
The independent build-up of luminance of the target of W, C two in whole coating process, avoids cross pollution.
The C target power outputs for preparing CN films are 50 ~ 300W；Ar flows are 10-30sccm；N2Flow is 1-7sccm；Work
Air pressure is maintained at 0.2 ~ 2.0Pa, sputtering time 30-60s.
The W target power outputs for preparing W films are 50-200w；Ar flows are 10-30sccm, air pressure 0.2-0.5Pa；During plated film
Between be 5-10s.
Beneficial effects of the present invention：
1）C, the targets of W two are all to carry out single sputter coating, reduce cross pollution；
2）C, the target technological parameters of W two are simple, and each target can be controlled individually, reproducible, workable；
3）By the technological parameter and N that change the target of W, C two2Amount, various high performance W doping CN films can be prepared；
4）It is CN-W-CN that the body structure surface of its film layer, which is seen, but W is not simply to pile up in actual coating process, but can be oozed
It thoroughly into CN films, or even can be reacted with C unnecessary in film, reach the effect of real doping.
Embodiment
With reference to specific experiment process, the present invention is described in further detail.
Embodiment 1：Using high purity graphite and high pure metal tungsten as experiment target, while the use of the high glass thoroughly of ultrawhite is substrate material
Material.It is first according to conventional method and ultrasonic wave cleaning is carried out to backing material, cleaning, which finishes, to be put it into magnetron sputtering chamber, when
Sputtering chamber vacuum reaches 1.0 × 10-4During Pa, sputter gas argon gas is passed through, makes C target build-ups of luminance, while be passed through N2, carry out first
Layer CN films are coated with, during plated film：Power 50w, Ar 30sccm, N2For 3sccm, operating air pressure is maintained at 0.5Pa, during sputtering
Between 60s.The preparation of second layer metal tungsten is then carried out, its technological parameter is：Power 50w, Ar 20sccm, operating air pressure are kept
In 0.5Pa, sputtering time 5s.Then it is identical with first layer in the preparation of progress third layer CN films, technological parameter.Testing result
Now CN thin film crystallizations are in good condition for display, resistivity 1.53*1015Ω .cm, transmitance 82.5%, hardness test shows
Film is harder.
Embodiment 2：Using high purity graphite and high pure metal tungsten as experiment target, while the use of the high glass thoroughly of ultrawhite is substrate material
Material.It is first according to conventional method and ultrasonic wave cleaning is carried out to backing material, cleaning, which finishes, to be put it into magnetron sputtering chamber, when
Sputtering chamber vacuum reaches 1.0 × 10-4During Pa, sputter gas argon gas is passed through, makes C target build-ups of luminance, while be passed through N2, carry out first
Layer CN films are coated with, during plated film：Power 100w, Ar 20sccm, N2For 1sccm, operating air pressure is maintained at 1.0Pa, sputtering
Time 45s.The preparation of second layer metal tungsten is then carried out, its technological parameter is：Power 50w, Ar 20sccm, operating air pressure are protected
Hold in 0.5Pa, sputtering time 7s.Then it is identical with first layer in the preparation of progress third layer CN films, technological parameter.Detection knot
Fruit shows that now CN thin film crystallizations are in good condition, resistivity 4.52*1014Ω .cm, transmitance 90.5%, hardness test table
Bright film is harder.
Embodiment 3：Using high purity graphite and high pure metal tungsten as experiment target, while the use of the high glass thoroughly of ultrawhite is substrate material
Material.It is first according to conventional method and ultrasonic wave cleaning is carried out to backing material, cleaning, which finishes, to be put it into magnetron sputtering chamber, when
Sputtering chamber vacuum reaches 1.0 × 10-4During Pa, sputter gas argon gas is passed through, makes C target build-ups of luminance, while be passed through N2, carry out first
Layer CN films are coated with, during plated film：Power 200w, Ar 15sccm, N2For 1sccm, operating air pressure is maintained at 1.5Pa, sputtering
Time 30s.The preparation of second layer metal tungsten is then carried out, its technological parameter is：Power 50w, Ar 20sccm, operating air pressure are protected
Hold in 0.5Pa, sputtering time 10s.Then it is identical with first layer in the preparation of progress third layer CN films, technological parameter.Detection
As a result show that now CN thin film crystallizations are in good condition, resistivity 5.76*1011Ω .cm, transmitance 93.5%, hardness test
Show that film is harder.
Above three embodiment is only the general implementation of the present invention, and the technical concept and reality of the present invention is described in detail
Main points are applied, are not that protection scope of the present invention is limited, it is all any simply to be repaiied according to what spirit of the invention was made
Change and equivalent structure transformation or modification, all should be included within the scope of the present invention.
Claims (4)
1. a kind of high, high resistant W doping CN films preparation method, it is characterised in that comprise the following steps：
1）From the high glass thoroughly of ultrawhite as backing material, ultrasonic wave cleaning is carried out to backing material, reaches removal substrate surface
The purpose of greasy dirt and dust；
2）Backing material after cleaning is placed on specimen holder, is sent into sputtering chamber, is opened equipment, is vacuumized, in vacuum
Reach 1.0 × 10-4When, Ar gas is passed through, makes C target build-ups of luminance, carries out pre-sputtering to remove the oxide on surface and impurity, pre-sputtering is complete
Finish, be passed through N2Gas, first layer CN films are prepared on backing material by the reaction with C targets, disconnect N2Gas, specimen holder turn to W
Target, the sputtering of W targets build-up of luminance, plated film, layer of metal W films are prepared on first layer CN films, it is thin then to repeat above-mentioned first layer CN
The technique of film carries out the preparation of second of CN film, and high saturating, high resistant W doping CN films are obtained after the completion of plated film.
A kind of 2. high, high resistant W doping CN films preparation method as claimed in claim 1, it is characterised in that whole plated film
During the independent build-up of luminance of the target of W, C two, avoid cross pollution.
3. a kind of high, high resistant W doping CN films preparation method as claimed in claim 1, it is characterised in that it is thin to prepare CN
The C target power outputs of film are 50 ~ 300W；Ar flows are 10-30sccm；N2Flow is 1-7sccm；Operating air pressure is maintained at 0.2 ~
2.0Pa, sputtering time 30-60s.
4. a kind of high, high resistant W doping CN films preparation method as claimed in claim 1, it is characterised in that prepare W films
W target power outputs be 50-200w；Ar flows are 10-30sccm, air pressure 0.2-0.5Pa；Plated film time is 5-10s.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710795449.5A CN107502868A (en) | 2017-09-06 | 2017-09-06 | A kind of high, high resistant W doping CN films preparation method |
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| CN201710795449.5A CN107502868A (en) | 2017-09-06 | 2017-09-06 | A kind of high, high resistant W doping CN films preparation method |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030091918A (en) * | 2003-11-17 | 2003-12-03 | 한전건 | Coating systhesized on the parts of motor engines and coating apparatus |
| CN101768722A (en) * | 2008-12-29 | 2010-07-07 | 中国科学院兰州化学物理研究所 | Preparation method of hydrogen-containing nano-structure CNx gradient film |
| CN102660729A (en) * | 2012-04-27 | 2012-09-12 | 江苏科技大学 | ZrCN nanometer composite membrane and preparation method thereof |
| CN103451608A (en) * | 2013-08-08 | 2013-12-18 | 西安交通大学 | Wolframium (W) doped diamond-like coating and preparation method thereof |
| CN106756847A (en) * | 2016-12-21 | 2017-05-31 | 蚌埠玻璃工业设计研究院 | A kind of preparation method of witch culture DLC film |
-
2017
- 2017-09-06 CN CN201710795449.5A patent/CN107502868A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030091918A (en) * | 2003-11-17 | 2003-12-03 | 한전건 | Coating systhesized on the parts of motor engines and coating apparatus |
| CN101768722A (en) * | 2008-12-29 | 2010-07-07 | 中国科学院兰州化学物理研究所 | Preparation method of hydrogen-containing nano-structure CNx gradient film |
| CN102660729A (en) * | 2012-04-27 | 2012-09-12 | 江苏科技大学 | ZrCN nanometer composite membrane and preparation method thereof |
| CN103451608A (en) * | 2013-08-08 | 2013-12-18 | 西安交通大学 | Wolframium (W) doped diamond-like coating and preparation method thereof |
| CN106756847A (en) * | 2016-12-21 | 2017-05-31 | 蚌埠玻璃工业设计研究院 | A kind of preparation method of witch culture DLC film |
Non-Patent Citations (2)
| Title |
|---|
| 张永宏: "《现代薄膜材料与技术》", 30 June 2016, 西安：西北工业大学出版社 * |
| 王继刚: ""磁控溅射法制备CNx薄膜及其结构表征"", 《材料工程》 * |
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