CN106947940A - A kind of DLC film and preparation method thereof - Google Patents
A kind of DLC film and preparation method thereof Download PDFInfo
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- CN106947940A CN106947940A CN201710270328.9A CN201710270328A CN106947940A CN 106947940 A CN106947940 A CN 106947940A CN 201710270328 A CN201710270328 A CN 201710270328A CN 106947940 A CN106947940 A CN 106947940A
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0605—Carbon
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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
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
This application provides a kind of DLC film and preparation method thereof.The preparation method that the present invention is provided includes：Graphite target is subjected to magnetron sputtering in mixed-gas environment, deposition obtains DLC film on substrate；The mixed gas is argon gas, hydrogen and nitrogen.Not only there is good optical characteristics according to DLC film made from the preparation method of the present invention, while also having good hardness and wearability, the device required to optically and mechanically performance can be applied to.
Description
Technical field
The present invention relates to thin film technique field, more particularly to a kind of DLC film and preparation method thereof.
Background technology
Carbon atom in diamond is with SP3The form of hybrid bond is combined, and the carbon atom in graphite is with SP2The form of hybrid bond
With reference to, and DLC film (abbreviation DLC film) is the SP by diamond lattic structure3The SP of hydbridized carbon atoms and graphite-structure2It is miscellaneous
Change carbon atom and mutually mix the three-dimensional network to be formed composition, be a kind of metastable state non-crystalline material.DLC film has high hard
Degree, low-friction coefficient, high heat conductance, low-k, broad-band gap, good light light transmittance, wear-and corrosion-resistant and good biofacies
The features such as capacitive, there is wide application in fields such as Aero-Space, machinery, electronics, optics, decorative appearance protection, biomedicines
Prospect.
DLC film is generally divided into hydrogen-containing carbon film (a-C:H) and the not class of hydrogen-containing carbon film (a-C) two, wherein, hydrogen-containing carbon
Carbon film is hydrogenated after film hydrogen loading, film is had excellent transparency, and can operate with has special to transparency and optical characteristics requirement
It is required that product, such as mobile phone front and rear cover plate, wrist-watch cover plate, camera eyeglass.But, compared to not hydrogeneous DLC film, mix
The hardness and wearability of DLC film after hydrogen have declined, it is impossible to while having good optical characteristics and the wear-resisting machine of hardness concurrently
Tool performance, it is difficult to suitable for the device required to optical characteristics and mechanical performance.
The content of the invention
In view of this, it is an object of the invention to provide a kind of DLC film and preparation method thereof, according to the present invention
Preparation method made from DLC film on the basis of optical characteristics is met, also with good hardness and wearability.
The invention provides a kind of preparation method of DLC film, including：
Graphite target is subjected to magnetron sputtering in mixed-gas environment, deposition obtains DLC film on substrate；
The mixed gas is argon gas, hydrogen and nitrogen.
It is preferred that, argon flow amount is 20~50sccm, and hydrogen flowing quantity is 10~20sccm, and nitrogen flow is 1~10sccm.
It is preferred that, in the mixed gas, the volume ratio of argon gas, hydrogen and nitrogen is 2：(1~2)：(0.1~0.3).
It is preferred that, the air pressure of the mixed gas is 1~8mTorr.
It is preferred that, the operating voltage of the magnetron sputtering is 400~700V.
It is preferred that, the power of the magnetron sputtering is 4~9KW.
It is preferred that, graphite target is carried out before magnetron sputtering in mixed-gas environment, also including sputtering chamber is vacuumized.
It is preferred that, the vacuum of the vacuum is 2 × 10-6~8 × 10-6mTorr。
Present invention also offers DLC film made from the preparation method described in above-mentioned technical proposal.
It is preferred that, the thickness of the DLC film is 2~4nm.
The invention provides a kind of preparation method of DLC film, graphite target is carried out in mixed-gas environment
Magnetron sputtering, deposition obtains DLC film on substrate；The mixed gas is argon gas, hydrogen and nitrogen.According to this hair
DLC film made from bright preparation method not only has good optical characteristics, while also having good hardness and resistance to
Mill property, can be applied to the device required to optically and mechanically performance.
Embodiment
The invention provides a kind of preparation method of DLC film, including：
Graphite target is subjected to magnetron sputtering in mixed-gas environment, deposition obtains DLC film on substrate；
The mixed gas is argon gas, hydrogen and nitrogen.
The general principle of magnetron sputtering is as follows：The electronics sent using electric field acceleration from negative electrode, electronics obtains enough kinetic energy,
The cation that working gas atom is ionized into plasma, plasma flies to target, target under target cathode electric field action
Material surface sputters ion, atom, atomic group etc., on these electrodeposition substances to substrate/substrate, forms film.
In the present invention, before magnetron sputtering is carried out, preferably first substrate or substrate are cleaned, surface and oil contaminant and ash is removed
After dirt, then it is placed in sputtering chamber.In the present invention, the species of substrate or substrate used is not particularly limited, and is to plate the need for routine
The object of DLC film, such as can be glass, ceramics or metal etc..
In the present invention, from target of the graphite target as magnetron sputtering.In the present invention, graphite target is preferably that purity is
More than 99.999% high purity graphite target.
In the present invention, the distance between substrate and target are not particularly limited, and are according to conventional sputter distance in this area
Can, such as can be 5~15cm.
In the present invention, before magnetron sputtering is carried out, preferably it will first be vacuumized in sputtering chamber.In the present invention, the vacuum
Vacuum is preferably 2 × 10-6~8 × 10-6mTorr。
After being vacuumized in sputtering chamber, gas is passed through, magnetron sputtering is carried out in the environment of mixed gas.In the present invention,
Environment is sputtered there is provided gas as mixed gas using argon gas, hydrogen and nitrogen, wherein, argon gas is working gas, hydrogen and nitrogen
Gas is reacting gas.In the present invention, argon flow amount is preferably 20~50sccm, more preferably 30~40sccm.Hydrogen flowing quantity is excellent
Elect 10~20sccm, more preferably 15sccm as.Nitrogen flow is preferably 1~10sccm, more preferably 2~5sccm.The present invention
In, in the mixed gas, the volume ratio of argon gas, hydrogen and nitrogen is preferably 2：(1~2)：(0.1~0.3), more preferably 2:
1:0.1, control various gases in mixed gas to be conducive to acquisition to have good optical and hardness, wearability concurrently in this proportion
Film product, if less than above range or beyond above range, being easily caused film performance decline, it is difficult to balance optical and hard
Degree, wearability.
In the present invention, in magnetron sputtering process, the overall air pressure for preferably controlling mixed gas is 1~8mTorr, if air pressure is low
In this scope, target as sputter efficiency is low during magnetron sputtering under the gaseous environment of the application, and film layer defect increases, film quality and
Hydraulic performance decline, if beyond above range, sputtering insufficient, makes film quality be deteriorated.
In the present invention, the operating voltage for preferably controlling magnetron sputtering is 400~700V, if less than this scope, in the application
Gaseous environment under magnetron sputtering when, target as sputter efficiency is low, rate of film build decline；If beyond this scope, in the gas of the application
Substrate is generated heat and is produced secondary sputtering under body environment during magnetron sputtering, make quality of forming film and film performance poor.This hair
In bright, the sputtering power for preferably controlling magnetron sputtering is 4~9KW.In the present invention, the time of magnetron sputtering is preferably 15~45s.
Graphite target is carried out after magnetron sputtering in mixed-gas environment, deposition obtains the class of hydrogen loading nitrating on substrate
Diamond thin (N-DLC films), according to the present invention preparation means and regulate and control sputtering condition and parameter to DLC film
It is doped, makes obtained N-DLC films that not only there is good optical characteristics, while also there is good hardness and wear-resisting
Property, the device required to optically and mechanically performance can be applied to.
Present invention also offers DLC film made from the preparation method described in above-mentioned technical proposal.In the present invention,
The thickness of the DLC film is preferably 2~4nm.
Test result indicate that, according to the light transmittance of most of DLC film product made from the preparation method of the present invention
More than 92% is reached, Mohs' hardness reaches more than 7, entered using the steel wool that size is 2 × 2cm under conditions of load is 1Kg
Row frictional experiment, Rubbing number reaches more than 100000.
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still
It should be appreciated that these descriptions are simply to further illustrate the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
Embodiment 1
Cleaned glass substrate is put into sputtering chamber, and the distance between regulation high purity graphite target and substrate are 10cm.It is right
Sputtering chamber is vacuumized, and it is 5 × 10 to make vacuum-6mTorr.Gas valve is opened, argon gas, hydrogen and nitrogen is passed through, gas is adjusted
Flow control valve, it is 30sccm to make argon flow amount, and hydrogen flowing quantity is 15sccm, and nitrogen flow is 5sccm, and control is passed through argon
The volume ratio of gas, hydrogen and nitrogen is 2:1:0.1, and it is 5mTorr to control the gas pressure intensity in sputtering chamber.Control magnetron sputtering
Operating voltage be 500V, regulation and control sputtering power be 5KW, sputtering 30s, the depositing diamond-like film on substrate.To gained class
The properties of diamond thin are detected, are as a result shown：Its light transmittance is 94%, and Mohs' hardness is 8, is 2 using size
× 2cm steel wool carries out frictional experiment under conditions of load is 1Kg, and Rubbing number reaches more than 100000.
Embodiment 2
Cleaned glass substrate is put into sputtering chamber, and the distance between regulation high purity graphite target and substrate are 10cm.It is right
Sputtering chamber is vacuumized, and it is 5 × 10 to make vacuum-6mTorr.Gas valve is opened, argon gas, hydrogen and nitrogen is passed through, gas is adjusted
Flow control valve, it is 30sccm to make argon flow amount, and hydrogen flowing quantity is 15sccm, and nitrogen flow is 5sccm, and control is passed through argon
The volume ratio of gas, hydrogen and nitrogen is 2:2:0.3, and it is 5mTorr to control the gas pressure intensity in sputtering chamber.Control magnetron sputtering
Operating voltage be 500V, regulation and control sputtering power be 5KW, sputtering 30s, the depositing diamond-like film on substrate.To gained class
The properties of diamond thin are detected, are as a result shown：Its light transmittance is 94%, and Mohs' hardness is 8, is 2 using size
× 2cm steel wool carries out frictional experiment under conditions of load is 1Kg, and Rubbing number reaches more than 100000.
Embodiment 3
Cleaned glass substrate is put into sputtering chamber, and the distance between regulation high purity graphite target and substrate are 10cm.It is right
Sputtering chamber is vacuumized, and it is 5 × 10 to make vacuum-6mTorr.Gas valve is opened, argon gas, hydrogen and nitrogen is passed through, gas is adjusted
Flow control valve, it is 30sccm to make argon flow amount, and hydrogen flowing quantity is 15sccm, and nitrogen flow is 5sccm, and control is passed through argon
The volume ratio of gas, hydrogen and nitrogen is 2:1:0.1, and it is 15mTorr to control the gas pressure intensity in sputtering chamber.Control magnetron sputtering
Operating voltage be 500V, regulation and control sputtering power be 5KW, sputtering 30s, the depositing diamond-like film on substrate.To gained class
The properties of diamond thin are detected, are as a result shown：Its light transmittance is 94%, and Mohs' hardness is 5, is 2 using size
× 2cm steel wool carries out frictional experiment under conditions of load is 1Kg, and Rubbing number reaches more than 50000.
Embodiment 4
Cleaned glass substrate is put into sputtering chamber, and the distance between regulation high purity graphite target and substrate are 10cm.It is right
Sputtering chamber is vacuumized, and it is 5 × 10 to make vacuum-6mTorr.Gas valve is opened, argon gas, hydrogen and nitrogen is passed through, gas is adjusted
Flow control valve, it is 30sccm to make argon flow amount, and hydrogen flowing quantity is 15sccm, and nitrogen flow is 5sccm, and control is passed through argon
The volume ratio of gas, hydrogen and nitrogen is 2:1:0.1, and it is 0.5mTorr to control the gas pressure intensity in sputtering chamber.Control magnetic control splashes
The operating voltage penetrated is 500V, and regulation and control sputtering power is 5KW, sputters 30s, the depositing diamond-like film on substrate.To gained
The properties of DLC film are detected, are as a result shown：Its light transmittance is 93%, and Mohs' hardness is 5, is using size
2 × 2cm steel wool carries out frictional experiment under conditions of load is 1Kg, and Rubbing number reaches more than 50000.
Embodiment 5
Cleaned glass substrate is put into sputtering chamber, and the distance between regulation high purity graphite target and substrate are 10cm.It is right
Sputtering chamber is vacuumized, and it is 5 × 10 to make vacuum-6mTorr.Gas valve is opened, argon gas, hydrogen and nitrogen is passed through, gas is adjusted
Flow control valve, it is 30sccm to make argon flow amount, and hydrogen flowing quantity is 15sccm, and nitrogen flow is 5sccm, and control is passed through argon
The volume ratio of gas, hydrogen and nitrogen is 2:1:0.1, and it is 5mTorr to control the gas pressure intensity in sputtering chamber.Control magnetron sputtering
Operating voltage be 100V, regulation and control sputtering power be 5KW, sputtering 30s, the depositing diamond-like film on substrate.To gained class
The properties of diamond thin are detected, are as a result shown：Its light transmittance is 94%, and Mohs' hardness is 5, is 2 using size
× 2cm steel wool carries out frictional experiment under conditions of load is 1Kg, and Rubbing number reaches more than 50000.
Comparative example 1
Cleaned glass substrate is put into sputtering chamber, and the distance between regulation high purity graphite target and substrate are 10cm.It is right
Sputtering chamber is vacuumized, and it is 5 × 10 to make vacuum-6mTorr.Gas valve is opened, argon gas and hydrogen, adjusting gas flow control is passed through
Valve processed, it is 30sccm to make argon flow amount, and hydrogen flowing quantity is 15sccm, and it is 2 to control the volume ratio for being passed through argon gas and hydrogen:1, and
It is 5mTorr to control the gas pressure intensity in sputtering chamber.The operating voltage for controlling magnetron sputtering is 500V, and regulation and control sputtering power is
5KW, sputters 30s, the depositing diamond-like film on substrate.The properties of gained DLC film are detected, tied
Fruit shows：Its light transmittance is 94%, and Mohs' hardness is 6, using the steel wool that size is 2 × 2cm under conditions of load is 1Kg
Frictional experiment is carried out, Rubbing number reaches less than 80000.
The explanation of above example is only intended to help and understands the method for the present invention and its core concept.To these embodiments
A variety of modifications will be apparent for those skilled in the art, generic principles defined herein can be with
Without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will not be limited
In the embodiments shown herein, and it is to fit to the most wide model consistent with features of novelty with principles disclosed herein
Enclose.
Claims (10)
1. a kind of preparation method of DLC film, it is characterised in that including：
Graphite target is subjected to magnetron sputtering in mixed-gas environment, deposition obtains DLC film on substrate；
The mixed gas is argon gas, hydrogen and nitrogen.
2. preparation method according to claim 1, it is characterised in that argon flow amount is 20~50sccm, hydrogen flowing quantity is
10~20sccm, nitrogen flow is 1~10sccm.
3. preparation method according to claim 1 or 2, it is characterised in that in the mixed gas, argon gas, hydrogen and nitrogen
The volume ratio of gas is 2：(1~2)：(0.1~0.3).
4. preparation method according to claim 1 or 2, it is characterised in that the air pressure of the mixed gas is 1~
8mTorr。
5. preparation method according to claim 1, it is characterised in that the operating voltage of the magnetron sputtering is 400~
700V。
6. preparation method according to claim 1 or 5, it is characterised in that the power of the magnetron sputtering is 4~9KW.
7. preparation method according to claim 1, it is characterised in that graphite target is subjected to magnetic in mixed-gas environment
Before control sputtering, also including sputtering chamber is vacuumized.
8. preparation method according to claim 7, it is characterised in that the vacuum of the vacuum is 2 × 10 -6~8 × 10 - 6mTorr。
9. DLC film made from a kind of preparation method according to any one of claims 1 to 8.
10. DLC film according to claim 9, it is characterised in that the thickness of the DLC film is 2~
4nm。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500566A (en) * | 2017-10-17 | 2017-12-22 | 信利光电股份有限公司 | A kind of wear-resisting anti-fingerprint ground glass and preparation method thereof |
| CN108149193A (en) * | 2017-12-26 | 2018-06-12 | 信利光电股份有限公司 | A kind of diamond-like carbon-base film and preparation method thereof |
| CN109087868A (en) * | 2018-07-10 | 2018-12-25 | 信利光电股份有限公司 | A kind of engraving method |
| CN114703451A (en) * | 2022-03-01 | 2022-07-05 | 常州工学院 | Preparation of high sp3Method for preparing diamond-like carbon film with carbon-carbon bond content |
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| CN1267745A (en) * | 2000-04-07 | 2000-09-27 | 上海交通大学 | Preparation of solar energy photovoltaic material-carbon film |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500566A (en) * | 2017-10-17 | 2017-12-22 | 信利光电股份有限公司 | A kind of wear-resisting anti-fingerprint ground glass and preparation method thereof |
| CN108149193A (en) * | 2017-12-26 | 2018-06-12 | 信利光电股份有限公司 | A kind of diamond-like carbon-base film and preparation method thereof |
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| CN114703451A (en) * | 2022-03-01 | 2022-07-05 | 常州工学院 | Preparation of high sp3Method for preparing diamond-like carbon film with carbon-carbon bond content |
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Application publication date: 20170714 |