CN111304586A - Humidity environment self-adaptive diamond-like film and preparation method thereof - Google Patents
Humidity environment self-adaptive diamond-like film and preparation method thereof Download PDFInfo
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- CN111304586A CN111304586A CN201811516645.5A CN201811516645A CN111304586A CN 111304586 A CN111304586 A CN 111304586A CN 201811516645 A CN201811516645 A CN 201811516645A CN 111304586 A CN111304586 A CN 111304586A
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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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
- C23C14/0073—Reactive sputtering by exposing the substrates to reactive gases intermittently
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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
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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Abstract
The invention discloses a humidity environment self-adaptive diamond-like film which comprises a base layer, N non-hydrogen type diamond-like sub-layers and M hydrogen type diamond-like sub-layers, wherein M is equal to N and is a natural number, the N is in one-to-one correspondence with the N, the hydrogen type diamond-like sub-layers are arranged on the base layer, the non-hydrogen type diamond-like sub-layers are arranged on the upper surfaces of the hydrogen type diamond-like sub-layers, and the hydrogen type diamond-like sub-layers and the non-hydrogen type diamond-like sub-layers are alternately stacked. Compared with the prior art, the design of the diamond-like film multilayer structure aims at self-adapting to the environment with large relative humidity change.
Description
Technical Field
The invention relates to a humidity environment self-adaptive diamond-like film and a preparation method thereof.
Background
Diamond-like Carbon (DLC) films are of great interest to researchers and manufacturers due to their high hardness, low coefficient of friction, low wear rate, good infrared transmittance, and excellent corrosion resistance. The diamond-like film can be divided into two categories, hydrogen-containing diamond-like film and hydrogen-free diamond-like film, depending on whether the film contains hydrogen or not. Relevant studies have shown that the environmental (e.g. relative humidity) impact on the wear resistance of diamond-like carbon is very significant. For the hydrogen-free diamond-like film, the wear rate of the film layer has a remarkable descending trend along with the increase of the relative humidity of the environment. Its wear rate in dry or vacuum environments (0% relative humidity) is two orders of magnitude higher than in high relative humidity environments. In contrast, the hydrogen-containing diamond-like film is excellent in a low relative humidity and even high vacuum environment, and the wear rate is greatly reduced compared with that in a high relative humidity environment, and the friction coefficient is correspondingly reduced, even can be as low as below 0.01. These properties of diamond-like carbon determine that the conventional single type of diamond-like carbon film containing hydrogen or no hydrogen can not fully satisfy the use requirements in the environment with large relative humidity change. These problems, while reducing the environmental sensitivity of the film to some extent by doping the film (e.g., with silicon), must be at the expense of a significant portion of the wear resistance and coefficient of friction.
Therefore, how to provide a humidity environment adaptive diamond-like film designed in a multilayer structure and aiming at adapting to an environment with large relative humidity change and a preparation method thereof is a technical problem to be solved by the invention.
Disclosure of Invention
In view of the above-mentioned drawbacks and problems of the prior art, it is an object of the present invention to provide a multilayer structure designed to be adaptive to a humidity environment adaptive diamond-like film of an environment having a large variation in relative humidity.
In order to achieve the above object, the present invention provides the following technical solutions
The humidity environment self-adaptive diamond-like film comprises a base layer, N non-hydrogen diamond-like sub-layers and M hydrogen diamond-like sub-layers, wherein M is equal to N and is a natural number, the N is in one-to-one correspondence, the base layer is provided with the hydrogen diamond-like sub-layers, the upper surfaces of the hydrogen diamond-like sub-layers are provided with the non-hydrogen diamond-like sub-layers, and the hydrogen diamond-like sub-layers and the non-hydrogen diamond-like sub-layers are alternately stacked.
Further, the hydrogen containing diamond-like sub-layer and the hydrogen-free diamond-like sub-layer each have a thickness of: 100 nm.
Further, the hydrogen-containing diamond-like sub-layer is arranged on the upper surface of the base layer in a plating mode, and the hydrogen-free diamond-like sub-layer is arranged on the upper surface of the hydrogen-containing diamond-like sub-layer in a plating process.
On the other hand, the invention also comprises a preparation method of the humidity environment self-adaptive diamond-like film, which comprises the following steps:
fourthly, preparation of workpieces to be plated
Placing a workpiece to be plated in acetone and isopropanol solutions in sequence, performing ultrasonic cleaning for 10 minutes respectively, and then drying the workpiece by using dry air to remove oil stains, impurities and the like attached to the surface of the workpiece to be plated;
fifthly, cleaning and activating the ion of the workpiece to be plated and pre-melting the film material
(1) Placing the processed workpiece to be plated on a rotary workpiece table in a vacuum chamber for fixing, and pumping the cavity of the vacuum chamber to 3 x 10-3Pa vacuum degree;
(2) the polycrystalline graphite film material in the copper crucible was pre-melted using an electron gun (8kV acceleration voltage, 150mA acceleration current) to remove adsorbed gas and surface impurities.
(3) Closing the electron gun, filling argon into the koffman ion source to maintain the vacuum degree in the vacuum chamber at 1 × 10-2Pa, regulating the voltage of a screen electrode to 300V, and keeping the ion beam current at 10mA for 5 minutes. Ar extraction by ion source+Cleaning the workpiece to be deposited by ion bombardment so as to clean and activate the surface of the workpiece;
sixthly, coating process
(1) Evaporating (sublimating) the polycrystalline graphite film material in the copper crucible by using an electron gun (8kV accelerating voltage, 300mA accelerating current), and simultaneously filling methane and argon (4:1 volume ratio) into a Koffman ion source to maintain the vacuum degree in the vacuum chamber at 1X 10-2Pa, regulating the voltage of a screen electrode to 300V and the ion beam current to 10mA to deposit a hydrogen-containing diamond-like film sub-layerStopping until the thickness reaches about 100 nm;
(2) keeping the parameters of the electron gun in the step (1) unchanged, stopping filling methane into the Kaufman ion source, and keeping the vacuum degree in the vacuum chamber at 1 x 10-2Pa, simultaneously keeping the working parameters of the Kaufman ion source unchanged to deposit a hydrogen-free diamond-like film sub-layer until the thickness is about 100 nm;
repeating the step (1) and the step (2) for several times alternately to deposit the hydrogen-containing type/hydrogen-free type diamond-like film with a multilayer structure.
Further, the volume ratio of methane to argon is 4: 1.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a structural view of the humidity environment adaptive diamond-like film of the present invention.
Description of reference numerals:
1 is a hydrogen-free diamond-like sublayer, 2 is a hydrogen-containing diamond-like sublayer, and 3 is a substrate.
Detailed Description
For the purpose of promoting a clear understanding of the objects, aspects and advantages of the embodiments of the invention, reference will now be made to the drawings and detailed description, wherein there are shown in the drawings and described in detail, various modifications of the embodiments described herein, and other embodiments of the invention will be apparent to those skilled in the art.
The exemplary embodiments of the present invention and the description thereof are provided to explain the present invention and not to limit the present invention. Additionally, the same or similar numbered elements/components used in the drawings and the embodiments are used to represent the same or similar parts.
As used herein, the terms "first," "second," …, etc., do not denote any order or sequence, nor are they used to limit the present invention, but rather are used to distinguish one element from another or from another element or operation described in the same technical language.
With respect to directional terminology used herein, for example: up, down, left, right, front or rear, etc., are simply directions with reference to the drawings. Accordingly, the directional terminology used is intended to be illustrative and is not intended to be limiting of the present teachings.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
As used herein, "and/or" includes any and all combinations of the described items.
As used herein, the terms "substantially", "about" and the like are used to modify any slight variation in quantity or error that does not alter the nature of the variation. Generally, the range of slight variations or errors modified by such terms may be 20% in some embodiments, 10% in some embodiments, 5% in some embodiments, or other values. It should be understood by those skilled in the art that the aforementioned values can be adjusted according to actual needs, and are not limited thereto.
Certain words used to describe the present application are discussed below or elsewhere in this specification to provide additional guidance to those skilled in the art in describing the present application.
As shown in fig. 1, the humidity environment adaptive diamond-like film disclosed by the invention comprises a base layer 3, N hydrogen-free diamond-like sublayers 1 and M hydrogen-containing diamond-like sublayers 2, wherein M is equal to N and is a natural number, the N and the N are in one-to-one correspondence, the hydrogen-containing diamond-like sublayers 2 are arranged on the base layer 3, the hydrogen-free diamond-like sublayers 1 are arranged on the upper surface of the hydrogen-containing diamond-like sublayers 2, and the hydrogen-containing diamond-like sublayers 2 and the hydrogen-free diamond-like sublayers 1 are alternately stacked.
The coating comprises a base layer, N hydrogen-free diamond sublayers 1 and M hydrogen-containing diamond sublayers 2, wherein M is equal to N and is a natural number, the N hydrogen-free diamond sublayers and the M hydrogen-free diamond sublayers correspond to each other one by one, the hydrogen-containing diamond sublayers and the hydrogen-free diamond sublayers are alternately superposed, the requirement on equipment is low, a common domestic general optical coating machine (provided with an electron beam evaporation source and an ion source) can meet the use requirement, and meanwhile, the coating process is simple and easy to implement and is easy to realize automatic control. The plated multilayer diamond-like film has a humidity environment self-adaptation function, and can maintain stable and excellent wear resistance in an alternating humidity environment.
In addition, the thicknesses of the hydrogen-containing diamond-like sub-layer 1 and the hydrogen-free diamond-like sub-layer 2 are as follows: 100nm, and is automatically controlled by a crystal controller, thereby being convenient to operate and saving materials.
In addition, it is worth mentioning that the hydrogen-containing diamond-like sub-layer 1 is arranged on the upper surface of the base layer by plating, and the hydrogen-free diamond-like sub-layer 1 is arranged on the upper surface of the hydrogen-containing diamond-like sub-layer 2 by plating, so that the hydrogen-containing diamond-like sub-layer and the hydrogen-free diamond-like sub-layer can be firmly fixed with each other without cracking, and the service life is prolonged.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (5)
1. The humidity environment self-adaptive diamond-like film is characterized by comprising a base layer, N non-hydrogen diamond-like sub-layers and M hydrogen diamond-like sub-layers, wherein M is equal to N and is a natural number, the N non-hydrogen diamond-like sub-layers correspond to the N non-hydrogen diamond-like sub-layers in a one-to-one mode, the hydrogen diamond-like sub-layers are arranged on the base layer, the non-hydrogen diamond-like sub-layers are arranged on the upper surfaces of the hydrogen diamond-like sub-layers, and the hydrogen diamond-like sub-layers and the non-hydrogen diamond-like sub-layers are alternately stacked.
2. The humidity environment adaptive diamond-like film according to claim 1, wherein: the hydrogen-containing diamond-like sub-layer and the hydrogen-free diamond-like sub-layer have the following thicknesses: 100 nm.
3. The humidity environment adaptive diamond-like film according to claim 1, wherein: the hydrogen-containing diamond-like sub-layer is arranged on the upper surface of the base layer in a plating mode, and the hydrogen-free diamond-like sub-layer is arranged on the upper surface of the hydrogen-containing diamond-like sub-layer in a plating process.
4. A method for preparing a humidity environment self-adaptive diamond-like film comprises the following steps:
first, preparation of workpiece to be plated
Placing a workpiece to be plated in acetone and isopropanol solutions in sequence, performing ultrasonic cleaning for 10 minutes respectively, and then drying the workpiece by using dry air to remove oil stains, impurities and the like attached to the surface of the workpiece to be plated;
secondly, cleaning and activating the ion of the workpiece to be plated and pre-melting the film material
(1) Placing the processed workpiece to be plated on a rotary workpiece table in a vacuum chamber for fixing, and pumping the cavity of the vacuum chamber to 3 x 10-3Pa vacuum degree;
(2) pre-melting the polycrystalline graphite film material in the copper crucible by using an electron gun to remove adsorbed gas and surface impurities;
(3) closing the electron gun, filling argon into the koffman ion source to maintain the vacuum degree in the vacuum chamber at 1 × 10- 2Pa, regulating the voltage of a screen electrode to 300V, and keeping the ion beam current at 10mA for 5 minutes. Ar extraction by ion source+Cleaning the workpiece to be deposited by ion bombardment so as to clean and activate the surface of the workpiece;
third, coating process
(1) Evaporating the polycrystalline graphite film material in the copper crucible by using an electron gun, simultaneously filling methane and argon into a Kaufman ion source,maintaining the vacuum degree in the vacuum chamber at 1 × 10-2Pa, regulating the voltage of a screen electrode to 300V and the ion beam current to 10mA to deposit a hydrogen-containing diamond-like film sub-layer until the thickness is about 100 nm;
(2) keeping the parameters of the electron gun in the step (1) unchanged, stopping filling methane into the Kaufman ion source, and keeping the vacuum degree in the vacuum chamber at 1 x 10-2Pa, simultaneously keeping the working parameters of the Kaufman ion source unchanged to deposit a hydrogen-free diamond-like film sub-layer until the thickness is about 100 nm;
repeating the step (1) and the step (2) for several times alternately to deposit the hydrogen-containing type/hydrogen-free type diamond-like film with a multilayer structure.
5. The method for preparing a humidity environment adaptive diamond-like film according to claim 4, wherein: the volume ratio of the methane to the argon is 4: 1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115198241A (en) * | 2022-06-27 | 2022-10-18 | 岭南师范学院 | Nano diamond-like amorphous carbon film and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103938211A (en) * | 2014-05-08 | 2014-07-23 | 西南交通大学 | Deposition method of low-stress corrosion-resistant multilayer diamond-like carbon (DLC) film |
| CN104630708A (en) * | 2015-03-06 | 2015-05-20 | 重庆大学 | Diamond-like thick film, preparation method of diamond-like thick film and work-piece |
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- 2018-12-12 CN CN201811516645.5A patent/CN111304586A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103938211A (en) * | 2014-05-08 | 2014-07-23 | 西南交通大学 | Deposition method of low-stress corrosion-resistant multilayer diamond-like carbon (DLC) film |
| CN104630708A (en) * | 2015-03-06 | 2015-05-20 | 重庆大学 | Diamond-like thick film, preparation method of diamond-like thick film and work-piece |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115198241A (en) * | 2022-06-27 | 2022-10-18 | 岭南师范学院 | Nano diamond-like amorphous carbon film and preparation method and application thereof |
| CN115198241B (en) * | 2022-06-27 | 2024-04-19 | 岭南师范学院 | Nano diamond-like amorphous carbon film and preparation method and application thereof |
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Application publication date: 20200619 |