CN110607510A - Method for preparing amorphous metal vanadium film by magnetron sputtering - Google Patents
Method for preparing amorphous metal vanadium film by magnetron sputtering Download PDFInfo
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- CN110607510A CN110607510A CN201910891147.7A CN201910891147A CN110607510A CN 110607510 A CN110607510 A CN 110607510A CN 201910891147 A CN201910891147 A CN 201910891147A CN 110607510 A CN110607510 A CN 110607510A
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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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
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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
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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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
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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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
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- Engineering & Computer Science (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to a method for preparing an amorphous metal vanadium film by magnetron sputtering, which comprises the following specific steps: 1) cleaning the surface of the substrate; 2) depositing an amorphous metal vanadium film on a substrate by adopting a magnetron sputtering instrument: placing the substrate on a substrate table in a vacuum chamber, and vacuumizing to 2.0 × 10‑4And (2) below Pa, taking argon as a working gas, keeping the substrate temperature at 25 +/-10 ℃, keeping the sputtering working pressure at 1.0-2.5 Pa, keeping the sputtering power at 50-100W, keeping the distance from the target to the substrate at 5-10 cm, keeping the substrate table at the rotating speed of 10-50 r/min, and depositing on the surface of the substrate to obtain the amorphous metal vanadium film. The amorphous metal vanadium film prepared by the invention has excellent corrosion resistance, uniform and compact structure, difficult electrochemical corrosion and surfaceThe formed layer of compact passive film can effectively prevent the interior of the metal from being further oxidized, and can be applied to the field of corrosion-resistant materials in the environments of chemical industry, oceans and the like.
Description
Technical Field
The invention belongs to the technical field of magnetron sputtering coating, and particularly relates to a method for preparing an amorphous metal vanadium film by magnetron sputtering.
Background
The corrosion resistance of vanadium metal is stronger, and is second to niobium and tantalum, and the vanadium metal has better corrosion resistance to saline water, dilute acid and alkali. It is resistant to corrosion by water, salt water, seawater, non-oxidizing acids and alkaline solutions. Except that hydrofluoric acid can slowly react with vanadium at room temperature, other halogen acids do not react with vanadium. Meanwhile, the vanadium metal core has outstanding physical properties, and has the characteristics of low irradiation activation, excellent mechanical property, high thermal conductivity, excellent corrosion resistance in molten alkali liquor, excellent irradiation resistance and the like, so that the vanadium metal core is widely applied to the high-tech fields of aviation, navigation, nuclear industry and the like.
However, in practical application, the vanadium film can be oxidized when being placed in the air, and the vanadium film after oxidation can greatly reduce the corrosion resistance of the vanadium film in an acid environment, and the hardness of the film can also be reduced to a certain extent. Furthermore, the vanadium film is finally oxidized to V2O5Then the melting point is reduced to 690 ℃, and the stability of the vanadium film at higher temperature is greatly reduced. These are fatal to the vanadium metal film, and can greatly limit the application of the vanadium metal film in aspects such as aluminum alloy protective layers, wall layer materials of reactors and the like.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing an amorphous metal vanadium film by magnetron sputtering aiming at the defects in the prior art, so that the oxidation resistance and the corrosion resistance of the vanadium film are improved.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the method for preparing the amorphous metal vanadium film by magnetron sputtering comprises the following specific steps:
1) surface cleaning of the substrate: sequentially putting the substrate into acetone and absolute ethyl alcohol for ultrasonic cleaning, then washing with deionized water, and then drying with high-purity dry nitrogen for later use;
2) depositing an amorphous metal vanadium film on a substrate by adopting a magnetron sputtering instrument: mounting a pure vanadium target on a sputtering target seat of a magnetron sputtering instrument, placing the substrate cleaned and reserved in the step 1) on a substrate table in a vacuum chamber, and vacuumizing to 2.0 multiplied by 10-4And (2) below Pa, taking argon as working gas, controlling the temperature of the substrate to be 25 +/-10 ℃, controlling the working pressure of sputtering to be 1.0-2.5 Pa, sputtering power to be 50-100W, controlling the distance from the target to the substrate to be 5-10 cm, and depositing the substrate table at the rotating speed of 10-50 r/min to obtain the amorphous metal vanadium film on the surface of the substrate.
According to the scheme, the substrate in the step 1) is lithium fluoride, diamond or a silicon wafer, and the thickness range of the substrate is 10 micrometers-2 mm.
According to the scheme, the purity of the pure vanadium target material in the step 2) is more than 99.999%.
According to the scheme, the purity of the argon in the step 2) is more than 99.999%, and the flow of the argon is 10-40 sccm.
According to the scheme, the sputtering time in the step 2) is 0.5-24 h, and when the sputtering time exceeds 2h, the sputtering is stopped for 30min every 2 h.
According to the scheme, the substrate table in the vacuum chamber in the step 2) is cooled by circulating water.
The invention further comprises the amorphous metal vanadium film prepared by the method, wherein the thickness of the amorphous metal vanadium film is 0.1-50 mu m.
The invention also comprises the application of the amorphous metal vanadium film as a corrosion-resistant material.
The method adopts a sputtering deposition method, and controls the sputtering temperature and the sputtering power to ensure that the energy of the sputtered vanadium particles is not enough to form crystalline substances, thereby obtaining the amorphous metal vanadium film.
The invention has the beneficial effects that: 1. the invention adopts the magnetron sputtering method for one-time deposition, does not need subsequent treatment, has simple process, high repeatability, energy consumption saving, low production cost and convenient large-scale production; 2. the amorphous metal vanadium film prepared by the invention has excellent corrosion resistance, uniform and compact structure, and no defects of crystal grains, crystal boundaries and the like frequently existing in metal crystals, so that electrochemical corrosion is not easy to generate, a compact passivation film formed on the surface can effectively prevent the interior of metal from being further oxidized, and the amorphous metal vanadium film can be applied to the field of corrosion-resistant materials in the environments of chemical engineering, oceans and the like.
Drawings
FIG. 1 is an X-ray diffraction pattern of the vanadium film prepared in example 1;
FIG. 2 is a surface scanning electron micrograph of a vanadium film prepared in example 1;
FIG. 3 is a scanning electron microscope image of a section of the vanadium film prepared in example 1;
FIG. 4 is the electrochemical test result of the vanadium film prepared in example 1 in 3.5 wt% NaCl solution;
FIG. 5 is an X-ray photoelectron spectrum of the vanadium film prepared in example 1;
FIG. 6 is a photograph of a sample of vanadium film prepared in example 2;
FIG. 7 is a surface scanning electron micrograph of a vanadium film prepared in example 2;
FIG. 8 is a scanning electron microscope image of a section of the vanadium film prepared in example 2;
FIG. 9 is an X-ray diffraction pattern of the vanadium film prepared in comparative example 1;
fig. 10 is a scanning electron micrograph of the surface of the vanadium film prepared in comparative example 1.
Detailed Description
The present invention is further described below in conjunction with the following figures, it being understood that the figures and the following embodiments are illustrative of the invention only and are not limiting.
Example 1
A method for preparing an amorphous metal vanadium film by magnetron sputtering comprises the following specific steps:
(1) cleaning the surface of the substrate:
the substrate is a Si (100) substrate with the thickness of 0.3mm, the substrate is sequentially placed in acetone and absolute ethyl alcohol to be respectively subjected to ultrasonic oscillation for 10min, organic matter impurities on the surface are removed, then the substrate is washed by deionized water, and then high-purity dry nitrogen is used for blow drying for standby;
(2) deposition of non-Si (100) substrates using magnetron sputtering apparatusCrystal metal vanadium film: installing a pure vanadium target on a sputtering target seat of a magnetron sputtering instrument, selecting a metal vanadium target with the purity of 99.999% as a deposition target, placing the substrate cleaned and reserved in the step (1) on a substrate table in a vacuum chamber, cooling the substrate table by circulating water, and vacuumizing to 2.0 multiplied by 10-4And (2) below Pa, taking argon with the purity of 99.999% as working gas, controlling the flow of the argon to be 30sccm, controlling the temperature of the substrate to be 25 +/-10 ℃, the working pressure of sputtering to be 1.0Pa, the sputtering power to be 100W, controlling the distance from the target to the substrate to be 70mm, controlling the rotating speed of the substrate table to be 10r/min, controlling the sputtering time to be 1h, and controlling the thickness of a vanadium film deposited on the surface of the substrate to be 680 nm.
The vanadium film obtained on the Si (100) substrate of this example was amorphous in X-ray diffraction pattern as shown in FIG. 1. The surface scanning electron microscope image of the vanadium film obtained in the embodiment is shown in fig. 2, and it can be seen from the photograph that the prepared film has a flat surface and uniform particle size; FIG. 3 is a scanning electron microscope image of the cross section of the vanadium film obtained in this example, and it can be seen from the photograph that the prepared film has uniform thickness, dense structure and good bonding with the substrate.
The electrochemical test result of the vanadium film obtained in the embodiment in the 3.5 wt% NaCl solution is shown in fig. 4, and as can be seen from the electrochemical test result in the 3.5 wt% NaCl solution shown in fig. 4, a long passivation platform appears in the anodic polarization region, which indicates that the vanadium film can generate an oxide film with good electrochemical stability during the anodic polarization process, and meanwhile, the vanadium film has a high corrosion potential (-0.803V) and a low self-corrosion current (13.074 μ a cm)-2) High polarization resistance (137.226 omega cm)-2) And the corrosion resistance is good.
The X-ray photoelectron spectrum of the vanadium film obtained in this example is shown in fig. 5, and as can be seen from the X-ray photoelectron spectrum test result shown in fig. 5, the surface of the prepared film after the sputtering chamber is taken out was oxidized in the air (the X-ray photoelectron spectrum immediately after the film was taken out from the sputtering chamber is shown in fig. 5 (a)), and the surface of the film after 90 days of standing was completely covered with the oxide layer (the X-ray photoelectron spectrum after 90 days of standing is shown in fig. 5 (b)). However, the oxidation state of the vanadium film at a depth of 200nm in the film (the X-ray photoelectron spectrum at 200nm in the vanadium film just after being taken out from the sputtering chamber is shown in FIG. 5 (c)) and the oxidation state of the vanadium film after being left for 90 days (the X-ray photoelectron spectrum at 200nm in the vanadium film after being left for 90 days is shown in FIG. 5 (d)) are basically the same, which shows that the vanadium film has good oxidation resistance at normal temperature, the surface oxidation thickness is less than 200nm, and a very thin and dense passivation film is formed on the surface. The existing conventional vanadium film is oxidized on the surface and in the interior after being placed in the air for a period of time.
Example 2
An amorphous vanadium metal film was prepared in a similar manner to example 1, except that:
the used substrate is a lithium fluoride substrate, the coating mode is that sputtering is stopped for 30min and then continues to be performed after each 2h of sputtering, and the total sputtering time is 16 h.
The vanadium film prepared in this example did not peel off, cracked, and had good adhesion (the actual photograph is shown in fig. 6).
The vanadium film prepared in the embodiment has a flat surface and uniform particle size (the surface scanning electron microscope image is shown in fig. 7).
The vanadium film prepared by the embodiment has uniform thickness of 15.7 μm, compact structure and good combination with the substrate (the cross-section scanning electron microscope picture is shown in figure 8).
Example 3
An amorphous vanadium metal film was prepared in a similar manner to example 1, except that:
the sputtering power in the step (2) is 50W.
The thickness of the amorphous vanadium film prepared in this example was measured to be 240 nm.
Comparative example 1
A metal vanadium thin film was prepared in a similar manner to example 1, except that:
in the step (2), the sputtering power is 200W, and the temperature of the substrate table is set to be 100 ℃.
In the X-ray diffraction pattern 9 of the vanadium film obtained in this comparative example, the diffraction peaks at about 42 ° and 76.7 ° correspond to the V (110) plane and the V (211) plane, respectively, and it is seen that the vanadium film is a vanadium film having a crystal structure.
The vanadium film obtained in the comparative example has a large surface particle size (about 120nm), and the particles have a tetrahedral shape (the surface scanning electron microscope image is shown in FIG. 10).
The present invention is not limited to the above-described embodiments, and any modifications, equivalent substitutions, improvements, etc., which are within the spirit and principle of the present invention, should be included in the scope of the present invention.
Claims (8)
1. A method for preparing an amorphous metal vanadium film by magnetron sputtering is characterized by comprising the following specific steps:
1) surface cleaning of the substrate: sequentially putting the substrate into acetone and absolute ethyl alcohol for ultrasonic cleaning, then washing with deionized water, and then drying with high-purity dry nitrogen for later use;
2) depositing an amorphous metal vanadium film on a substrate by adopting a magnetron sputtering instrument: mounting a pure vanadium target on a sputtering target seat of a magnetron sputtering instrument, placing the substrate cleaned and reserved in the step 1) on a substrate table in a vacuum chamber, and vacuumizing to 2.0 multiplied by 10-4And (2) below Pa, taking argon as working gas, controlling the temperature of the substrate to be 25 +/-10 ℃, controlling the working pressure of sputtering to be 1.0-2.5 Pa, sputtering power to be 50-100W, controlling the distance from the target to the substrate to be 5-10 cm, and depositing the substrate table at the rotating speed of 10-50 r/min to obtain the amorphous metal vanadium film on the surface of the substrate.
2. The method for preparing the amorphous metal vanadium film by magnetron sputtering according to claim 1, wherein the substrate in the step 1) is lithium fluoride, diamond or a silicon wafer, and the thickness of the substrate ranges from 10 μm to 2 mm.
3. The method for preparing the amorphous metal vanadium film by magnetron sputtering according to claim 1, wherein the purity of the pure vanadium target in the step 2) is more than 99.999%.
4. The method for preparing the amorphous metal vanadium film by magnetron sputtering according to claim 1, wherein the argon purity in the step 2) is more than 99.999 percent, and the argon flow is 10-40 sccm.
5. The method for preparing the amorphous metal vanadium film by magnetron sputtering according to claim 1, wherein the sputtering time in the step 2) is 0.5-24 h, and when the sputtering time exceeds 2h, the sputtering is stopped for 30min every 2 h.
6. The method for preparing the amorphous metal vanadium film by magnetron sputtering as claimed in claim 1, wherein the substrate stage in the vacuum chamber in the step 2) is cooled by circulating water.
7. The amorphous metal vanadium film prepared according to any one of claims 1 to 6, wherein the thickness of the amorphous metal vanadium film is 0.1 to 50 μm.
8. Use of the amorphous vanadium metal film of claim 7 as a corrosion resistant material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910891147.7A CN110607510A (en) | 2019-09-20 | 2019-09-20 | Method for preparing amorphous metal vanadium film by magnetron sputtering |
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| CN201910891147.7A CN110607510A (en) | 2019-09-20 | 2019-09-20 | Method for preparing amorphous metal vanadium film by magnetron sputtering |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113774348A (en) * | 2021-09-22 | 2021-12-10 | 季华实验室 | High-temperature superconductor with amorphous vanadium oxide film, preparation method thereof and high-temperature superconducting coil |
| CN116514055A (en) * | 2023-06-27 | 2023-08-01 | 深圳市汉嵙新材料技术有限公司 | Composite hydrogen storage membrane material, preparation method thereof and hydrogen storage tank |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105018881A (en) * | 2015-07-09 | 2015-11-04 | 北京理工大学 | Amorphous vanadium oxide film material containing V6O13 crystals and preparing method thereof |
-
2019
- 2019-09-20 CN CN201910891147.7A patent/CN110607510A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105018881A (en) * | 2015-07-09 | 2015-11-04 | 北京理工大学 | Amorphous vanadium oxide film material containing V6O13 crystals and preparing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| SONG ZHANG等: "Microstructure and Oxidation Behavior of Metal V Films Deposited by Magnetron Sputtering", 《MATERIALS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113774348A (en) * | 2021-09-22 | 2021-12-10 | 季华实验室 | High-temperature superconductor with amorphous vanadium oxide film, preparation method thereof and high-temperature superconducting coil |
| CN113774348B (en) * | 2021-09-22 | 2023-06-02 | 季华实验室 | High-temperature superconductor with amorphous vanadium oxide film, preparation method thereof and high-temperature superconducting coil |
| CN116514055A (en) * | 2023-06-27 | 2023-08-01 | 深圳市汉嵙新材料技术有限公司 | Composite hydrogen storage membrane material, preparation method thereof and hydrogen storage tank |
| CN116514055B (en) * | 2023-06-27 | 2023-11-28 | 深圳市汉嵙新材料技术有限公司 | Composite hydrogen storage membrane material, preparation method thereof and hydrogen storage tank |
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Application publication date: 20191224 |