CN114150266A - Preparation method of molybdenum disulfide film - Google Patents
Preparation method of molybdenum disulfide film Download PDFInfo
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- CN114150266A CN114150266A CN202111466962.2A CN202111466962A CN114150266A CN 114150266 A CN114150266 A CN 114150266A CN 202111466962 A CN202111466962 A CN 202111466962A CN 114150266 A CN114150266 A CN 114150266A
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- molybdenum disulfide
- disulfide film
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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
- C23C14/0623—Sulfides, selenides or tellurides
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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
- C23C14/22—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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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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
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
- C23C14/5853—Oxidation
Abstract
The invention discloses a preparation method of a molybdenum disulfide film, which comprises the steps of cleaning a workpiece, then placing the cleaned workpiece in a magnetron sputtering furnace, and carrying out constant-current source sputtering treatment in a vacuum environment; the treated workpiece is put into a heating furnace for heating, and oxygen is introduced for high-temperature oxidation; and finally, blowing the high-temperature oxidized workpiece by using a nitrogen spray gun for annealing, and annealing to normal temperature to obtain the workpiece attached with the molybdenum disulfide film. The invention adopts the high-temperature oxidation and annealing process after sputtering, and is effectively combined with the surface of the metal workpiece, thereby ensuring the binding force between the molybdenum disulfide material and the surface of the metal workpiece, avoiding introducing additional defects in the transfer process and improving the quality of the prepared attached molybdenum disulfide workpiece; and then the quality of the prepared film is improved by adjusting each reaction parameter or the mass ratio of the raw materials in the preparation process. The operation steps are simple, the product quality is high, and the method is suitable for meeting the requirements of the surface quality of the workpiece with wear resistance, compression resistance, high temperature resistance and lubrication.
Description
Technical Field
The invention relates to the field of material technical processing methods, in particular to a preparation method of a molybdenum disulfide film.
Background
The traditional preparation method of the molybdenum disulfide film is to prepare a molybdenum disulfide material Si substrate and then transplant the substrate to other materials. Although the technology is simple and easy to implement and strong in universality, the technology has the fatal defects that the bonding force between the molybdenum disulfide material and the substrate material is poor, additional defects are introduced in the transfer process, the product quality is reduced, and in addition, the transfer and transplantation process is quite complicated. Therefore, the material prepared in this way cannot be widely used, the physical properties of the material are weak, and a new preparation method of a new molybdenum disulfide film is needed.
Disclosure of Invention
The invention aims to solve the problems and provide a preparation method of a molybdenum disulfide film.
The invention realizes the purpose through the following technical scheme:
the invention comprises the following steps:
s1: cleaning the workpiece;
s2: putting the cleaned workpiece in a magnetron sputtering furnace, and performing constant-current source sputtering treatment in a vacuum environment;
s3: putting the processed workpiece into a heating furnace for heating, and introducing oxygen for high-temperature oxidation;
s4: and (3) blowing the high-temperature oxidized workpiece by adopting a nitrogen spray gun for annealing, and annealing to normal temperature to obtain the workpiece attached with the molybdenum disulfide film.
Further, in step S1, the cleaning of the workpiece includes the following steps:
s1.1: carrying out sand blasting cleaning on the workpiece;
s1.2: and putting the workpiece cleaned by sand blasting into deionized water for ultrasonic cleaning.
Preferably, the grain size of the spraying material is as follows: 0.2mm-0.3 mm; the compressed air pressure used to spray the spray was: 0.6 plus or minus 0.05 MPa; the distance from a nozzle for spraying the spray material to the surface of the workpiece is as follows: 20cm-25 cm.
Preferably, the power of the ultrasonic cleaning is 300-.
Preferably, in the step S2, the vacuum degree is 1.5 × 10-3Pa。
Preferably, in the step S2, the magnetron sputtering gas pressure is 12 to 15 Pa; the magnetron sputtering voltage is 900-1000V; magnetron sputtering current is 4-6A; the magnetron sputtering time is 40-50 min. Preferably, in the step S3, the heating temperature is 800-1100 ℃, and the high-temperature oxidation time is 70-90 min.
The invention has the beneficial effects that:
the invention relates to a preparation method of a molybdenum disulfide film, compared with the prior art, the preparation method adopts a high-temperature oxidation and annealing process after sputtering, and is effectively combined with the surface of a metal workpiece, so that the binding force between a molybdenum disulfide material and the surface of the metal workpiece is ensured, no additional defect is introduced in the transfer process, and the quality of the prepared attached molybdenum disulfide workpiece is improved; and the quality of the prepared film is further improved by adjusting each reaction parameter or the mass ratio of the raw materials in the preparation process. In general, the method has the advantages of simple operation steps and high product quality, is suitable for meeting the surface quality requirements of wear-resistant, pressure-resistant, high-temperature-resistant and lubricated workpieces, and has popularization and application values.
Drawings
FIG. 1 is a microscopical surface view of the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings in which:
the invention comprises the following steps:
s1: cleaning the workpiece;
s2: putting the cleaned workpiece in a magnetron sputtering furnace, and performing constant-current source sputtering treatment in a vacuum environment;
s3: putting the processed workpiece into a heating furnace for heating, and introducing oxygen for high-temperature oxidation;
s4: and (3) blowing the high-temperature oxidized workpiece by adopting a nitrogen spray gun for annealing, and annealing to normal temperature to obtain the workpiece attached with the molybdenum disulfide film.
Further, in step S1, the cleaning of the workpiece includes the following steps:
s1.1: carrying out sand blasting cleaning on the workpiece;
s1.2: and putting the workpiece cleaned by sand blasting into deionized water for ultrasonic cleaning.
Preferably, the grain size of the spraying material is as follows: 0.2mm-0.3 mm; the compressed air pressure used to spray the spray was: 0.6 plus or minus 0.05 MPa; the distance from a nozzle for spraying the spray material to the surface of the workpiece is as follows: 20cm-25 cm.
Preferably, the power of the ultrasonic cleaning is 300-.
Preferably, in the step S2, the vacuum degree is 1.5 × 10-3Pa。
Preferably, in the step S2, the magnetron sputtering gas pressure is 12 to 15 Pa; the magnetron sputtering voltage is 900-1000V; magnetron sputtering current is 4-6A; the magnetron sputtering time is 40-50 min.
Preferably, in the step S3, the heating temperature is 800-1100 ℃, and the high-temperature oxidation time is 70-90 min.
The microscopic observation surface of the workpiece surface of the molybdenum disulfide film prepared by the method of the invention is shown in figure 1.
Example 1:
s1: the workpiece is cleaned by sand blasting and then is put into deionized water for ultrasonic cleaning, and the particle size of the spraying material is as follows: 0.2 mm; the compressed air pressure used to spray the spray was: 0.6 plus or minus 0.05 MPa; the distance from a nozzle for spraying the spray material to the surface of the workpiece is as follows: 20 cm; the power of ultrasonic cleaning is 300W, and the cleaning time is 100 min.
S2: the cleaned work piece was placed in a magnetron sputtering furnace at a vacuum of 1.5X 10-3Carrying out constant current source sputtering treatment in a Pa vacuum environment; the magnetron sputtering pressure is 12 Pa; magnetron sputtering voltage is 900V; magnetron sputtering current is 4A; magnetron sputtering time is 40 min;
s3: putting the treated workpiece into a heating furnace for heating at 800 ℃, and introducing oxygen for high-temperature oxidation for 70 min;
s4: and (3) blowing the high-temperature oxidized workpiece by adopting a nitrogen spray gun for annealing, and annealing to normal temperature to obtain the workpiece attached with the molybdenum disulfide film.
Example 2:
s1: the workpiece is cleaned by sand blasting and then is put into deionized water for ultrasonic cleaning, and the particle size of the spraying material is as follows: 0.25 mm; the compressed air pressure used to spray the spray was: 0.6 plus or minus 0.05 MPa; the distance from a nozzle for spraying the spray material to the surface of the workpiece is as follows: 22 cm; the power of ultrasonic cleaning is 350W, and the cleaning time is 110 min.
S2: the cleaned work piece was placed in a magnetron sputtering furnace at a vacuum of 1.5X 10-3Carrying out constant current source sputtering treatment in a Pa vacuum environment; the magnetron sputtering pressure is 14 Pa; magnetron sputtering voltage is 950V; magnetron sputtering current is 5A; magnetron sputtering time is 45 min;
s3: putting the treated workpiece into a heating furnace for heating at 900 ℃, and introducing oxygen for high-temperature oxidation for 80 min;
s4: and (3) blowing the high-temperature oxidized workpiece by adopting a nitrogen spray gun for annealing, and annealing to normal temperature to obtain the workpiece attached with the molybdenum disulfide film.
Example 3:
s1: the workpiece is cleaned by sand blasting and then is put into deionized water for ultrasonic cleaning, and the particle size of the spraying material is as follows: 0.3 mm; the compressed air pressure used to spray the spray was: 0.6 plus or minus 0.05 MPa; the distance from a nozzle for spraying the spray material to the surface of the workpiece is as follows: 25 cm; the power of ultrasonic cleaning is 400W, and the cleaning time is 120 min.
S2: the cleaned work piece was placed in a magnetron sputtering furnace at a vacuum of 1.5X 10-3Carrying out constant current source sputtering treatment in a Pa vacuum environment; the magnetron sputtering pressure is 15 Pa; magnetron sputtering voltage is 1000V; magnetron sputtering current is 6A; magnetron sputtering time is 50 min;
s3: putting the treated workpiece into a heating furnace for heating at 1100 ℃, and introducing oxygen for high-temperature oxidation for 90 min;
s4: and (3) blowing the high-temperature oxidized workpiece by adopting a nitrogen spray gun for annealing, and annealing to normal temperature to obtain the workpiece attached with the molybdenum disulfide film.
The results of the tests performed on the workpieces from examples 1-3 above are shown in the following table:
as can be seen from the above measurements of the physical properties of the workpiece, the physical properties of example 2 are superior to those of examples 1 and 3, and example 1 and example 3.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A preparation method of a molybdenum disulfide film is characterized by comprising the following steps:
s1: cleaning the workpiece;
s2: putting the cleaned workpiece in a magnetron sputtering furnace, and performing constant-current source sputtering treatment in a vacuum environment;
s3: putting the processed workpiece into a heating furnace for heating, and introducing oxygen for high-temperature oxidation;
s4: and (3) blowing the high-temperature oxidized workpiece by adopting a nitrogen spray gun for annealing, and annealing to normal temperature to obtain the workpiece attached with the molybdenum disulfide film.
2. The method for preparing a molybdenum disulfide film according to claim 1, wherein: in step S1, the cleaning of the workpiece includes the following steps:
s1.1: carrying out sand blasting cleaning on the workpiece;
s1.2: and putting the workpiece cleaned by sand blasting into deionized water for ultrasonic cleaning.
3. The method for preparing a molybdenum disulfide film according to claim 2, wherein: the grain size of the spraying material is as follows: 0.2mm-0.3 mm; the compressed air pressure used to spray the spray was: 0.6 plus or minus 0.05 MPa; the distance from a nozzle for spraying the spray material to the surface of the workpiece is as follows: 20cm-25 cm.
4. The method for preparing a molybdenum disulfide film according to claim 2, wherein: the power of the ultrasonic cleaning is 300-400W, and the cleaning time is 100-120 min.
5. The method for preparing a molybdenum disulfide film according to claim 1, wherein: in the step S2, the vacuum degree is 1.5 × 10-3Pa。
6. The method for preparing a molybdenum disulfide film according to claim 1, wherein: in the step S2, the magnetron sputtering air pressure is 12-15 Pa; the magnetron sputtering voltage is 900-1000V; magnetron sputtering current is 4-6A; the magnetron sputtering time is 40-50 min.
7. The method for preparing a molybdenum disulfide film according to claim 1, wherein: in the step S3, the heating temperature is 800-1100 ℃, and the high-temperature oxidation time is 70-90 min.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4943558A (en) * | 1988-04-15 | 1990-07-24 | Ford Motor Company | Preparation of superconducting oxide films using a pre-oxygen nitrogen anneal |
| CN101805892A (en) * | 2010-04-02 | 2010-08-18 | 上海工程技术大学 | Method for preparing zinc oxide films |
| CN103227286A (en) * | 2013-04-02 | 2013-07-31 | 武汉工程大学 | Organic photovoltaic cell taking sulfur-doped MoO3 film as anode interface layer and preparation method thereof |
| CN106835019A (en) * | 2016-12-26 | 2017-06-13 | 中科微机电技术（北京）有限公司 | Vanadium oxide composite film and preparation method thereof |
| CN109735807A (en) * | 2019-02-27 | 2019-05-10 | 华中科技大学 | A kind of preparation method of negative temperature coefficient heat-sensitive film |
| CN112210753A (en) * | 2020-10-20 | 2021-01-12 | 中国科学院宁波材料技术与工程研究所 | Molybdenum disulfide silver-doped sulfide film and preparation method and application thereof |
| CN112501555A (en) * | 2020-11-19 | 2021-03-16 | 南京大学 | Preparation method of single-layer molybdenum disulfide film |
| CN112853290A (en) * | 2021-01-05 | 2021-05-28 | 南昌大学 | Preparation method of large-area molybdenum disulfide film |
-
2021
- 2021-12-02 CN CN202111466962.2A patent/CN114150266A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4943558A (en) * | 1988-04-15 | 1990-07-24 | Ford Motor Company | Preparation of superconducting oxide films using a pre-oxygen nitrogen anneal |
| CN101805892A (en) * | 2010-04-02 | 2010-08-18 | 上海工程技术大学 | Method for preparing zinc oxide films |
| CN103227286A (en) * | 2013-04-02 | 2013-07-31 | 武汉工程大学 | Organic photovoltaic cell taking sulfur-doped MoO3 film as anode interface layer and preparation method thereof |
| CN106835019A (en) * | 2016-12-26 | 2017-06-13 | 中科微机电技术（北京）有限公司 | Vanadium oxide composite film and preparation method thereof |
| CN109735807A (en) * | 2019-02-27 | 2019-05-10 | 华中科技大学 | A kind of preparation method of negative temperature coefficient heat-sensitive film |
| CN112210753A (en) * | 2020-10-20 | 2021-01-12 | 中国科学院宁波材料技术与工程研究所 | Molybdenum disulfide silver-doped sulfide film and preparation method and application thereof |
| CN112501555A (en) * | 2020-11-19 | 2021-03-16 | 南京大学 | Preparation method of single-layer molybdenum disulfide film |
| CN112853290A (en) * | 2021-01-05 | 2021-05-28 | 南昌大学 | Preparation method of large-area molybdenum disulfide film |
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