CN109576658B - Preparation of dendritic amorphous MoS based on magnetron sputtering method2Method of nano-structuring - Google Patents

Preparation of dendritic amorphous MoS based on magnetron sputtering method2Method of nano-structuring Download PDF

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CN109576658B
CN109576658B CN201811531214.6A CN201811531214A CN109576658B CN 109576658 B CN109576658 B CN 109576658B CN 201811531214 A CN201811531214 A CN 201811531214A CN 109576658 B CN109576658 B CN 109576658B
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CN109576658A (en
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张湉
夏钰东
王红艳
张勇
赵勇
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Southwest Jiaotong University
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    • C23COATING 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
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    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
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    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0623Sulfides, selenides or tellurides

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Abstract

The inventionRelates to the technical field of photoelectrocatalysis materials, in particular to a method for preparing dendritic amorphous MoS based on magnetron sputtering2Method of nano-structuring with MoS2As a target material, a quartz plate is used as a substrate, the target material and the substrate are arranged in a closed environment, the distance between the substrate and the target material is adjusted to 9-12 cm, the included angle between the substrate and the horizontal plane is adjusted to 0-15 degrees, sputtering is started by a direct current sputtering source for 40-90 min, and the dendritic amorphous MoS is obtained2A nanostructure. The invention can effectively reduce the energy of the deposited particles under the mutual cooperation of low air pressure, small angle, low rotating speed, low current, proper target base distance and argon flow, so that the incident particles can be stably grown into the material with the nano structure, and the prepared dendritic amorphous MoS can be used for preparing the nano-structure amorphous MoS2The specific surface area of the nano structure is large, and MoS is improved2The photoelectric property of the photocatalytic material can be widely applied to the field of photocatalytic oxidation reduction.

Description

Preparation of dendritic amorphous MoS based on magnetron sputtering method2Method of nano-structuring
Technical Field
The invention relates to the technical field of photoelectric catalytic materials, in particular to a method for preparing dendritic amorphous MoS based on a magnetron sputtering method2A method of nano-structuring.
Background
With the rapid development of society in the 20 th century, some problems such as energy shortage and environmental pollution have become more and more serious. The semiconductor photocatalytic material has great research value in solving the energy and environmental problems. MoS2The semiconductor material has the characteristics of narrow band gap, two-dimensional layered structure and the like, and has certain practical value in the fields of photocatalysis, aerospace industry and the like. MoS with nano structure compared with common molybdenum disulfide2The photocatalytic material has a large specific surface area, can improve the scattering of light among the nano structures, and increase the absorption effect of the nano materials on light, so that the photocatalytic performance of the photocatalytic material can be effectively improved. MoS2The nanomaterial can be prepared by hydrothermal method, template method, mechanical stripping method, electrochemical stripping method, solvothermal method, fluid dynamic method, ball milling method, and Hum methodThe preparation method comprises a mer method, a steam jet method, an ultrasonic water bath method and the like, but the preparation process of the method is complicated and is inconvenient for large-scale preparation.
In addition, in the existing preparation method of molybdenum disulfide, for example, the preparation method of molybdenum disulfide thin film material disclosed in Chinese patent publication No. CN103205724A uses MoS2The target material is used as a raw material, and MoS is prepared on a substrate by a magnetron sputtering method in an argon and hydrogen sulfide mixed gas environment2The thickness of the molybdenum disulfide film material is 0.1-10.0 μm; the invention has the advantages that: by using Ar gas-H in magnetron sputtering technology2The heating in-situ annealing mode of S mixed gas and substrate can ensure MoS2The film realizes uniform deposition, the S/Mo atomic ratio is kept at 2: 1, the thickness can be effectively increased by increasing the sputtering time, and the MoS is improved2The yield of the nano film is high, but the photoelectric property of the molybdenum disulfide material prepared by the method is poor.
Therefore, the invention provides a dynamic glancing angle deposition technology based on the development of a magnetron sputtering technology, and the amorphous MoS with the dendritic nano structure is prepared2The material effectively improves the photoelectrocatalysis property of the material, can realize large-area large-scale preparation, and has important application value.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for preparing dendritic amorphous MoS based on a magnetron sputtering method2The method of the nanometer structure can effectively reduce the energy of the deposited particles under the mutual cooperation of low pressure, small angle, low rotating speed, low current, proper target base distance and argon flow, so that the incident particles can stably grow into the material with the nanometer structure, and the prepared dendritic amorphous MoS can be used for preparing the nano-structure material2The nanostructure has good photoelectric properties.
The purpose of the invention is realized by the following technical scheme:
preparation of dendritic amorphous MoS based on magnetron sputtering method2Method of nano-structuring with MoS2As the target material, a quartz plate is used as a substrate, the target material and the substrate are arranged in a closed environment, and the substrate and the target are adjustedThe distance between the materials is 9 cm-12 cm, the included angle between the substrate and the horizontal plane is adjusted to 0-15 degrees, then the closed environment is vacuumized, and the air pressure in the closed environment is reduced to 2 multiplied by 10-4When in use, argon is introduced into the closed environment to be used as sputtering gas; then controlling the air pressure of the closed environment to be 0.15 Pa-0.2 Pa, starting sputtering by a direct current sputtering source for 40 min-90 min to obtain the dendritic amorphous MoS2A nanostructure.
Further, the MoS2MoS with the purity of not less than 99.99 percent is adopted2
Further, the quartz plate is firstly subjected to ultrasonic cleaning in acetone, absolute ethyl alcohol and deionized water in sequence, then is dried by blowing with nitrogen, and then is used as a substrate.
Further, the quartz plate is sequentially subjected to ultrasonic cleaning in an acetone solution for 20min, in an absolute ethanol solution for 20min and in a deionized water solution for 5 min.
Further, the substrate is spun during sputtering.
Further, the self-rotation speed of the substrate is 1 r/min.
Further, the sputtering current of the direct current sputtering source is 0.1A.
Further, the flow rate of the argon gas is 12.5sccm to 20 sccm.
Further, the preparation was performed by a magnetron sputtering apparatus.
The invention has the beneficial effects that: the invention provides a magnetron sputtering method based method for preparing dendritic amorphous MoS2The method of the nano structure has low preparation cost, simple preparation process, high sample repeatability and no environmental pollution, and can effectively reduce the energy of deposited particles under the mutual cooperation of low pressure, small angle, low rotating speed, low current, proper target base distance and argon flow, so that incident particles can stably grow into a material with the nano structure, and the prepared dendritic amorphous MoS can be used for preparing the nano-structure2The nano structure has large specific surface area, and the large specific surface area can provide more active sites for the photocatalysis process, thereby effectively improving MoS2The photoelectric property of the photocatalytic material can be widely applied to lightThe field of catalytic oxidation reduction.
Drawings
FIG. 1 shows a dendritic amorphous MoS obtained in test example 1 of the present invention2A 100000 Scanning Electron Microscope (SEM) photograph of the nanostructure;
FIG. 2 shows a dendritic amorphous MoS obtained in test example 1 of the present invention2A 100000 Scanning Electron Microscope (SEM) cross-sectional photograph of the nanostructure;
FIG. 3 shows a dendritic amorphous MoS obtained in test example 1 of the present invention2An ultraviolet-visible light (UV-vis) absorption spectrum of the nanostructure;
FIG. 4 shows a dendritic amorphous MoS obtained in test example 1 of the present invention2Time current density profile of the nanostructure;
FIG. 5 shows dendritic amorphous MoS obtained in test examples 1 and 2 of the present invention2I-V spectra of the nanostructures.
FIG. 6 is a dendritic amorphous MoS of the present invention2Model diagrams of nanostructures.
Detailed Description
The technical solutions of the present invention are further described in detail below with reference to specific embodiments and drawings, but the scope of the present invention is not limited to the following.
Examples
Preparation of dendritic amorphous MoS based on magnetron sputtering method2Method of nano-structuring with MoS2As a target material, a quartz plate is used as a substrate, the target material and the substrate are arranged in a closed environment, the distance between the substrate and the target material is adjusted to 9-12 cm, the included angle between the substrate and the horizontal plane is adjusted to 0-15 degrees, then the closed environment is vacuumized, and the air pressure in the closed environment is reduced to 2 multiplied by 10-4When in use, argon is introduced into the closed environment to be used as sputtering gas; then controlling the air pressure of the closed environment to be 0.15 Pa-0.2 Pa, starting sputtering by a direct current sputtering source for 40 min-90 min to obtain the dendritic amorphous MoS2A nanostructure.
In particular, the MoS2MoS with the purity of not less than 99.99 percent is adopted2(ii) a Sequentially ultrasonically cleaning quartz plates in acetone solution 2Ultrasonic cleaning in absolute ethanol solution for 20min and deionized water solution for 5min for 0 min; the substrate spins automatically in the sputtering process, and the self-rotation speed is 1 r/min; the sputtering current of the direct current sputtering source is 0.1A; the flow rate of the argon is 12.5 sccm-20 sccm.
Test example 1
The preparation method of the test example comprises the following steps:
step one, taking quartz plates with regular shapes and conductive glass as substrate raw materials, sequentially placing the substrate raw materials in acetone and absolute ethyl alcohol solution for ultrasonic cleaning for 20 minutes respectively, then performing ultrasonic cleaning in deionized water for 5 minutes, and drying the surface moisture of the substrate raw materials by using nitrogen to serve as a sample substrate for later use;
step two, MoS with the purity of 99.99%, the diameter of 6cm and the thickness of 5mm is added2Mounting the target material on the target position No. 2 of the magnetron sputtering instrument, fixing the quartz plate and the conductive glass cleaned in the step one on a disc by using a high-temperature adhesive tape, reserving a surface area of 5mm multiplied by 5mm on the conductive glass, fixing the disc on a rotatable substrate table, adjusting the distance between the target base and the disc to be 10cm, and adjusting the included angle between the plane of the disc and the horizontal plane to be 5 degrees;
step three, closing the magnetron sputtering cavity door, opening the mechanical pump, vacuumizing the cavity, opening the electromagnetic valve when the air pressure of the cavity is reduced to 15Pa, opening the molecular pump and the gate valve, and then continuously vacuumizing; when the vacuum degree of the chamber is reduced to 2 x 10-4When in use, an argon gas valve, a stop valve and a substrate spin switch are sequentially opened, argon with the purity of 99.999 percent is introduced as sputtering gas, the flow of the argon gas valve is 12.5sccm, and the substrate self-rotation speed is 1 r/min;
opening a direct current sputtering source, adjusting the sputtering current to be 0.1A, adjusting a gate valve to enable the sputtering air pressure to be 0.15Pa, and performing sputtering for 60 minutes;
step five, after sputtering is finished, a sputtering power supply, a stop valve, an argon gas valve, a substrate spin switch, a gate valve, a molecular pump, an electromagnetic valve and a mechanical pump are sequentially closed, nitrogen is introduced to open a cavity door, and a sample is taken out to obtain the dendritic amorphous MoS2Nano structure, for maintenance of magnetron sputtering instrument, the cavity needs to be re-filledA vacuum is drawn.
Test example 2
The preparation method of the test example comprises the following steps:
taking a quartz plate and conductive glass as substrate raw materials, sequentially placing the substrate raw materials in acetone and absolute ethyl alcohol solutions, respectively carrying out ultrasonic cleaning for 20 minutes, then carrying out ultrasonic cleaning for 5 minutes in deionized water, and drying the surface moisture of the substrate with nitrogen to be used as a sample substrate for later use;
step two, MoS with the purity of 99.99%, the diameter of 6cm and the thickness of 5mm is added2The target material is arranged at the position of the target of the magnetron sputtering instrument No. 2, the quartz plate cleaned in the step one and the conductive glass are fixed on the disc by using an adhesive tape, the surface area of 5mm multiplied by 5mm is reserved on the conductive glass, the disc is fixed on a rotatable substrate table, the distance between the target substrate and the disc is adjusted to be 10cm, and the included angle between the plane of the disc and the horizontal plane is 15 degrees;
step three, closing the magnetron sputtering cavity door, opening the mechanical pump, vacuumizing the cavity, opening the electromagnetic valve when the air pressure of the cavity is reduced to 15Pa, opening the molecular pump and the gate valve, and then continuously vacuumizing; when the vacuum degree of the chamber is reduced to 2 x 10-4When in use, an argon gas valve, a stop valve and a substrate spin switch are sequentially opened, argon with the purity of 99.999 percent is introduced as sputtering gas, the flow of the argon gas valve is 12.5sccm, and the substrate self-rotation speed is 1 r/min;
opening a direct current sputtering source, adjusting the sputtering current to be 0.1A, adjusting a gate valve to enable the sputtering air pressure to be 0.15Pa, and performing sputtering for 40 minutes;
step five, after sputtering is finished, a sputtering power supply, a stop valve, an argon gas valve, a substrate spin switch, a gate valve, a molecular pump, an electromagnetic valve and a mechanical pump are sequentially closed, nitrogen is introduced to open a cavity door, and a sample is taken out to obtain the dendritic amorphous MoS2A nanostructure.
And sixthly, in order to maintain the magnetron sputtering instrument, vacuumizing the cavity again.
Test example 3
The preparation method of the test example comprises the following steps:
taking a quartz plate and conductive glass as substrate raw materials, sequentially placing the substrate raw materials in acetone and absolute ethyl alcohol solutions, respectively carrying out ultrasonic cleaning for 20 minutes, then carrying out ultrasonic cleaning for 5 minutes in deionized water, and drying the surface moisture of the substrate with nitrogen to be used as a sample substrate for later use;
step two, MoS with the purity of 99.99%, the diameter of 6cm and the thickness of 5mm is added2Mounting the target material on a target position No. 2 of a magnetron sputtering instrument, fixing the quartz plate and the conductive glass cleaned in the step one on a disc by using an adhesive tape, reserving a surface area of 5mm multiplied by 5mm on the conductive glass, fixing the disc on a rotatable substrate table, adjusting the distance between the target base and the substrate to be 10cm, and adjusting the included angle between the plane of the disc and the horizontal plane to be 5 degrees;
step three, closing the magnetron sputtering cavity door, opening the mechanical pump, vacuumizing the cavity, opening the electromagnetic valve when the air pressure of the cavity is reduced to 15Pa, opening the molecular pump and the gate valve, and then continuously vacuumizing; when the vacuum degree of the chamber is reduced to 2 x 10-4When in use, an argon gas valve, a stop valve and a substrate spin switch are sequentially opened, argon with the purity of 99.999 percent is introduced as sputtering gas, the flow of the argon gas valve is 15sccm, and the substrate spin speed is 1 r/min;
opening a direct current sputtering source, adjusting the sputtering current to be 0.1A, adjusting a gate valve to enable the sputtering air pressure to be 0.2Pa, and performing sputtering for 60 minutes;
step five, after sputtering is finished, a sputtering power supply, a stop valve, an argon gas valve, a substrate spin switch, a gate valve, a molecular pump, an electromagnetic valve and a mechanical pump are sequentially closed, nitrogen is introduced to open a cavity door, and a sample is taken out to obtain the dendritic amorphous MoS2A nanostructure.
In order to maintain the magnetron sputtering instrument, the cavity needs to be evacuated again.
Test example 4
The preparation method of the test example comprises the following steps:
taking a quartz plate and conductive glass as substrate raw materials, sequentially placing the substrate raw materials in acetone and absolute ethyl alcohol solutions, respectively carrying out ultrasonic cleaning for 20 minutes, then carrying out ultrasonic cleaning for 5 minutes in deionized water, and drying the surface moisture of the substrate with nitrogen to be used as a sample substrate for later use;
step two, MoS with the purity of 99.99%, the diameter of 6cm and the thickness of 5mm is added2The target material is arranged at the position of the target of the magnetron sputtering instrument No. 2, the quartz plate and the conductive glass cleaned in the step one are fixed on a disc by using an adhesive tape, the surface area of 5mm multiplied by 5mm is reserved on the conductive glass, the disc is fixed on a rotatable sample table, the target base distance is adjusted to be 9cm, and the included angle between the plane of the disc and the horizontal plane is 5 degrees;
step three, closing the magnetron sputtering cavity door, opening the mechanical pump, vacuumizing the cavity, opening the electromagnetic valve when the air pressure of the cavity is reduced to 15Pa, opening the molecular pump and the gate valve, and then continuously vacuumizing; when the vacuum degree of the chamber is reduced to 2 x 10-4When in use, an argon gas valve, a stop valve and a substrate spin switch are sequentially opened, high-purity argon gas is introduced as sputtering gas, the flow of the argon gas valve is 20sccm, and the substrate spin speed is 1 r/min;
opening a direct current sputtering source, adjusting the sputtering current to be 0.1A, adjusting a gate valve to enable the sputtering air pressure to be 0.2Pa, and performing sputtering for 50 minutes;
step five, after sputtering is finished, a sputtering power supply, a stop valve, an argon gas valve, a substrate spin switch, a gate valve, a molecular pump, an electromagnetic valve and a mechanical pump are sequentially closed, nitrogen is introduced to open a cavity door, and a sample is taken out to obtain the dendritic amorphous MoS2And the nano structure is used for maintaining the magnetron sputtering instrument, and the cavity needs to be vacuumized again.
Test example 5
The preparation method of the test example comprises the following steps:
step one, taking quartz plates with regular shapes and conductive glass as substrate raw materials, sequentially placing the substrate raw materials in acetone and absolute ethyl alcohol solution, respectively carrying out ultrasonic cleaning for 20 minutes, then carrying out ultrasonic cleaning in deionized water for 5 minutes, and drying surface moisture by using nitrogen to serve as a sample substrate for later use;
step two, MoS with the purity of 99.99%, the diameter of 6cm and the thickness of 5mm is added2The target material is arranged at the No. 2 target position of the magnetron sputtering instrument, and the quartz plate and the conductive glass which are cleaned in the step one are usedFixing the glass on a disc by using a high-temperature adhesive tape, reserving a surface area of 5mm multiplied by 5mm for the conductive glass, fixing the disc on a rotatable sample table, adjusting the target base distance to be 12cm, and adjusting the included angle between the plane of the disc and the horizontal plane to be 3 degrees;
step three, closing the magnetron sputtering cavity door, opening the mechanical pump, vacuumizing the cavity, opening the electromagnetic valve when the air pressure of the cavity is reduced to 15Pa, opening the molecular pump and the gate valve, and then continuously vacuumizing; when the vacuum degree of the chamber is reduced to 2 x 10-4When in use, an argon gas valve, a stop valve and a substrate spin switch are sequentially opened, argon with the purity of 99.999 percent is introduced as sputtering gas, the flow of the argon gas valve is 12.5sccm, and the substrate self-rotation speed is 1 r/min;
opening a direct current sputtering source, adjusting the sputtering current to be 0.1A, adjusting a gate valve to enable the sputtering air pressure to be 0.15Pa, and performing sputtering for 90 minutes;
step five, after sputtering is finished, a sputtering power supply, a stop valve, an argon gas valve, a substrate spin switch, a gate valve, a molecular pump, an electromagnetic valve and a mechanical pump are sequentially closed, nitrogen is introduced to open a cavity door, and a sample is taken out to obtain the dendritic amorphous MoS2And the nano structure is used for maintaining the magnetron sputtering instrument, and the cavity needs to be vacuumized again.
Testing and characterization of photocatalytic materials:
the types of magnetron sputtering apparatuses used in the test examples were: SKY-450 type magnetron sputtering instrument. The dendritic amorphous MoS obtained in test examples 1 and 2 was collected2Nanostructure, scanning Electron microscopy on the dendritic amorphous MoS obtained in test example 12The surface morphology and the cross-sectional nanostructure of the nanostructure were characterized and the results are shown in fig. 1 and fig. 2, respectively; then, the dendritic amorphous MoS prepared in test example 1 was subjected to UV-6300 type UV-visible spectrophotometer2The nano structure is subjected to an absorption spectrum experiment, and the optical property of the nano structure is characterized, and the result is shown in fig. 3 and 4; 1mol/L sulfuric acid electrolyte was prepared, and an electrochemical workstation was used to test the dendritic amorphous MoS prepared in examples 1 and 22The nanostructure was subjected to an I-V test, and the test results are shown in fig. 5, which characterizes its electrical properties. FIG. 1 shows the sputtering angle at 5 degTo obtain the dendritic amorphous MoS2Surface view of the nanostructure, FIG. 2 is the dendritic amorphous MoS obtained at a sputtering angle of 5 °2Sectional view of the nanostructure, FIG. 3 is a dendritic amorphous MoS2The absorption spectrum of the nanostructure in the wavelength range of 200nm-1000nm, FIG. 4 is the dendritic amorphous MoS2Time current density curve of the nanostructure under 0V voltage, FIG. 5 is dendritic amorphous MoS with sputtering angles of 5 and 15 °2I-V plot of nanostructures, FIG. 6 is a dendritic amorphous MoS of the invention2Model diagram of the nanostructure, it can be seen that there is a dendritic amorphous MoS2The nano structure can absorb visible light, has sensitive and stable light response and good photoelectric property.
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (5)

1. Preparation of dendritic amorphous MoS based on magnetron sputtering method2Method for producing nanostructures, characterized in that the nanostructures are produced as MoS2As a target material, a quartz plate is used as a substrate, the target material and the substrate are arranged in a closed environment, the distance between the substrate and the target material is adjusted to be 9-12 cm, the included angle between the substrate and the horizontal plane is adjusted to be 5 degrees, then the closed environment is vacuumized, and the air pressure in the closed environment is reduced to 2 multiplied by 10-4When in use, argon is introduced into the closed environment to be used as sputtering gas; then controlling the air pressure of the closed environment to be 0.15-0.2 Pa, and performing magnetron sputtering by a direct-current sputtering source for 40-90 min to obtain the dendritic amorphous MoS2A nanostructure; the MoS2MoS with the purity of not less than 99.99 percent is adopted2(ii) a The quartz plate is firstly ultrasonically cleaned in acetone, absolute ethyl alcohol and deionized water in sequence, then is dried by nitrogen,then used as a substrate; the substrate spins in the sputtering process, and the spin speed of the substrate is 1 r/min.
2. The method of claim 1 for preparing dendritic amorphous MoS based on magnetron sputtering2The method for preparing the nano structure is characterized in that the quartz plate is ultrasonically cleaned in an acetone solution for 20min, an absolute ethyl alcohol solution for 20min and deionized water for 5min in sequence.
3. The method of claim 1 for preparing dendritic amorphous MoS based on magnetron sputtering2A method of nanostructures, wherein the dc sputtering source has a sputtering current of 0.1A.
4. The method of claim 1 for preparing dendritic amorphous MoS based on magnetron sputtering2The method for preparing the nano structure is characterized in that the flow of the argon is 12.5 sccm-20 sccm.
5. The method of claim 1 for preparing dendritic amorphous MoS based on magnetron sputtering2A method of making a nanostructure, characterized in that the preparation is performed by a magnetron sputtering apparatus.
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CN103205724A (en) * 2013-04-23 2013-07-17 南开大学 Preparation method of molybdenum disulfide film material
CN104278241B (en) * 2013-07-02 2017-10-31 中国科学院兰州化学物理研究所 A kind of technology of preparing of the thin-film material with multi-environment adaptability
US20150345010A1 (en) * 2013-09-30 2015-12-03 University Of Dayton Methods of magnetically enhanced physical vapor deposition
CN106206254A (en) * 2016-07-13 2016-12-07 合肥工业大学 There is the preparation method of the large-area two-dimensional stratified material of excellent photoluminescence property
CN108220896B (en) * 2016-12-14 2020-02-18 有研工程技术研究院有限公司 cupronickel/Ni-MoS with ultralow friction coefficient2Composite material and preparation method thereof
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JPH01290776A (en) * 1988-05-18 1989-11-22 Tokico Ltd Composite plating method

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