CN108899267B - Preparation method of metal-doped molybdenum disulfide film - Google Patents
Preparation method of metal-doped molybdenum disulfide film Download PDFInfo
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 11
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- 238000000576 coating method Methods 0.000 claims abstract description 6
- 230000001678 irradiating effect Effects 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 32
- 239000002243 precursor Substances 0.000 claims description 26
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 9
- 150000002751 molybdenum Chemical class 0.000 claims description 9
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 5
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 3
- 229940010552 ammonium molybdate Drugs 0.000 claims description 3
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 3
- 239000011609 ammonium molybdate Substances 0.000 claims description 3
- 239000010410 layer Substances 0.000 claims description 3
- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical group [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 229910052594 sapphire Inorganic materials 0.000 claims description 2
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- 239000000463 material Substances 0.000 abstract description 10
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 14
- 239000010409 thin film Substances 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 7
- GICWIDZXWJGTCI-UHFFFAOYSA-I molybdenum pentachloride Chemical compound Cl[Mo](Cl)(Cl)(Cl)Cl GICWIDZXWJGTCI-UHFFFAOYSA-I 0.000 description 5
- 238000004528 spin coating Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000005693 optoelectronics Effects 0.000 description 3
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- 239000010931 gold Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910019964 (NH4)2MoS4 Inorganic materials 0.000 description 1
- 101100069231 Caenorhabditis elegans gkow-1 gene Proteins 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
- H01L21/02557—Sulfides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02623—Liquid deposition
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0296—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe
- H01L31/02963—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe characterised by the doping material
Abstract
The invention belongs to the field of semiconductor film material preparation, and particularly relates to a preparation method of a metal-doped molybdenum disulfide film material. And coating a mixed solution containing a sulfur source, a molybdenum source and a metal element to be doped on a substrate, and irradiating the surface of the substrate coated with the mixed solution by adopting laser under a vacuum condition to prepare the metal-doped molybdenum disulfide film. The preparation method can realize the one-step completion of the growth and doping of the molybdenum sulfide. The molybdenum disulfide film doped with the metal prepared by the method has good uniformity and large area, and the doping concentration can be adjusted according to the concentration of the metal salt solution. The control of the crystal morphology can be realized by changing the power, spot size and pulse number of the laser radiation. The preparation method is easy to operate, high in repetition rate, short in preparation time and high in efficiency.
Description
Technical Field
The invention belongs to the field of semiconductor film material preparation, and particularly relates to a preparation method of a metal-doped molybdenum disulfide film material.
Background
In recent years, two-dimensional layered nanomaterials have attracted much attention because of their excellent properties in electrical, mechanical, optical, thermal, etc., such as graphene, h-BN, transition metal sulfides, etc. Molybdenum disulfide (MoS2) as a representative of transition metal sulfides has high carrier mobility, good thermal stability, high electrical conductivity, good mechanical properties, high specific surface area, excellent semiconductor properties, and a controllable band gap, and thus has great potential in applications of optoelectronic devices. The PN junction is the most basic structure of the optoelectronic device, and the MoS2 thin film prepared by a Chemical Vapor Deposition (CVD) method belongs to natural weak n-property, so that p-type doping of MoS2 becomes an important problem to be solved urgently in the development of two-dimensional optoelectronic devices. Currently, MoS2 doping approaches mainly include displacement doping during growth, surface charge transfer, layer-dependent effect, and plasma implantation, and the most common of these approaches is displacement doping during growth, which mainly includes Chemical Vapor Deposition (CVD) and Chemical Vapor Transport (CVT). MoS2 is prepared by CVD by thermally evaporating a solid source, such as MoO3/S powder or (NH4)2MoS4, and then reaction depositing to form a thin film on a substrate. The carrier type and carrier density can be regulated and controlled by controlling the components of the precursor in the CVD process. The chemical vapor transport method can also realize the doping of the molybdenum sulfide.
Although the doping of MoS2 can be realized by placing the doping in the growth process, the controllability of the doping is still to be further improved, the selection of the doped region is difficult to realize by placing the doping in the growth process, and meanwhile, the doping method has high requirements on temperature and harsh preparation conditions.
Disclosure of Invention
Aiming at the defects or the improvement requirements of the prior art, the invention provides a preparation method of a metal-doped molybdenum disulfide film, which aims to realize one-step completion of molybdenum sulfide growth and doping by a laser method, thereby solving the technical problems of poor controllability, harsh doping conditions and the like of the metal-doped molybdenum disulfide in the prior art.
In order to achieve the above object, according to one aspect of the present invention, a method for preparing a metal-doped molybdenum disulfide thin film is provided, in which a mixed solution containing a sulfur source, a molybdenum source, and a metal element to be doped is coated on a substrate, and the surface of the substrate coated with the mixed solution is irradiated with laser under a vacuum condition to prepare the metal-doped molybdenum disulfide thin film.
Preferably, the laser energy is 30-2000J/cm2And the thickness of the prepared metal-doped molybdenum disulfide film is 5-20 nm.
Preferably, the preparation method specifically comprises the following steps:
(1) dissolving thiourea and molybdenum salt in an alcohol solvent, wherein the molar ratio of sulfur to molybdenum is 20: 1-5: 1, and obtaining a precursor solution;
(2) mixing a metal salt solution with the precursor solution in the step (1), and coating the mixture on a substrate to obtain the substrate coated with the precursor solution, wherein the concentration of the metal salt is 1-15 mmol/L;
(3) placing the substrate coated with the precursor solution in a vacuum chamber, and irradiating the surface of the substrate coated with the mixed solution by using laser, wherein the laser energy is 30-2000J/cm2And preparing the metal-doped molybdenum disulfide film with the thickness of 5-20 nm.
Preferably, the alcoholic solvent is isopropanol or ethanol.
Preferably, the molybdenum salt is molybdenum chloride or ammonium molybdate.
Preferably, in the step (1), the thiourea and the molybdenum salt are dissolved in the alcohol solvent by stirring for 0.8 to 1.5 hours at the temperature of 60 to 100 ℃ and the rotation speed of 1500 to 2000 r/min.
Preferably, the concentration of sulfur in the precursor solution is 15-25 g/L, and the concentration of molybdenum is 4-12 g/L.
Preferably, the substrate is a silicon wafer with an oxide layer, quartz, sapphire or ceramic.
Preferably, the laser in step (3) is a continuous laser or a pulsed laser.
Preferably, the laser in the step (3) is pulse laser, the laser power is 150-350 mJ, the radiation frequency is 3-8 Hz, the number of pulses is 1000-2500 times, the spot size is 3mm × 3mm, and the laser moving speed is 2-4 mm/s.
Preferably, the metal salt solution is one or more of gold chloride, silver nitrate and copper nitrate.
In general, compared with the prior art, the above technical solution contemplated by the present invention can achieve the following beneficial effects:
(1) the invention realizes the growth of molybdenum sulfide and the doping of metal by adopting a laser method. The laser method can realize the selection of the doped region by changing the incident position of laser, and can regulate and control the size of the prepared film by changing the power of laser radiation, the size of light spots and the number of pulses; the preparation method of the metal-doped molybdenum disulfide film has good controllability.
(2) The molybdenum disulfide film obtained by the method has good uniformity and large area, and the doping concentration can be adjusted according to the concentration of the metal salt solution.
(3) The preparation method of the metal-doped molybdenum disulfide film is simple and convenient, easy to operate, high in repetition rate, short in preparation time and high in efficiency, and can realize synchronous growth and doping.
Drawings
FIG. 1 is a schematic diagram of an experimental apparatus for preparing a metal-doped molybdenum-disulfide thin film material, in which 1 is a laser source, 2 is a substrate, 3 is a vacuum cavity, and 4 is a laser window.
FIG. 2 is an XPS plot of the gold-doped molybdenum disulfide thin film material prepared in example 1, wherein FIG. 2(a) shows the Mo photoelectron peak and FIG. 2(b) shows the S photoelectron peak; FIG. 2(c) shows the peak of Au photoelectrons.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention provides a preparation method of a metal-doped molybdenum disulfide film, which containsAnd coating a mixed solution of a sulfur source, a molybdenum source and a metal element to be doped on the substrate, and irradiating the surface of the substrate coated with the mixed solution by adopting laser under a vacuum condition to prepare the metal-doped molybdenum disulfide film. The laser energy is 30-2000J/cm2And the thickness of the prepared metal-doped molybdenum disulfide film is 5-20 nm.
The preparation method specifically comprises the following steps:
(1) thiourea and molybdenum salt are dissolved in an alcohol solvent, wherein the molar ratio of sulfur to molybdenum is 20: 1-5: 1, a precursor solution is obtained, the molybdenum salt is molybdenum chloride or ammonium molybdate, the alcohol solvent is isopropanol or ethanol, and the thiourea and the molybdenum salt are preferably dissolved in the alcohol solvent by stirring for 0.8-1.5 hours at the temperature of 60-100 ℃ and the rotating speed of 1500-2000 r/min, the concentration of the sulfur in the precursor solution is 15-25 g/L, the concentration of the molybdenum in the precursor solution is 4-12 g/L, and the control of the growth size of the molybdenum sulfide film is realized by adjusting the concentration ratio of the sulfur to the molybdenum.
(2) Mixing a metal salt solution with the precursor solution in the step (1), and coating the mixture on a substrate to obtain the substrate coated with the precursor solution, wherein the metal salt solution can be one or more of gold chloride, silver nitrate and copper nitrate, the concentration of the metal salt determines the doping concentration of metal in molybdenum disulfide, and the doping concentration can be 1-15 mmol/L2For example, the substrate is generally cleaned before use, and the substrate may be first ultrasonically cleaned with acetone, then ultrasonically cleaned with alcohol to remove organic matters and impurities on the surface of the substrate, finally ultrasonically cleaned again with deionized water and dried to obtain a clean substrate for later use.
(3) Placing the substrate coated with the precursor solution in a vacuum chamber, and irradiating the surface of the substrate coated with the mixed solution by using laser, wherein the laser energy is 30-2000J/cm2And preparing the metal-doped molybdenum disulfide film with the thickness of 5-20 nm. The laser may be a continuous laser or a pulsed laser. When the laser is a pulse laser, the preferred laser power is 150-350 mJ, and the radiation frequency is 3-up to8Hz, the number of pulses is 1000-2500 times, the size of a light spot is 3mm, × 3mm and the moving speed of the laser is 2-4 mm/s.
The invention provides a method for promoting the growth of molybdenum disulfide and the doping of metal by utilizing laser energy excitation, the laser energy is controllable, the laser energy can be specifically adjusted by controlling laser power, radiation frequency, spot size, laser moving speed, laser incidence angle and the like, and parameters such as pulse times and the like can be adjusted if the laser is a pulse laser, the position of laser radiation is adjusted, the controllable doping of a target area is realized, and the controllability is better compared with the existing CVD doping method. Proper laser energy is crucial to the preparation of metal-doped molybdenum disulfide films, and the laser energy is not too small, otherwise molybdenum disulfide cannot be obtained or doping cannot be realized, but too large laser energy may cause damage to the films and the integrity is damaged. The invention controls the laser radiation energy to be 30-2000J/cm2The concentration range of the metal solution is 1-15 mmol/L, a metal-doped molybdenum disulfide film with the thickness of 5-20 nm can be prepared,
one preferred preparation method is as follows:
(1) using a substrate of SiO2And the silicon wafer is firstly ultrasonically cleaned by acetone, then ultrasonically cleaned by alcohol to remove organic matters and impurities on the surface of the substrate, finally ultrasonically cleaned again by deionized water and dried to obtain a clean substrate for later use. Adding 200mg of thiourea into a flask, then adding 20-120 mg of molybdenum pentachloride and 3.75ml of isopropanol, and magnetically stirring for 0.8-1.5 hours at the rotating speed of 1500-2000 r/min and the temperature of 60-100 ℃.
(2) Uniformly mixing 0.1-0.3 ml of precursor solution drop with 0.1ml of metal salt solution with the molar concentration of 1-15 mmol/L, uniformly spin-coating the mixture on a substrate, then placing the substrate in a vacuum chamber, and radiating the substrate by using pulse laser through a laser window, wherein the laser power is 150-350 mJ, the radiation frequency is 3-8 Hz, the pulse number is 1000-2500 times, the spot size is 3mm × 3mm, and the laser moving speed is 2-4 mm/s.
(3) And after the laser radiation is finished, taking the substrate out of the vacuum cavity to obtain the metal-doped molybdenum disulfide film material.
Fig. 1 shows a schematic diagram of an experimental apparatus for preparing a metal-doped molybdenum disulfide thin film material, wherein 1 is a laser source, 2 is a substrate, 3 is a vacuum cavity, and 4 is a laser window. The incident direction of the laser source and the surface of the substrate form a certain included angle, and the included angle is larger than 0 degree and is preferably 90 degrees.
The following are examples:
example 1
Adding 200mg of thiourea, 80mg of molybdenum pentachloride and 3.75ml of isopropanol into a flask, magnetically stirring for 1 hour to obtain a precursor solution, wherein the rotation speed of magnetic stirring is 1800r/min, the temperature is 80 ℃, taking 0.1ml of the precursor solution and 0.1ml of gold chloride solution with the molar concentration of 5 mmol/L to be fully mixed, uniformly spin-coating the mixture on a substrate, then placing the substrate into a vacuum chamber, and radiating the substrate by using pulse laser through a laser window, wherein the schematic diagram of the device is shown in figure 1, the laser power is set to be 250mJ, the radiation frequency is 3Hz, the pulse number is 2000 times, the spot size is 3mm × 3mm, the laser moving speed is 3mm/s, and after the laser radiation is finished, taking out the substrate from the vacuum chamber to obtain the gold-doped molybdenum disulfide film.
FIG. 2 is an XPS plot of the gold-doped molybdenum disulfide thin film material prepared in example 1, and FIG. 2(a) is a photoelectron peak of Mo, consisting of two peaks with binding energies of 234.5eV and 231.4eV, respectively, corresponding to tetravalent molybdenum ion (Mo)4+) Mo3d3/2And Mo3d5/2FIG. 2(b) shows the photoelectron peak (S) of S2-) Also composed of two peaks, respectively S2p with a binding energy of 162.1eV2/3And S2p with a binding energy of 163.2eV1/2Two peaks, the sample prepared can be judged to be MoS 2. FIG. 2(c) shows the peak of Au photoelectrons, which is represented by Au4f having a binding energy of 88.1eV5/2And Au4f with binding energy of 84.0eV7/2Two peaks in composition, indicating the preparation of a gold-doped molybdenum disulfide material.
Example 2
Adding 200mg of thiourea, 60mg of molybdenum pentachloride and 3.75ml of isopropanol into a flask, magnetically stirring for 1.5 hours to obtain a precursor solution, wherein the rotation speed of magnetic stirring is 1600r/min, the temperature is 80 ℃, taking 0.1ml of the precursor solution and 0.1ml of gold chloride solution with the molar concentration of 1 mmol/L to be fully mixed, uniformly spin-coating the mixture on a substrate, then placing the substrate into a vacuum chamber, radiating the substrate by using pulse laser through a laser window, setting the laser power to be 250mJ, the radiation frequency to be 3Hz, the pulse number to be 2500 times, setting the light spot size to be 3mm, × 3mm, and taking out the substrate from the vacuum chamber after the laser moving speed is 3 mm/s.
Example 3
Adding 200mg of thiourea, 120mg of molybdenum pentachloride and 3.75ml of isopropanol into a flask, magnetically stirring for 1 hour to obtain a precursor solution, wherein the rotating speed of magnetic stirring is 1800r/min, the temperature is 60 ℃, taking 0.1ml of the precursor solution to be fully mixed with 0.1ml of silver nitrate solution with the molar concentration of 1 mmol/L, uniformly spin-coating the mixture on a substrate, then placing the substrate into a vacuum cavity, radiating the substrate by using pulse laser through a laser window, setting the laser power to be 350mJ, the radiation frequency to be 5Hz, the pulse number to be 2000 times, the spot size to be 3mm, × 3mm, and taking out the substrate from the vacuum cavity after the laser moving speed is 3 mm/s.
Example 4
Adding 200mg of thiourea, 80mg of molybdenum pentachloride and 3.75ml of isopropanol into a flask, magnetically stirring for 1.5 hours to obtain a precursor solution, wherein the rotation speed of the magnetic stirring is 1800r/min, the temperature is 80 ℃, taking 0.1ml of the precursor solution and 0.1ml of copper nitrate solution with the molar concentration of 15 mmol/L to be fully mixed, uniformly spin-coating the mixture on a substrate, then placing the substrate into a vacuum chamber, radiating the substrate by using pulse laser through a laser window, setting the laser power to be 150mJ, the radiation frequency to be 3Hz, the pulse number to be 2000 times, setting the light spot size to be 3mm, × 3mm, and taking out the substrate from the vacuum chamber after the laser radiation is finished, thus obtaining the copper-doped molybdenum disulfide film.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of a metal-doped molybdenum disulfide film is characterized by coating a mixed solution containing a sulfur source, a molybdenum source and a metal element to be doped on a substrate, and irradiating the surface of the substrate coated with the mixed solution by adopting laser under a vacuum condition to prepare the metal-doped molybdenum disulfide film.
2. The method according to claim 1, wherein the laser energy is 30 to 2000J/cm2And the thickness of the prepared metal-doped molybdenum disulfide film is 5-20 nm.
3. The method of claim 1, wherein the step of applying the mixed solution comprises:
(1) dissolving thiourea and molybdenum salt in an alcohol solvent, wherein the molar ratio of sulfur to molybdenum is 20: 1-5: 1, and obtaining a precursor solution;
(2) mixing a metal salt solution with the precursor solution in the step (1), and coating the mixture on a substrate to obtain the substrate coated with the precursor solution, wherein the concentration of the metal salt is 1-15 mmol/L;
(3) placing the substrate coated with the precursor solution in a vacuum chamber, and irradiating the surface of the substrate coated with the mixed solution by using laser, wherein the laser energy is 30-2000J/cm2And preparing the metal-doped molybdenum disulfide film with the thickness of 5-20 nm.
4. The method of claim 3, wherein the molybdenum salt is molybdenum chloride or ammonium molybdate.
5. The method according to claim 3, wherein the thiourea and the molybdenum salt are dissolved in the alcohol solvent by stirring in the step (1) at a temperature of 60 to 100 ℃ and a rotation speed of 1500 to 2000r/min for 0.8 to 1.5 hours.
6. The method according to claim 3, wherein the concentration of sulfur in the precursor solution is 15 to 25 g/L, and the concentration of molybdenum is 4 to 12 g/L.
7. The method according to claim 3, wherein the substrate is a silicon wafer having an oxide layer, quartz, sapphire, or ceramic.
8. The method according to claim 3, wherein the laser in the step (3) is a continuous laser or a pulsed laser.
9. The preparation method according to claim 3, wherein the laser in the step (3) is a pulse laser, the laser power is 150 to 350mJ, the radiation frequency is 3 to 8Hz, the number of pulses is 1000 to 2500 times, the spot size is 3mm × 3mm, and the laser moving speed is 2 to 4 mm/s.
10. The method of claim 3, wherein the metal salt solution is one or more of gold chloride, silver nitrate, and copper nitrate.
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