CN109455675B - Preparation method of sulfur vacancy of transition metal sulfide nanosheet - Google Patents

Preparation method of sulfur vacancy of transition metal sulfide nanosheet Download PDF

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CN109455675B
CN109455675B CN201811428631.8A CN201811428631A CN109455675B CN 109455675 B CN109455675 B CN 109455675B CN 201811428631 A CN201811428631 A CN 201811428631A CN 109455675 B CN109455675 B CN 109455675B
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drying
sulfide
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pmma
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CN109455675A (en
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张跃
高丽
张铮
廖庆亮
高放放
张先坤
柳柏杉
杜君莉
于慧慧
洪孟羽
欧洋
肖建坤
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University of Science and Technology Beijing USTB
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G1/00Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
    • C01G1/12Sulfides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/20Methods for preparing sulfides or polysulfides, in general
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00Selenium; Tellurium; Compounds thereof
    • C01B19/007Tellurides or selenides of metals
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/288Sulfides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00Compounds of molybdenum
    • C01G39/06Sulfides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00Compounds of tungsten
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    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention belongs to the field of defect regulation and control, and relates to a simple, mild and accurate preparation method of a transition metal group sulfide nanosheet sulfur vacancy of the transition metal group sulfide sulfur vacancy. Transferring the prepared transition metal sulfide nanosheet to a substrate which can be firmly bonded with the transition metal sulfide nanosheet, soaking the nanosheet in a prepared weakly oxidizing solution, washing the residual solution with DI water, and drying the washed residual solution with a hot plate. By utilizing the matching of the electron induction of weak oxidizing ions and the formation energy of sulfur vacancies of the sulfide of the transition metal group, the construction of the sulfur vacancies can be accurately realized without introducing other types of defects. Furthermore, this approach does not cause local material wrinkling and breakage as compared to conventional physical defect control strategies. The sulfur vacancies in transition metal group sulfides can be manipulated over a large area. And meanwhile, the method is compatible with the traditional CMOS process. Therefore, the method has great significance for exploring the characteristic regulation and control of sulfur vacancies in the transition metal sulfide and promoting the application of defect engineering.

Description

Preparation method of sulfur vacancy of transition metal sulfide nanosheet
Technical Field
The invention belongs to the field of defect regulation and control, and relates to a simple, mild and accurate preparation method of a transition metal group sulfide nanosheet sulfur vacancy of the transition metal group sulfide sulfur vacancy.
Background
The 2004 discovery of graphene opened the door to the development of two-dimensional materials. Graphene is a two-dimensional material with a single carbon atom layer, and has ultrahigh carrier mobility and thermal conductivity and excellent mechanical strength. But the zero band gap of graphene greatly limits its development. Transition metal group Sulfides (TMDCs) which have appeared at the same time are also a layered material which can be exfoliated. Has certain band gap and different electrical properties, including insulator, semiconductor, semimetal, metal and superconductor. The method has great development and application space in the fields of electronics, photoelectron, catalysis, energy storage and conversion, sensing, biomedicine and the like. Studies have shown that transition metal group sulphides possess abundant crystal structures, and that most of these abundant crystal structures are caused by defects. Common defects include vacancy defects, inversion defects, clusters, grain boundaries, and boundary reconstruction. The defects can reduce the barrier height of the gold semi-contact to a certain extent, adjust the carrier type and transport, enhance the optical, ferroelectric and catalytic properties and the like. Therefore, the deep understanding and research of the defects have great significance on the regulation and control of the properties of the transition metal group sulfide.
The current regulating and controlling means of the transition metal sulfide defects mainly comprise ion beam/electron beam excitation, plasma etching, ultrahigh vacuum thermal annealing, a stoichiometric control method, a sulfur vacancy self-repairing method, stretching deformation control and the like. It can be seen that most common defect control means are physical methods. The defects regulated and controlled by the methods often belong to a multi-type defect system, and in addition, the physical means are very easy to damage materials to different degrees; the plasma etching, the stretching method and the like are incompatible with the traditional CMSO process; furthermore, most physical methods that have been found are difficult to achieve large area modulation of defects; the high requirement on equipment and poor controllability are also one of the important reasons for limiting the development of the equipment. Most importantly, the defects of multiple types seriously mislead the understanding of the same type on the missing item regulation and control performance, and restrict the development of defect engineering.
We therefore propose a mild and precise liquid phase chemistry strategy to prepare sulfur vacancies in transition metal group sulfide nanosheets. The liquid phase chemical preparation process is simple and effective, the regulation and control of the sulfur vacancy are mild, and only TMDC is preparedSThe sulfur vacancy in the material has no other defects, simultaneously, the preparation of large-area sulfur vacancy can be carried out, the material of the transition metal group sulfide has no destructiveness, the local folds and damages of the material can not be caused, and the material is compatible with the traditional CMOS process, so the defect of traditional defect regulation and control is effectively avoided, and the purpose of accurately preparing the defect is achieved.
Disclosure of Invention
The invention aims to provide a method for preparing sulfur vacancies of transition metal sulfide nanosheets by a liquid phase chemical method. The process aims to get rid of the traditional physical defect regulation and control means which is destructive to materials, incompatible with the traditional CMOS process and uncontrollable in defect types, and provides a simple, mild, accurate and effective sulfur vacancy preparation strategy by a liquid phase chemical method.
In order to achieve the purpose, the technical scheme of the invention is as follows: a method for constructing sulfur vacancies of sulfide nanosheets of transition metal groups comprises the following specific steps:
s1: transferring the selected transition metal group sulfide nanosheets to a target substrate which is not reacted with a weak oxidizing solution and can be in firm contact with the transition metal group sulfide nanosheets for later use;
s2: diluting the weak oxidizing solution to a weak oxidizing aqueous solution with a certain concentration, and placing the weak oxidizing aqueous solution in a brown light-proof stripping container for later use;
s3: placing the target substrate of the transition metal sulfide nanosheet obtained from S1 in a brown light-proof stripping vessel in S2 for soaking, and then cleaning with deionized water to realize the construction of a full liquid-phase chemical sulfur vacancy; and finally, drying the cleaned sample to obtain a half of nanosheet which is intrinsic and constructed by weak oxidizing solution.
Further, the specific step of S1 is:
s1.1: preparing a silicon wafer deposited with transition metal group vulcanized nanosheets by using a CVD (chemical vapor deposition) method, a micromechanical stripping method, a liquid phase intercalation method or a chemical intercalation method;
s1.2 spin-coating PMMA glue on the silicon wafer deposited with the transition metal group sulfide nanosheets in the step 1, drying the PMMA glue by using a hot plate, placing the silicon wafer into diluted FH solution to etch away the silicon wafer, and obtaining a PMMA film with the transition metal group sulfide nanosheets;
s1.3, fishing the PMMA film into deionized water by using a clean silicon wafer, repeatedly cleaning, finally fishing the cleaned PMMA film onto a marked target substrate, drying at the temperature of 100-130 ℃ for 10-20 min, and then heating by using acetone to remove PMMA, thereby obtaining the target substrate containing the transition metal sulfide nanosheets;
s1.4 spin-coating PMMA to the target substrate again, drying at the temperature of 150-.
Further, the concentration of the weak oxidizing aqueous solution in S2 is less than 30%.
Further, the specific step of S3 is:
s3.1, placing the transition metal sulfide nanosheets obtained in S1 in a weak oxidizing solution water solution prepared in S2 for 1-60min, and then taking out and placing in deionized water for cleaning;
s3.2, drying the target substrate processed by the step S3.1 on a hot plate at 70-90 ℃ for 3-6 min, then heating and drying on the hot plate at 90-110 ℃ for 8-12 min, then removing the PMMA protective layer by using acetone, and heating and drying again to obtain a transition metal group sulfide nanosheet with half of intrinsic property and half of oversulfuric vacancy constructed by using weak oxidizing solution.
Further, the transition metal group sulfide nanosheet is a molybdenum disulfide, molybdenum diselenide, tungsten disulfide or tungsten diselenide nanosheet with high crystalline quality.
Further, the weak oxidizing solution is H2O2Solutions, hypochlorous acid solutions or dilute nitric acid solutions.
Further, the thickness of the transition metal group sulfide nanosheet in S1 is 0.65-100 nanometers.
Further, the target substrate is a silicon wafer, a sapphire substrate or a PET substrate.
The method mainly has the following characteristics in the preparation of the sulfur vacancy of the sulfide of the transition metal group:
1. the preparation method of the sulfur vacancy is simple and is a full liquid phase chemical method. The preparation of sulfur vacancies in transition metal group sulfides can be achieved by soaking with a weakly oxidizing aqueous solution, such as a hydrogen peroxide solution.
2. The preparation method of the sulfur vacancy is mild, mainly utilizes the electronegativity of negative ions in weak oxidizing aqueous solution, such as the strong electron adsorption effect of oxygen in hydrogen peroxide, namely the matching relationship of the strong electronegativity of oxygen and the formation energy of the sulfur vacancy, only relates to the formation of the sulfur vacancy, and has no damage to materials.
3. The preparation of the sulfur vacancy belongs to a liquid phase chemical method, the defect type of the preparation is single, only the sulfur vacancy is involved, molybdenum defect and other structural defects are not generated, the accurate preparation and regulation of the sulfur vacancy can be realized, and the liquid phase chemical method can realize 1012-1014cm-2Efficient production of a single type of sulfur vacancy.
4. The liquid phase chemical preparation of the sulfur vacancy can realize the preparation of the large-area transition metal group sulfide sulfur vacancy, breaks through the restriction of defect regulation of the traditional physical method and promotes the application of defect engineering.
5. The liquid phase chemical preparation process of the sulfur vacancy is compatible with the traditional CMOS process, and the development of defect engineering in the field of two-dimensional integrated electronic devices is promoted.
Drawings
FIG. 1 is a flow chart of hydrogen peroxide liquid phase chemical water solution method for preparing single sulfur vacancy.
FIG. 2 shows the control of the sum H by the precise region2O2Auger electron spectrum of monolayer molybdenum disulfide obtained by solution regulation and control method and atom structure diagram of monolayer molybdenum disulfide for preparing sulfur vacancy and intrinsic property observed by scanning transmission electron microscope.
Detailed Description
The technical solutions of the present invention will be described in detail with reference to the following examples, and it is obvious that the described examples are only a small part of the present invention, but not all examples. All other examples, which can be obtained by a person skilled in the art without making any inventive step, based on the examples of the present invention, fall within the scope of protection of the present invention.
The invention relates to a construction method of sulfur vacancies of transition metal sulfide nanosheets, which comprises the following specific steps:
s1: transferring the selected transition metal group sulfide nanosheets to a target substrate which is not reacted with a weak oxidizing solution and can be in firm contact with the transition metal group sulfide nanosheets for later use;
s2: diluting the weak oxidizing solution to a weak oxidizing aqueous solution with a certain concentration, and placing the weak oxidizing aqueous solution in a brown light-proof stripping container for later use;
s3: placing the target substrate of the transition metal sulfide nanosheet obtained from S1 in a brown light-proof stripping vessel in S2 for soaking, and then cleaning with deionized water to realize the construction of a full liquid-phase chemical sulfur vacancy; and finally, drying the cleaned sample to obtain a half of nanosheet which is intrinsic and constructed by weak oxidizing solution.
The specific steps of S1 are as follows:
s1.1: preparing a silicon wafer deposited with transition metal group vulcanized nanosheets by using a CVD (chemical vapor deposition) method, a micromechanical stripping method, a liquid phase intercalation method or a chemical intercalation method;
s1.2 spin-coating PMMA glue on the silicon wafer deposited with the transition metal group sulfide nanosheets in the step 1, drying the PMMA glue by using a hot plate, placing the silicon wafer into diluted FH solution to etch away the silicon wafer, and obtaining a PMMA film with the transition metal group sulfide nanosheets;
s1.3, fishing the PMMA film into deionized water by using a clean silicon wafer, repeatedly cleaning, finally fishing the cleaned PMMA film onto a marked target substrate, drying at the temperature of 100-130 ℃ for 10-20 min, and then heating by using acetone to remove PMMA, thereby obtaining the target substrate containing the transition metal sulfide nanosheets;
s1.4 spin-coating PMMA to the target substrate again, drying at the temperature of 150-.
The concentration of the weak oxidizing aqueous solution in the S2 is less than 30%.
The specific steps of S3 are as follows:
s3.1, placing the transition metal sulfide nanosheets obtained in S1 in a weak oxidizing solution water solution prepared in S2 for 1-60min, and then taking out and placing in deionized water for cleaning;
s3.2, drying the target substrate processed by the step S3.1 on a hot plate at 70-90 ℃ for 3-6 min, then heating and drying on the hot plate at 90-110 ℃ for 8-12 min, then removing the PMMA protective layer by using acetone, and heating and drying again to obtain a transition metal group sulfide nanosheet with half of intrinsic property and half of oversulfuric vacancy constructed by using weak oxidizing solution.
The transition metal group sulfide nanosheet is a molybdenum disulfide, molybdenum diselenide, tungsten disulfide or tungsten diselenide nanosheet with high crystallization quality.
The weak oxidizing solution is H2O2Solutions, hypochlorous acid solutions or dilute nitric acid solutions.
The thickness of the transition metal group sulfide nanosheet in S1 is 0.65-100 nanometers.
The target substrate is a silicon wafer, a sapphire substrate or a PET substrate.
Example 1:
s1, preparing a monolayer of molybdenum disulfide on the target substrate:
s1.1: and selecting a molybdenum disulfide nanosheet with the thickness of 100 nanometers, and transferring the molybdenum disulfide nanosheet onto a silicon wafer to obtain the silicon wafer containing the molybdenum disulfide nanosheet with the size of 30 micrometers.
S1.2: and spin-coating PMMA glue on a silicon wafer in S1, drying at 120 ℃ for 2 min, and putting the silicon wafer into a FH (hydrogen fluoride) solution with a ratio of 1:5 to etch away silicon dioxide to obtain the PMMA film with molybdenum disulfide.
S1.3: fishing the PMMA film into deionized water by using a clean silicon wafer, repeatedly cleaning for 15 times, finally fishing the cleaned PMMA film onto a marked target substrate, drying for 10 min at 120 ℃, and then removing PMMA by using acetone at 100 ℃ to obtain the monolayer molybdenum disulfide on the target substrate.
S1.4: and spin-coating PMMA again to the target substrate, drying at 180 ℃ for 2 min, exposing a half area of the single-layer triangular molybdenum disulfide by using an electron beam precise exposure technology, covering the other half area with PMMA, and developing the exposed area.
S2:
S2.1: hydrogen peroxide was formulated into 24% by volume aqueous hydrogen peroxide and placed in a brown light-resistant stripping vessel.
S3:
S3.1, placing the sample in S1.4 in the prepared aqueous hydrogen peroxide solution in S2.1 for 10 min, and taking out the substrate with the sample after the time is up and placing the substrate into deionized water for cleaning.
S3.2 when the cleaning is finished, drying the target base with the sample on a hot plate at 85 ℃ for 5 min, then heating and drying on a hot plate at 100 ℃ for 10 min, then removing the PMMA protective layer by using acetone, and heating and drying again at 100 ℃ to obtain half of intrinsic substance, and using H to obtain half of intrinsic substance2O2Preparing a single-layer molybdenum disulfide nanosheet with oversulfide vacancy.
To more accurately illustrate H2O2The scheme is implemented on the same single-layer molybdenum disulfide by selectively regulating sulfur vacancy of transition metal sulfide, firstly exposing a half of single-layer molybdenum disulfide region in a micro-region, covering the other half with PMMA, and then carrying out H2O2The specific flow chart of the sulfur vacancy preparation is shown in figure 1. (a) Monolayer disulfide transfer to target substrateMolybdenum nano-sheets are oxidized; (FIG. 1 b) half of the molybdenum disulfide nanosheets were precisely exposed and half were protected with PMMA; (FIG. 1 c) H2O2Soaking in water solution; (FIG. 1 d) DI water wash process; (FIG. 1 e) Hot plate drying process; (FIG. 1 f) acetone stripping. The oxygen in the hydrogen peroxide has stronger electron adsorption capacity, and the energy provided by the electron adsorption capacity is matched with the energy for forming the single sulfur vacancy, so by utilizing the characteristic, the sulfur vacancy in the single-layer molybdenum disulfide can be treated by H with different concentrations2O2And (5) regulating and controlling. The mild chemical method can effectively avoid the generation of other types of defects and avoid other damages to materials caused by the regulation and control process. The method can realize the precise regulation and control of the large-area transition metal group sulfide defects. In addition, PMMA assists in achieving precise zone control, as shown in FIG. 2 by precise zone control and H2O2Auger electron spectrum of monolayer molybdenum disulfide obtained by a solution regulation and control method and atom structure diagram of intrinsic and regulated monolayer molybdenum disulfide observed by a scanning transmission electron microscope. (a) Half of the area passes through H2O2An AES distribution diagram of the S element of the single-layer molybdenum disulfide processed by the aqueous solution; (b) half of the area passes through H2O2AES distribution diagram of molybdenum disulfide Mo element processed by aqueous solution; (c) a single-layer molybdenum disulfide STEM image grown by original CVD; (d) through H2O2STEM picture of treated monolayer molybdenum disulfide. It can be seen that H2O2The concentration of the single sulfur vacancy in the regulated region is obviously increased.
Example 2
S1 preparation of tungsten disulfide on a target substrate:
s1.1, selecting a tungsten disulfide nanosheet with the thickness of 20 nanometers, and transferring the tungsten disulfide nanosheet onto a silicon wafer to obtain the silicon wafer containing the tungsten disulfide nanosheet.
S1.2: spin-coating PMMA glue on a silicon wafer containing the tungsten disulfide nanosheets obtained in S1, drying at 100 ℃ for 6 min, and placing the silicon wafer into a FH solution with a ratio of 1:5 to etch away silicon dioxide to obtain the PMMA film with the tungsten disulfide nanosheets.
S1.3: and fishing the PMMA film into deionized water by using a clean silicon wafer, repeatedly cleaning for 15 times, finally fishing the cleaned PMMA film onto a sapphire substrate with marks, drying for 10 min at 120 ℃, and then removing PMMA by using acetone at 100 ℃ to obtain the single-layer tungsten disulfide on the target substrate.
S1.4: and spin-coating PMMA again to the target substrate, drying at 180 ℃ for 2 min, exposing a half area of the tungsten disulfide by using an electron beam precise exposure technology, covering the other half area with PMMA, and developing the exposed area.
S2:
S2.1: the hypochlorous acid solution is prepared into a hypochlorous acid water solution with the volume concentration of 20 percent and is placed in a brown light-proof stripping container.
S3:
S3.1, placing the sample in S1.5 in the prepared aqueous hydrogen peroxide solution in S2.1 for 60min, and taking out the substrate with the sample after the time is up and placing the substrate into deionized water for cleaning.
And S3.2, drying the target base with the sample on a hot plate at 85 ℃ for 5 min after the cleaning is finished, then heating and drying the target base on the hot plate at 100 ℃ for 10 min, removing the PMMA protective layer by using acetone, and heating and drying the target base at 100 ℃ again to obtain a half of intrinsic and a half of single-layer tungsten disulfide nanosheet with a sulfur passing vacancy prepared by using hypochlorous acid.
Example 3
S1, preparing molybdenum diselenide on the target substrate:
s1.1, selecting a molybdenum diselenide nanosheet with the thickness of 60 nanometers, and transferring the molybdenum diselenide nanosheet onto a silicon wafer to obtain a silicon wafer containing the molybdenum diselenide nanosheet with the size of 80 micrometers.
S1.2: and (3) spin-coating PMMA glue on a silicon wafer in S1, drying at 120 ℃ for 2 min, and putting the silicon wafer into a FH (hydrogen fluoride) solution with a ratio of 1:5 to etch away silicon dioxide to obtain the PMMA film with the molybdenum diselenide nanosheets.
S1.3: fishing the PMMA film into deionized water by using a clean silicon wafer, repeatedly cleaning for 15 times, finally fishing the cleaned PMMA film onto a PET substrate with a mark, drying for 10 min at 120 ℃, and then removing PMMA by using acetone at 100 ℃ to obtain the monolayer molybdenum diselenide on the PET substrate.
S1.4: and spin-coating PMMA again to the target substrate, drying at 180 ℃ for 2 min, exposing a half area of the molybdenum diselenide by using an electron beam precise exposure technology, covering the other half area with PMMA, and developing the exposed area.
S2:
S2.1: preparing dilute nitric acid solution with volume concentration of 16%, and placing the dilute nitric acid solution in a brown light-resistant stripping container.
S3:
S3.1, placing the sample in S1.5 in the prepared aqueous hydrogen peroxide solution in S2.1 for 40 min, and taking out the PET substrate with the sample after the time is up, and placing the PET substrate into deionized water for cleaning.
And 3.2, when the cleaning is finished, drying the target base with the sample on a hot plate at 85 ℃ for 10 min, then heating and drying the target base on a hot plate at 100 ℃ for 10 min, then removing the PMMA protective layer by using acetone, and heating and drying the target base at 100 ℃ again to obtain a half intrinsic substance, and preparing a sulfur vacancy single-layer molybdenum diselenide nanosheet by using dilute nitric acid for the half intrinsic substance.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims (7)

1. A method for constructing sulfur vacancies of sulfide nanosheets of transition metal groups is characterized by comprising the following specific steps:
s1: transferring the selected transition metal group sulfide nanosheets to a target substrate which is not reacted with a weak oxidizing solution and can be in firm contact with the transition metal group sulfide nanosheets for later use;
the method comprises the following specific steps:
s1.1: preparing a silicon wafer deposited with transition metal group vulcanized nanosheets by using a CVD (chemical vapor deposition) method, a micromechanical stripping method, a liquid phase intercalation method or a chemical intercalation method;
s1.2 spin-coating PMMA glue on the silicon wafer deposited with the transition metal group sulfide nanosheets in the step 1, drying the PMMA glue by using a hot plate, placing the silicon wafer into diluted FH solution to etch away the silicon wafer, and obtaining a PMMA film with the transition metal group sulfide nanosheets;
s1.3, fishing the PMMA film into deionized water by using a clean silicon wafer, repeatedly cleaning, finally fishing the cleaned PMMA film onto a marked target substrate, drying at the temperature of 100-130 ℃ for 10-20 min, and then heating by using acetone to remove PMMA, thereby obtaining the target substrate containing the transition metal sulfide nanosheets;
s1.4, spin-coating PMMA to the target substrate again, drying at the temperature of 150-;
s2: diluting the weak oxidizing solution to a weak oxidizing aqueous solution with a certain concentration, and placing the weak oxidizing aqueous solution in a brown light-proof stripping container for later use;
s3: placing the target substrate of the transition metal sulfide nanosheet obtained from S1 in a brown light-proof stripping vessel in S2 for soaking, and then cleaning with deionized water to realize the construction of a full liquid-phase chemical sulfur vacancy; and finally, drying the cleaned sample to obtain a half of nanosheet which is intrinsic and constructed by weak oxidizing solution.
2. The method of claim 1, wherein the concentration of the weakly oxidizing aqueous solution in S2 is less than 30%.
3. The method according to claim 1, wherein the specific steps of S3 are:
s3.1, placing the transition metal sulfide nanosheets obtained in S1 in a weak oxidizing solution water solution prepared in S2 for 1-60min, and then taking out and placing in deionized water for cleaning;
s3.2, drying the target substrate processed by the step S3.1 on a hot plate at 70-90 ℃ for 3-6 min, then heating and drying on the hot plate at 90-110 ℃ for 8-12 min, then removing the PMMA protective layer by using acetone, and heating and drying again to obtain a transition metal group sulfide nanosheet with half of intrinsic property and half of oversulfuric vacancy constructed by using weak oxidizing solution.
4. The method of claim 1, wherein the transition metal group sulfide nanosheets are molybdenum disulfide, molybdenum diselenide, tungsten disulfide, or tungsten diselenide nanosheets of high crystalline quality.
5. The method of claim 1, wherein the weakly oxidizing solution is H2O2Solutions, hypochlorous acid solutions or dilute nitric acid solutions.
6. The method of claim 1, wherein the transition metal group sulfide nanosheets in S1 have a thickness of from 0.65 to 100 nanometers.
7. The method of claim 1, wherein the target substrate is a silicon wafer, a sapphire substrate, or a PET substrate.
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