CN114150290A - Two-dimensional nano tungsten disulfide semiconductor film and preparation method thereof - Google Patents
Two-dimensional nano tungsten disulfide semiconductor film and preparation method thereof Download PDFInfo
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- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000004065 semiconductor Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 81
- 238000000034 method Methods 0.000 claims abstract description 71
- 239000000758 substrate Substances 0.000 claims abstract description 63
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 55
- 239000010980 sapphire Substances 0.000 claims abstract description 55
- 239000000919 ceramic Substances 0.000 claims abstract description 53
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 39
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000010453 quartz Substances 0.000 claims abstract description 34
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 49
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- 238000000502 dialysis Methods 0.000 claims description 43
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- 239000007788 liquid Substances 0.000 claims description 36
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 26
- 238000009210 therapy by ultrasound Methods 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
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- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 1
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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Abstract
The invention discloses a preparation method of a two-dimensional nano tungsten disulfide semiconductor film, which comprises the following steps: putting tungsten trioxide into a ceramic boat, and putting the ceramic boat into a quartz tube cavity; placing the sapphire substrate with the graphene quantum dots in a ceramic boat with the front surface facing downwards; placing the ceramic boat in the central position of a high-temperature constant-temperature area in a tubular furnace; putting the sulfur powder into a ceramic boat, and placing the ceramic boat in a low-temperature area in a tubular furnace; connecting a vacuum pump for vacuum pumping so as to ensure that the air in the quartz tube cavity is exhausted; and heating the tube furnace to a first preset temperature within a first preset time, and reacting at constant temperature for a second preset time to obtain the tungsten disulfide semiconductor film. The invention also discloses a two-dimensional nano tungsten disulfide semiconductor film. The graphene quantum dots with uniform sizes are prepared by a citric acid pyrolysis method. The graphene quantum dots are used as a tungsten disulfide growth promoter, and the graphene quantum dots are introduced on the sapphire substrate, so that surface impurities are reduced, and tungsten disulfide deposition is promoted.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a two-dimensional nano tungsten disulfide semiconductor film and a preparation method thereof.
Background
Two-dimensional materials are an important part of the field of nanomaterials, and are a general term for a class of materials, which refer to thin film materials having a thickness of only one or a few atomic layers. Thin films with thicknesses as small as the atomic size are considered to be thermodynamically unstable and thus impossible, and the existence of two-dimensional materials was not proved until 2004 when graphene with a single-layer structure was prepared, and thus scientific research on two-dimensional materials has gradually started to attract a great deal of attention.
The existing method for preparing the two-dimensional material mainly comprises a chemical vapor deposition method, a mechanical stripping method, a lithium ion intercalation method, a liquid phase stripping method, a chemical stripping method, a hydrothermal method and the like. The chemical vapor deposition method is a main method for preparing large-area two-dimensional materials at present. However, the tungsten disulfide thin films prepared by the methods have the defects of obvious defects of poor yield and quality and the like, and a mature preparation process for preparing large-area high-quality two-dimensional tungsten disulfide semiconductor thin films is lacked at present.
Disclosure of Invention
In view of this, an object of the embodiments of the present invention is to provide a two-dimensional nano tungsten disulfide semiconductor film and a preparation method thereof, in which a graphene quantum dot with a uniform size is prepared by a citric acid pyrolysis method. The graphene quantum dots are used as a tungsten disulfide growth promoter, and the graphene quantum dots are introduced on the sapphire substrate, so that surface impurities are reduced, and tungsten disulfide deposition is promoted.
Based on the above purpose, an aspect of the embodiments of the present invention provides a method for preparing a two-dimensional nano tungsten disulfide semiconductor film, including the following steps: putting tungsten trioxide into a ceramic boat, and putting the ceramic boat into a quartz tube cavity; placing the sapphire substrate with the graphene quantum dots in a ceramic boat with the front surface facing downwards; placing the ceramic boat in the central position of a high-temperature constant-temperature area in a tubular furnace; putting the sulfur powder into a ceramic boat, and placing the ceramic boat in a low-temperature area in a tubular furnace; connecting a vacuum pump for vacuum pumping so as to ensure that the air in the quartz tube cavity is exhausted; and heating the tube furnace to a first preset temperature within a first preset time, and reacting at constant temperature for a second preset time to obtain the tungsten disulfide semiconductor film.
In some embodiments, the tungsten trioxide is added in an amount of 0.1 to 1g, preferably 0.5g, and the sulfur powder is added in an amount of 0.4 to 4g, preferably 2 g; the first preset time is 15-60 min, preferably 30 min; the first predetermined temperature is 750 ℃ to 1200 ℃, preferably 950 ℃; the second preset time is 5-30 min, preferably 15 min.
In some embodiments, before placing the sapphire substrate dripped with the graphene quantum dots facing down in the ceramic boat, the method further comprises: wiping the sapphire substrate with cotton for a third preset time, and then carrying out ultrasonic treatment in a liquid detergent solution for a fourth preset time; sequentially carrying out ultrasonic treatment in deionized water, ultrasonic treatment in alcohol and ultrasonic treatment in acetone; taking out the sapphire substrate, drying the sapphire substrate by using high-purity nitrogen, and cleaning the sapphire substrate for fifth preset time by using a plasma cleaning machine to remove organic impurities on the sapphire substrate; and absorbing the graphene quantum dot solution by using a liquid transfer gun, dropwise adding the graphene quantum dot solution on the cleaned sapphire substrate, and blow-drying by using high-purity nitrogen for later use.
In some embodiments, the third predetermined time is 1-15 min, preferably 5 min; the fourth preset time is 15-60 minutes, preferably 30 minutes; the fifth predetermined time is 1-30min, preferably 10 min.
In some embodiments, sonicating in deionized water, in alcohol, and in acetone, in sequence, comprises: sequentially performing ultrasonic treatment in deionized water for 30min, in alcohol for 30min, and finally in acetone for 30 min.
In some embodiments, before the drawing the graphene quantum dot solution with the pipette, the method further comprises: cleaning and drying a weighing bottle, weighing 1g of citric acid and putting the citric acid into a flat-bottomed flask; the flask was placed in an oil bath and heated at the second predetermined temperature for a sixth predetermined time. In some embodiments, the second predetermined temperature is 150 ℃ to 300 ℃, preferably 200 ℃, and the sixth predetermined time is 15 to 60min, preferably 30 min; weighing 1g of sodium hydroxide, and dissolving the sodium hydroxide in 100mL of deionized water to prepare a sodium hydroxide solution with the concentration of 10 mg/mL; pouring sodium hydroxide solution into the heated citric acid; stirring with glass rod to dissolve sodium hydroxide solution and citric acid thoroughly, ultrasonic cleaning with ultrasonic cleaner for seventh preset time (for example 60min), and filtering with water-based 0.22 μm microporous membrane to obtain orange liquid; transferring the orange liquid into a dialysis bag, putting the dialysis bag into a beaker filled with deionized water for dialysis, and dialyzing until the liquid in the beaker is neutral by using pH test paper to obtain the graphene quantum dot solution.
In some embodiments, the dialysis bag is placed in a beaker containing deionized water for dialysis until the liquid in the beaker is neutral as measured by a PH paper, comprising: and (3) putting the dialysis bag into a beaker filled with deionized water for dialysis, changing the deionized water every eighth preset time (for example, 2 hours), and dialyzing for ninth preset time (for example, about two days) until the liquid in the beaker is measured to be neutral by using a PH test paper, so as to obtain the graphene quantum dot solution.
In some embodiments, after obtaining the graphene quantum dot solution, the method further includes: and diluting the graphene quantum dot solution to obtain the graphene quantum dot solution with the concentration of 1.5 mg/mL.
In some embodiments, after obtaining the tungsten disulfide semiconductor film, the method further comprises: argon gas was continuously introduced at a flow rate of 100sccm until the tube furnace was cooled to room temperature at a cooling rate of about 1 ℃/s.
In some embodiments, connecting a vacuum pump to evacuate the quartz tube chamber to ensure that the quartz tube chamber is exhausted of air comprises: connecting a vacuum pump for vacuum pumping, and introducing argon with the flow rate of 100sccm for 60min to fill the whole quartz tube cavity with the argon so as to ensure that the air in the quartz tube cavity is exhausted.
In some embodiments, heating the tube furnace to a first predetermined temperature for a first predetermined time, and reacting at constant temperature for a second predetermined time to obtain the tungsten disulfide semiconductor film, comprising: and continuously introducing argon as a protective atmosphere, heating the tubular furnace to a first preset temperature within first preset time, and reacting at constant temperature for second preset time to obtain the tungsten disulfide semiconductor film.
In another aspect of the embodiments of the present invention, there is provided a two-dimensional nano tungsten disulfide semiconductor film, which is prepared by the following method: weighing 0.5g of tungsten trioxide and placing the tungsten trioxide into a ceramic boat, wherein the ceramic boat is placed in a quartz tube cavity; placing the sapphire substrate with the graphene quantum dots in a ceramic boat with the front surface facing downwards; the ceramic boat is placed in the central position of a high-temperature constant-temperature area in the tube furnace; weighing 2g of sulfur powder in a ceramic boat, and placing the ceramic boat in a low-temperature area in a tube furnace; connecting a vacuum pump for vacuum pumping so as to ensure that the air in the quartz tube cavity is exhausted; and heating the tube furnace to 950 ℃ within 30min, and reacting at constant temperature for 15min to obtain the tungsten disulfide semiconductor film.
In some embodiments, before placing the sapphire substrate dripped with the graphene quantum dots facing down in the ceramic boat, the method further comprises: wiping the sapphire substrate with cotton for 5min, and performing ultrasonic treatment in a detergent solution for 30 min; sequentially carrying out ultrasonic treatment in deionized water, ultrasonic treatment in alcohol and ultrasonic treatment in acetone; taking out the sapphire substrate, drying the sapphire substrate by using high-purity nitrogen, and cleaning the sapphire substrate for 10min by using a plasma cleaning machine to remove organic impurities on the substrate; and absorbing the graphene quantum dot solution by using a liquid transfer gun, dropwise adding the graphene quantum dot solution on the cleaned sapphire substrate, and blow-drying by using high-purity nitrogen for later use.
In some embodiments, sonicating in deionized water, in alcohol, and in acetone, in sequence, comprises: sequentially performing ultrasonic treatment in deionized water for 30min, in alcohol for 30min, and finally in acetone for 30 min.
In some embodiments, before the drawing the graphene quantum dot solution with the pipette, the method further comprises: cleaning and drying a weighing bottle, weighing 1g of citric acid and putting the citric acid into a flat-bottomed flask; placing the flat-bottomed flask in an oil bath pan, and heating at 200 ℃ for 30 min; weighing 1g of sodium hydroxide, and dissolving the sodium hydroxide in 100mL of deionized water to prepare a sodium hydroxide solution with the concentration of 10 mg/mL; pouring sodium hydroxide solution into the heated citric acid; stirring with a glass rod to fully dissolve the sodium hydroxide solution and the citric acid, performing ultrasonic treatment for 60min with an ultrasonic cleaner, and filtering with a water-based 0.22 micrometer microporous filter membrane to obtain an orange liquid; transferring the orange liquid into a dialysis bag, putting the dialysis bag into a beaker filled with deionized water for dialysis, and dialyzing until the liquid in the beaker is neutral by using pH test paper to obtain the graphene quantum dot solution.
In some embodiments, the dialysis bag is placed in a beaker containing deionized water for dialysis until the liquid in the beaker is neutral as measured by a PH paper, comprising: and (3) putting the dialysis bag into a beaker filled with deionized water for dialysis, changing the deionized water every 2 hours, and dialyzing for about two days until the liquid in the beaker is measured to be neutral by using pH test paper to obtain the graphene quantum dot solution.
In some embodiments, after obtaining the graphene quantum dot solution, the method further includes: and diluting the graphene quantum dot solution to obtain the graphene quantum dot solution with the concentration of 1.5 mg/mL.
In some embodiments, after obtaining the tungsten disulfide semiconductor film, the method further comprises: argon gas was continuously introduced at a flow rate of 100sccm until the tube furnace was cooled to room temperature at a cooling rate of about 1 ℃/s.
In some embodiments, connecting a vacuum pump to evacuate the quartz tube chamber to ensure that the quartz tube chamber is exhausted of air comprises: connecting a vacuum pump for vacuum pumping, and introducing argon with the flow rate of 100sccm for 60min to fill the whole quartz tube cavity with the argon so as to ensure that the air in the quartz tube cavity is exhausted.
In some embodiments, the tube furnace is heated to 950 ℃ within 30min, and the isothermal reaction is carried out for 15min, so as to obtain the tungsten disulfide semiconductor film, which comprises the following steps: and continuously introducing argon as protective atmosphere, heating the tube furnace to 950 ℃ within 30min, and reacting at constant temperature for 15min to obtain the tungsten disulfide semiconductor film.
The invention has at least the following beneficial technical effects:
according to the embodiment of the invention, tungsten trioxide is placed in a ceramic boat, and the ceramic boat is placed in a quartz tube cavity; placing the sapphire substrate with the graphene quantum dots in a ceramic boat with the front surface facing downwards; placing the ceramic boat in the central position of a high-temperature constant-temperature area in a tubular furnace; putting the sulfur powder into a ceramic boat, and placing the ceramic boat in a low-temperature area in a tubular furnace; connecting a vacuum pump for vacuum pumping so as to ensure that the air in the quartz tube cavity is exhausted; and heating the tube furnace to a first preset temperature within a first preset time, and reacting at constant temperature for a second preset time to obtain the tungsten disulfide semiconductor film. The invention also discloses a two-dimensional nano tungsten disulfide semiconductor film. The graphene quantum dots with uniform sizes are prepared by a citric acid pyrolysis method. The graphene quantum dots are used as a tungsten disulfide growth promoter, and the graphene quantum dots are introduced on the sapphire substrate, so that surface impurities are reduced, and tungsten disulfide deposition is promoted.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other embodiments can be obtained by using the drawings without creative efforts.
FIG. 1 is a schematic view of an embodiment of a method for preparing a two-dimensional nano tungsten disulfide semiconductor film according to the present invention;
fig. 2 is a schematic structural diagram adopted in the preparation process of the two-dimensional nano tungsten disulfide semiconductor film provided by the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following embodiments of the present invention are described in further detail with reference to the accompanying drawings.
It should be noted that all expressions using "first" and "second" in the embodiments of the present invention are used for distinguishing two entities with the same name but different names or different parameters, and it should be noted that "first" and "second" are merely for convenience of description and should not be construed as limitations of the embodiments of the present invention, and they are not described in any more detail in the following embodiments.
The tungsten trioxide and the sulfur powder react to generate the tungsten disulfide, which is a mature process. Tungsten disulfide is a two-dimensional material that is two-dimensional when it exists in a state where the number of layers is reduced to the thickness of one or several layers, and three-dimensional when the number of layers is several layers or more. Tungsten disulfide has excellent electrical and optical properties and has been applied to various optoelectronic devices. In the process of growing the tungsten disulfide by adopting a chemical vapor deposition method, impurities and defects on the substrate are the positions which are preferentially selected during deposition of a sample, the single-layer tungsten disulfide is easy to nucleate and grow on scratches, stains, edges or rough surfaces of the substrate, the nucleation density of the substrate is reduced when large-area growth is realized, and therefore the nucleation process can be influenced by the treatment of the substrate. The influence of the nucleation point on the growth of the two-dimensional material is provided by using seeds such as tetracarboxylic acid tetrapotassium salt (PTAS), tetracarboxylic dianhydride, dibutyl phthalate, graphene oxide and the like as an accelerant, and the addition of the seeds is found to enable a single-layer two-dimensional material to be obtained more easily, and the size of a sample, the film forming quality and the continuity are improved. Under this initiative, it is thought to grow a two-dimensional tungsten disulfide thin film using graphene quantum dots as seeds.
In view of the above objects, a first aspect of the embodiments of the present invention provides an embodiment of a method for preparing a two-dimensional nano tungsten disulfide semiconductor film. Fig. 1 is a schematic diagram illustrating an embodiment of a method for preparing a two-dimensional nano tungsten disulfide semiconductor film provided by the present invention. As shown in fig. 1, the preparation method of the two-dimensional nano tungsten disulfide semiconductor film according to the embodiment of the present invention includes the following steps:
s101, placing tungsten trioxide into a ceramic boat, and placing the ceramic boat into a quartz tube cavity.
S102, placing the sapphire substrate with the graphene quantum dots in a downward mode in a ceramic boat in a face-down mode.
That is, as shown in fig. 2, the sapphire substrate on which the graphene quantum dots are dropped is placed face down in a ceramic boat containing tungsten trioxide.
S103, placing the ceramic boat in the central position of a high-temperature constant-temperature area in the tube furnace.
And S104, putting the sulfur powder into a ceramic boat, and placing the ceramic boat in a low-temperature area in a tube furnace.
S105, connecting a vacuum pump to vacuumize so as to ensure that air in the quartz tube cavity is exhausted;
wherein, connect the evacuation of vacuum pump to guarantee that the air of quartz capsule cavity is arranged to the greatest extent, specifically be:
connecting a vacuum pump for vacuum pumping, and introducing argon with the flow rate of 100sccm for 60min to fill the whole quartz tube cavity with the argon so as to ensure that the air in the quartz tube cavity is exhausted.
And S106, heating the tube furnace to a first preset temperature within a first preset time, and reacting at constant temperature for a second preset time to obtain the tungsten disulfide semiconductor film.
Heating the tube furnace to a first preset temperature within a first preset time, and reacting at constant temperature for a second preset time to obtain the tungsten disulfide semiconductor film, wherein the tungsten disulfide semiconductor film can be:
and continuously introducing argon as protective atmosphere, heating the tube furnace to 950 ℃ within 30min, and reacting at constant temperature for 15min to obtain the tungsten disulfide semiconductor film.
In the embodiment of the invention, 0.5g of tungsten trioxide is weighed and placed in a ceramic boat, and the ceramic boat is placed in a quartz tube cavity; placing the sapphire substrate with the graphene quantum dots in a ceramic boat with the front surface facing downwards; placing the ceramic boat in the central position of a high-temperature constant-temperature area in a tubular furnace; weighing 2g of sulfur powder in a ceramic boat, and placing the ceramic boat in a low-temperature area in a tube furnace; connecting a vacuum pump for vacuum pumping so as to ensure that the air in the quartz tube cavity is exhausted; and heating the tube furnace to 950 ℃ within 30min, and reacting at constant temperature for 15min to obtain the tungsten disulfide semiconductor film. The invention also discloses a two-dimensional nano tungsten disulfide semiconductor film. The graphene quantum dots with uniform sizes are prepared by a citric acid pyrolysis method. The graphene quantum dots are used as a tungsten disulfide growth promoter, and the graphene quantum dots are introduced on the sapphire substrate, so that surface impurities are reduced, and tungsten disulfide deposition is promoted.
In some embodiments of the present invention, the preparation method of a two-dimensional nano tungsten disulfide semiconductor film provided by the present invention may further include: the sapphire substrate was wiped with cotton for 5min and then sonicated in a detergent solution for 30 min. Sonication in deionized water, sonication in alcohol, and sonication in acetone were performed in sequence. Wherein, the ultrasonic treatment in deionized water, the ultrasonic treatment in alcohol and the ultrasonic treatment in acetone in turn can be: sequentially performing ultrasonic treatment in deionized water for 30min, in alcohol for 30min, and finally in acetone for 30 min. Taking out the sapphire substrate, drying the sapphire substrate by using high-purity nitrogen, and cleaning the sapphire substrate for 10min by using a plasma cleaning machine to remove organic impurities on the sapphire substrate. And absorbing the graphene quantum dot solution by using a liquid transfer gun, dropwise adding the graphene quantum dot solution on the cleaned sapphire substrate, and blow-drying by using high-purity nitrogen for later use.
According to the embodiment of the invention, the graphene quantum dot solution is absorbed by the liquid-transferring gun and is dripped on the cleaned sapphire substrate. Therefore, the method selects the sapphire as the substrate and carries out pretreatment on the graphene quantum dots, so that the tungsten disulfide film is easier to obtain, and the size, the quality and the continuity of the single crystal are improved.
In some embodiments of the present invention, the preparation method of a two-dimensional nano tungsten disulfide semiconductor film provided by the present invention may further include: the weighing bottle was rinsed clean and dried, and 1g of citric acid was weighed and placed in a flat bottom flask. The flask was placed in an oil bath and heated at 200 ℃ for 30 min. 1g of sodium hydroxide was weighed and dissolved in 100mL of deionized water to prepare a 10mg/mL sodium hydroxide solution. And pouring the sodium hydroxide solution into the citric acid obtained after heating. Stirring with glass rod to dissolve sodium hydroxide solution and citric acid thoroughly, ultrasonic cleaning with ultrasonic cleaner for 60min, and filtering with water system 0.22 μm microporous membrane to obtain orange liquid. Transferring the orange liquid into a dialysis bag, putting the dialysis bag into a beaker filled with deionized water for dialysis, and dialyzing until the liquid in the beaker is neutral by using pH test paper to obtain the graphene quantum dot solution.
In a specific implementation manner, the dialysis bag is put into a beaker filled with deionized water for dialysis until the liquid in the beaker is measured to be neutral by a PH test paper, which specifically can be: and (3) putting the dialysis bag into a beaker filled with deionized water for dialysis, changing the deionized water every 2 hours, and dialyzing for about two days until the liquid in the beaker is measured to be neutral by using pH test paper to obtain the graphene quantum dot solution.
In a specific implementation manner, after obtaining the graphene quantum dot solution, the method for preparing the two-dimensional nano tungsten disulfide semiconductor film provided by the invention may further include: and diluting the graphene quantum dot solution to obtain the graphene quantum dot solution with the concentration of 1.5 mg/mL.
In the embodiment of the invention, a beaker filled with deionized water is placed into a dialysis bag for dialysis until the liquid in the beaker is measured to be neutral by a pH test paper, and the method comprises the following steps: and (3) putting the dialysis bag into a beaker filled with deionized water for dialysis, changing the deionized water every 2 hours, and dialyzing for about two days until the liquid in the beaker is measured to be neutral by using pH test paper to obtain the graphene quantum dot solution. The method for preparing the graphene quantum dots with uniform sizes by using the citric acid pyrolysis method is simple and convenient, and the treatment method of the sapphire substrate is simple and convenient.
In some embodiments of the present invention, after obtaining the tungsten disulfide semiconductor film, the method for preparing a two-dimensional nano tungsten disulfide semiconductor film provided by the present invention may further include: argon gas was continuously introduced at a flow rate of 100sccm until the tube furnace was cooled to room temperature at a cooling rate of about 1 ℃/s.
The invention provides a method for preparing a large-area continuous high-quality two-dimensional tungsten disulfide film. The graphene quantum dots serve as a seed promoter to provide nucleation points for growth of tungsten disulfide, and impurities with similar structures of the graphene quantum dots and the crystals are introduced on the substrate, so that surface energy is reduced, and deposition of tungsten disulfide is promoted. The tungsten disulfide film can be more easily obtained by reaction on the sapphire substrate and treatment of graphene quantum dots, and the size, quality and continuity of the single crystal are improved. The method for preparing the graphene quantum dots with uniform sizes by using the citric acid thermal decomposition method is simple and convenient, and the method for processing the sapphire substrate is simple and convenient. The specific reaction condition for generating the tungsten disulfide by the reaction of the tungsten trioxide and the sulfur powder is combined with the promotion effect of the graphene quantum dots under the mature reaction condition, so that the large-area continuous high-quality two-dimensional tungsten disulfide film can be obtained.
It should be understood by those skilled in the art that although specific values of the first predetermined time, the first predetermined temperature … …, etc. are shown in the above embodiments, these values may be adjusted as needed and are included within the scope of the present application.
In view of the above objects, according to a second aspect of the embodiments of the present invention, there is provided a two-dimensional nano tungsten disulfide semiconductor film, which can be prepared by the following method, the method may include the following steps: weighing 0.5g of tungsten trioxide and placing the tungsten trioxide into a ceramic boat, wherein the ceramic boat is placed in a quartz tube cavity; placing the sapphire substrate with the graphene quantum dots in a ceramic boat with the front surface facing downwards; the ceramic boat is placed in the central position of a high-temperature constant-temperature area in the tube furnace; weighing 2g of sulfur powder in a ceramic boat, and placing the ceramic boat in a low-temperature area in a tube furnace; connecting a vacuum pump for vacuum pumping so as to ensure that the air in the quartz tube cavity is exhausted; and heating the tube furnace to 950 ℃ within 30min, and reacting at constant temperature for 15min to obtain the tungsten disulfide semiconductor film.
In some embodiments, before placing the sapphire substrate dripped with the graphene quantum dots facing down in the ceramic boat, the method further comprises: wiping the sapphire substrate with cotton for 5min, and performing ultrasonic treatment in a detergent solution for 30 min; sequentially carrying out ultrasonic treatment in deionized water, ultrasonic treatment in alcohol and ultrasonic treatment in acetone; taking out the sapphire substrate, drying the sapphire substrate by using high-purity nitrogen, and cleaning the sapphire substrate for 10min by using a plasma cleaning machine to remove organic impurities on the substrate; and absorbing the graphene quantum dot solution by using a liquid transfer gun, dropwise adding the graphene quantum dot solution on the cleaned sapphire substrate, and blow-drying by using high-purity nitrogen for later use.
In some embodiments, sonicating in deionized water, in alcohol, and in acetone, in sequence, comprises: sequentially performing ultrasonic treatment in deionized water for 30min, in alcohol for 30min, and finally in acetone for 30 min.
According to the embodiment of the invention, the graphene quantum dot solution is absorbed by the liquid-transferring gun and is dripped on the cleaned sapphire substrate. Therefore, the method selects the sapphire as the substrate and carries out pretreatment on the graphene quantum dots, so that the tungsten disulfide film is easier to obtain, and the size, the quality and the continuity of the single crystal are improved.
In some embodiments, before the drawing the graphene quantum dot solution with the pipette, the method further comprises: cleaning and drying a weighing bottle, weighing 1g of citric acid and putting the citric acid into a flat-bottomed flask; placing the flat-bottomed flask in an oil bath pan, and heating at 200 ℃ for 30 min; weighing 1g of sodium hydroxide, and dissolving the sodium hydroxide in 100mL of deionized water to prepare a sodium hydroxide solution with the concentration of 10 mg/mL; pouring sodium hydroxide solution into the heated citric acid; stirring with a glass rod to fully dissolve the sodium hydroxide solution and the citric acid, performing ultrasonic treatment for 60min with an ultrasonic cleaner, and filtering with a water-based 0.22 micrometer microporous filter membrane to obtain an orange liquid; transferring the orange liquid into a dialysis bag, putting the dialysis bag into a beaker filled with deionized water for dialysis, and dialyzing until the liquid in the beaker is neutral by using pH test paper to obtain the graphene quantum dot solution.
In some embodiments, the dialysis bag is placed in a beaker containing deionized water for dialysis until the liquid in the beaker is neutral as measured by a PH paper, comprising: and (3) putting the dialysis bag into a beaker filled with deionized water for dialysis, changing the deionized water every 2 hours, and dialyzing for about two days until the liquid in the beaker is measured to be neutral by using pH test paper to obtain the graphene quantum dot solution.
In some embodiments, after obtaining the graphene quantum dot solution, the method further includes: and diluting the graphene quantum dot solution to obtain the graphene quantum dot solution with the concentration of 1.5 mg/mL.
In the embodiment of the invention, a beaker filled with deionized water is placed into a dialysis bag for dialysis until the liquid in the beaker is measured to be neutral by a pH test paper, and the method comprises the following steps: and (3) putting the dialysis bag into a beaker filled with deionized water for dialysis, changing the deionized water every 2 hours, and dialyzing for about two days until the liquid in the beaker is measured to be neutral by using pH test paper to obtain the graphene quantum dot solution. The method for preparing the graphene quantum dots with uniform sizes by using the citric acid pyrolysis method is simple and convenient, and the treatment method of the sapphire substrate is simple and convenient.
In some embodiments, after obtaining the tungsten disulfide semiconductor film, the method further comprises: argon gas was continuously introduced at a flow rate of 100sccm until the tube furnace was cooled to room temperature at a cooling rate of about 1 ℃/s.
In some embodiments, connecting a vacuum pump to evacuate the quartz tube chamber to ensure that the quartz tube chamber is exhausted of air comprises: connecting a vacuum pump for vacuum pumping, and introducing argon with the flow rate of 100sccm for 60min to fill the whole quartz tube cavity with the argon so as to ensure that the air in the quartz tube cavity is exhausted.
In some embodiments, the tube furnace is heated to 950 ℃ within 30min, and the isothermal reaction is carried out for 15min, so as to obtain the tungsten disulfide semiconductor film, which comprises the following steps: and continuously introducing argon as protective atmosphere, heating the tube furnace to 950 ℃ within 30min, and reacting at constant temperature for 15min to obtain the tungsten disulfide semiconductor film.
The invention provides a method for preparing a large-area continuous high-quality two-dimensional tungsten disulfide film. The graphene quantum dots serve as a seed promoter to provide nucleation points for growth of tungsten disulfide, and impurities with similar structures of the graphene quantum dots and the crystals are introduced on the substrate, so that surface energy is reduced, and deposition of tungsten disulfide is promoted. The tungsten disulfide film can be more easily obtained by reaction on the sapphire substrate and treatment of graphene quantum dots, and the size, quality and continuity of the single crystal are improved. The method for preparing the graphene quantum dots with uniform sizes by using the citric acid thermal decomposition method is simple and convenient, and the method for processing the sapphire substrate is simple and convenient. The specific reaction condition for generating the tungsten disulfide by the reaction of the tungsten trioxide and the sulfur powder is combined with the promotion effect of the graphene quantum dots under the mature reaction condition, so that the large-area continuous high-quality two-dimensional tungsten disulfide film can be obtained.
The foregoing is an exemplary embodiment of the present disclosure, but it should be noted that various changes and modifications could be made herein without departing from the scope of the present disclosure as defined by the appended claims. The functions, steps and/or actions of the method claims in accordance with the disclosed embodiments described herein need not be performed in any particular order. Furthermore, although elements of the disclosed embodiments of the invention may be described or claimed in the singular, the plural is contemplated unless limitation to the singular is explicitly stated.
It should be understood that, as used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly supports the exception. It should also be understood that "and/or" as used herein is meant to include any and all possible combinations of one or more of the associated listed items.
The numbers of the embodiments disclosed in the embodiments of the present invention are merely for description, and do not represent the merits of the embodiments.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, of embodiments of the invention is limited to these examples; within the idea of an embodiment of the invention, also technical features in the above embodiment or in different embodiments may be combined and there are many other variations of the different aspects of the embodiments of the invention as described above, which are not provided in detail for the sake of brevity. Therefore, any omissions, modifications, substitutions, improvements, and the like that may be made without departing from the spirit and principles of the embodiments of the present invention are intended to be included within the scope of the embodiments of the present invention.
Claims (10)
1. A preparation method of a two-dimensional nano tungsten disulfide semiconductor film is characterized by comprising the following steps:
putting tungsten trioxide into a ceramic boat, and putting the ceramic boat into a quartz tube cavity;
placing the sapphire substrate dripped with the graphene quantum dots in the ceramic boat with the front surface facing downwards;
placing the ceramic boat in the central position of a high-temperature constant-temperature area in a tubular furnace;
putting sulfur powder into the ceramic boat and placing the ceramic boat in a low-temperature area in the tubular furnace;
connecting a vacuum pump for vacuum pumping to ensure that the air in the quartz tube cavity is exhausted;
and heating the tube furnace to a first preset temperature within a first preset time, and reacting at constant temperature for a second preset time to obtain the tungsten disulfide semiconductor film.
2. The method for preparing the two-dimensional nanometer tungsten disulfide semiconductor film according to claim 1, wherein before placing the sapphire substrate dropped with the graphene quantum dots in the ceramic boat with the front surface facing downward, the method further comprises:
wiping the sapphire substrate with cotton for third preset time, and then carrying out ultrasonic treatment in a liquid detergent solution for fourth preset time;
sequentially carrying out ultrasonic treatment in deionized water, ultrasonic treatment in alcohol and ultrasonic treatment in acetone;
taking out the sapphire substrate, drying the sapphire substrate by using high-purity nitrogen, and cleaning the sapphire substrate for fifth preset time by using a plasma cleaning machine to remove organic impurities on the sapphire substrate;
and absorbing the graphene quantum dot solution by using a liquid transfer gun, dropwise adding the graphene quantum dot solution on the cleaned sapphire substrate, and blow-drying by using high-purity nitrogen for later use.
3. The method for preparing the two-dimensional nanometer tungsten disulfide semiconductor film as claimed in claim 1, wherein the loading amount of the tungsten trioxide is 0.1-1 g, and the loading amount of the sulfur powder is 0.4-4 g.
4. The method for preparing the two-dimensional nanometer tungsten disulfide semiconductor film as claimed in claim 2, wherein before the drawing of the graphene quantum dot solution with the pipette, the method further comprises:
cleaning and drying a weighing bottle, weighing 1g of citric acid and putting the citric acid into a flat-bottomed flask;
placing the flat-bottomed flask in an oil bath, and heating at the second preset temperature for sixth preset time;
weighing 1g of sodium hydroxide, and dissolving the sodium hydroxide in 100mL of deionized water to prepare a sodium hydroxide solution with the concentration of 10 mg/mL;
pouring the sodium hydroxide solution into the heated citric acid;
stirring with a glass rod to fully dissolve the sodium hydroxide solution and the citric acid, performing ultrasonic treatment for seventh preset time by using an ultrasonic cleaner, and filtering with a microporous filter membrane with a water system of 0.22 micron to obtain orange liquid;
and transferring the orange liquid into a dialysis bag, putting the dialysis bag into a beaker filled with deionized water for dialysis, and dialyzing until the liquid in the beaker is measured to be neutral by using pH test paper to obtain the graphene quantum dot solution.
5. The method for preparing the two-dimensional nanometer tungsten disulfide semiconductor film as claimed in claim 4, wherein the dialysis bag is placed into a beaker filled with deionized water for dialysis until the liquid in the beaker is neutral by pH test paper, and the method comprises the following steps:
and putting the dialysis bag into a beaker filled with deionized water for dialysis, changing the deionized water every eighth preset time, and dialyzing for ninth preset time until the liquid in the beaker is measured to be neutral by using PH test paper to obtain the graphene quantum dot solution.
6. The method for preparing the two-dimensional nanometer tungsten disulfide semiconductor film as claimed in claim 4, wherein after obtaining the graphene quantum dot solution, the method further comprises:
and diluting the graphene quantum dot solution to obtain the graphene quantum dot solution with the concentration of 1.5 mg/mL.
7. The method for preparing the two-dimensional nanometer tungsten disulfide semiconductor film according to claim 1, further comprising, after obtaining the tungsten disulfide semiconductor film:
argon gas was continuously introduced at a flow rate of 100sccm until the tube furnace was cooled to room temperature at a cooling rate of about 1 ℃/s.
8. The method for preparing the two-dimensional nanometer tungsten disulfide semiconductor film as claimed in claim 1, wherein a vacuum pump is connected for vacuum pumping to ensure that the air in the quartz tube chamber is exhausted, comprising:
connecting a vacuum pump for vacuum pumping, and introducing argon with the flow rate of 100sccm for a tenth preset time to fill the whole quartz tube cavity with argon so as to ensure that the air in the quartz tube cavity is exhausted.
9. The method for preparing the two-dimensional nanometer tungsten disulfide semiconductor film according to claim 8, wherein the tube furnace is heated to a first preset temperature within a first preset time, and is subjected to isothermal reaction for a second preset time to obtain the tungsten disulfide semiconductor film, and the method comprises the following steps:
and continuously introducing argon as a protective atmosphere, heating the tubular furnace to a first preset temperature within first preset time, and reacting at constant temperature for second preset time to obtain the tungsten disulfide semiconductor film.
10. A two-dimensional nano tungsten disulfide semiconductor film prepared by the method of any one of claims 1-9.
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