CN113233431A - Two-dimensional material film forming method - Google Patents
Two-dimensional material film forming method Download PDFInfo
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- CN113233431A CN113233431A CN202110477748.0A CN202110477748A CN113233431A CN 113233431 A CN113233431 A CN 113233431A CN 202110477748 A CN202110477748 A CN 202110477748A CN 113233431 A CN113233431 A CN 113233431A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
Abstract
The invention discloses a two-dimensional material film forming method, which makes a two-dimensional material film more uniform through ultrasound and standing, and transfers the two-dimensional material film on a metal substrate uniformly, in a large area, without damage and with low cost through liquid drainage. As the solution is volatile solvent, no other impurity pollution is generated in the preparation process. The supernatant is obtained by liquid phase stripping and centrifugal treatment, the number of nanosheets of the supernatant is small, the area of the nanosheets is small, the coverage of the two-dimensional material film can be increased, the boundary can be in better contact, the quality of the two-dimensional material film formed on the liquid surface is more compact, the compactness of the two-dimensional material film is increased by pressing the sample wafer tightly under pressure, when the pressed sample wafer is annealed at the melting point of the metal substrate, the two-dimensional material and the metal substrate are in the optimal contact state, and the dangling bond of the two-dimensional material is activated at high temperature, so that the lattice defect is repaired, and the film forming quality is ensured.
Description
Technical Field
The invention relates to the technical field of nanometer, in particular to a two-dimensional material film forming method.
Background
Since the discovery of two-dimensional material graphene, various two-dimensional materials are discovered successively, and due to the unique structure of the two-dimensional material, the two-dimensional material has a plurality of peculiar performances, has a plurality of researches in the directions of optics, electronics, mechanics and the like, and has a wide prospect in the fields of polarization photoelectric devices, polarization thermoelectric devices, bionic devices, polarization optical detection and the like. However, how to form a large-area, high-uniformity, low-cost two-dimensional material film has been a key obstacle to the application of two-dimensional materials.
At present, the following films are prepared from two-dimensional materials: (1) chemical vapor deposition vaporizes reactants that react to form the target two-dimensional material, and the reactants are carried by the inert gas to the substrate to react to form the two-dimensional material. (2) Spin coating, selecting a proper organic solvent, preparing a two-dimensional material suspension with a proper concentration, and forming a film on the substrate by the two-dimensional material through high-speed rotation. (3) And (4) drop casting, namely selecting a proper organic solvent to configure the two-dimensional material into a proper concentration, dropping the two-dimensional material on the substrate, and forming a film on the substrate by a natural drying method. The method (1) can obtain a large-area two-dimensional material film with good quality, but the requirement on equipment and the requirement of high temperature make the preparation of the two-dimensional material very expensive, and the growth substrate is not a desirable substrate in general, and then the two-dimensional material film needs to be transferred to the required substrate through wet transfer or dry transfer. Whereas wet transfer may introduce less volatile impurities during transfer and may produce environmentally polluting solutions during transfer. The method (2) can directly form a film on a required substrate, has high requirements on the surface bonding force, the particle size, the solute viscosity and the volatility of the two-dimensional material, generally needs to perform surface treatment on the material or the substrate before spin coating, but can change the characteristics of the two-dimensional material or the substrate to a certain extent. The method (3) can also directly form a film on a desired substrate, but the film forming quality and the film forming thickness thereof are changed by the change of the external environment, and the controllability is poor. In view of the above, the mainstream two-dimensional material large-area preparation methods have different short plates, and the short plates mainly focus on high cost, severe conditions and uncontrollable conditions.
Disclosure of Invention
The invention aims to provide a two-dimensional material film forming method, and aims to solve the technical problems of high cost, severe conditions and uncontrollable film forming of two-dimensional materials in the prior art.
In order to achieve the above object, the present invention provides a two-dimensional material film forming method, comprising the steps of:
preparing a suspension of a two-dimensional material, carrying out water-bath ultrasonic treatment on the suspension, and then carrying out centrifugal treatment to obtain a first suspension;
fixing a metal substrate in a container, pouring deionized water into the container, and submerging the metal substrate;
pouring the supernatant of the first suspension into the container to form a mixed solution;
carrying out ultrasonic treatment on the container, then standing, and forming a two-dimensional material film on the liquid surface of the mixed solution;
opening a drainage switch at the bottom of the container, and receiving the two-dimensional material film by the metal substrate when the liquid level of the mixed solution descends;
covering a single-polished silicon wafer on the two-dimensional material film, covering the single-polished silicon wafer with a plastic film, and sealing the periphery with wax to obtain a sample wafer;
and drying the sample wafer, then carrying out pressurization treatment, then removing the plastic film, and carrying out annealing treatment.
The method comprises the following steps of preparing a suspension of a two-dimensional material, carrying out water bath ultrasonic treatment on the suspension, and then carrying out centrifugal treatment to obtain a first suspension:
preparing a suspension of the two-dimensional material by using an organic solution;
the water bath ultrasonic treatment time is 6-12 h;
centrifuging at 8000-20000 RPM for 1-2 h.
Fixing a metal substrate in a container, pouring deionized water, and submerging the metal substrate:
the liquid level of the solution is 0.25 cm-0.5 cm higher than the metal substrate.
Wherein the step of pouring the supernatant of the first suspension into the container:
selecting 1/4-1/3 of supernatant of the first suspension, and pouring the supernatant into the container.
Wherein, the step of sonicating the container and then standing:
and carrying out ultrasonic treatment on the container for 10-30 min, and then standing for 0.5-1 h.
Wherein the step of subjecting the sample to pressure treatment comprises:
and pressurizing the single polished silicon wafer and the metal substrate to tightly press the two-dimensional material film and the metal substrate.
Wherein, the annealing treatment comprises the following steps:
the annealing temperature is the melting point of the metal substrate +/-50 ℃.
The invention has the beneficial effects that: the two-dimensional material film is made more uniform by ultrasound and standing, and the two-dimensional material film is transferred uniformly, over a large area, non-injurious, and low-cost by liquid discharge onto the metal substrate. As the solution is volatile solvent, no other impurity pollution is generated in the preparation process. The supernatant is obtained by liquid phase stripping and centrifugal treatment, the number of the layers of the nanosheets of the supernatant is small, the area of the nanosheets is small, the coverage of the two-dimensional material film can be improved, the boundary can be in better contact, the quality of the two-dimensional material film formed on the liquid level is more compact, then the sample wafer is pressed tightly through pressurization, the compactness of the two-dimensional material film can be improved from the physical layer, the contact among the nanosheets is improved, and a foundation is provided for defect repair through annealing treatment. When the pressed sample wafer is annealed at the melting point of the metal substrate, because the metal substrate is in a molten state, the two-dimensional material and the metal substrate are in an optimal contact state at the time, the dangling bond of the two-dimensional material is activated at high temperature, so that the two-dimensional material can be better combined to repair the lattice defect, and the film forming quality is ensured.
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, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart showing the steps of a two-dimensional material film forming method of the present invention.
Fig. 2 is a surface view of a two-dimensional material film prepared using hexagonal boron nitride of the present invention.
FIG. 3 is a cross-sectional view of a two-dimensional material film of the present invention prepared using hexagonal boron nitride.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1 to 3, the present invention provides a two-dimensional material film forming method, including the following steps:
s1, preparing a suspension of a two-dimensional material, carrying out water bath ultrasonic treatment on the suspension, and then carrying out centrifugal treatment to obtain a first suspension;
s2, fixing the metal substrate in a container, pouring deionized water into the container, and submerging the metal substrate;
s3, pouring the supernatant of the first suspension into the container to form a mixed solution;
s4, carrying out ultrasonic treatment on the container, and then standing, wherein a two-dimensional material film is formed on the liquid surface of the mixed solution;
s5, opening a drainage switch at the bottom of the container, and receiving the two-dimensional material film by the metal substrate when the liquid level of the mixed solution descends;
s6, covering a single-polished silicon wafer on the two-dimensional material film, covering the plastic film on the single-polished silicon wafer, and sealing the periphery with wax to obtain a sample wafer;
and S7, drying the sample wafer, pressurizing, removing the plastic film and annealing.
Specifically, an organic solvent is used as a solvent to prepare a suspension of a two-dimensional material, water bath ultrasound is carried out for 6-12 h, the suspension after the water bath ultrasound is subjected to centrifugal treatment for 1-2 h at 8000-20000 RPM, and the first suspension is obtained. The organic solvent includes Dimethylformamide (DMF), N-methylpyrrolidone (NMP), 1,2 dichloroethane, cyclohexanone, chloroform, etc.
Specifically, the metal substrate is fixed in a container, deionized water is poured into the container, the metal substrate is submerged by the deionized water, and the liquid level of the deionized water is 0.25 cm-0.5 cm higher than that of the metal substrate.
Specifically, 1/4-1/3 of supernatant of the first suspension is selected and poured into the container.
Specifically, the container is subjected to ultrasonic treatment for 10min to 30min and then is kept stand for 0.5h to 1 h.
Specifically, a drainage switch at the bottom of a container is turned on, or a mixed solution in the container is sucked from the bottom of the solution through a syringe hose, so that the liquid level of the mixed solution is lowered, and the metal substrate receives a two-dimensional material film on the liquid level of the mixed solution when the liquid level of the mixed solution is lowered;
specifically, a single polished silicon wafer is polished downwards and covered on the two-dimensional material film, the single polished silicon wafer is slightly larger than the metal substrate, a plastic film is covered on the single polished silicon wafer, and the periphery of the single polished silicon wafer is sealed by wax to obtain a sample wafer.
Specifically, the sample wafer is put into a pressurizing device for pressurizing treatment, then is dried, and finally is annealed, so that the two-dimensional material film forming is completed.
Specifically, in the annealing treatment step, the annealing temperature is ± 50 ℃ of the melting point of the metal substrate.
The two-dimensional material film prepared by the liquid phase method has the problems of poor compactness, serious defects and the like, the supernatant is obtained by liquid phase stripping and centrifugal treatment, the number of nanosheet layers of the supernatant is small, the area is small, the coverage of the two-dimensional material film can be increased, the boundary can be better contacted, the quality of the two-dimensional material film formed on the liquid surface is more compact, then the sample plate is pressed tightly by pressurization, and the two-dimensional material film can increase the compactness from the physical layer, increase the contact among the nanosheets and provide a foundation for repairing the defects by annealing treatment. When the pressed sample wafer is annealed at the melting point of the metal substrate, the metal substrate is in a molten state, so that the two-dimensional material and the metal substrate are in an optimal contact state, and the suspension bond of the two-dimensional material is activated at high temperature to be better combined so as to achieve the purpose of repairing the defect, thereby ensuring the film forming quality.
The invention utilizes the process of self-forming of the two-dimensional material on the liquid surface to form a film independently, the two-dimensional material is more uniform through ultrasound and standing, and the two-dimensional material is transferred on the metal substrate through liquid drainage in a uniform, large-area, non-destructive and low-cost manner. Since the solutions are volatile solvents, no additional contamination of impurities occurs during the preparation process, and then densification is improved by compression and lattice defects are repaired by annealing. The method effectively overcomes the defects that the two-dimensional material film formed on the liquid level has poor compactness, poor film quality and the like.
The first embodiment is as follows:
preparing 1g of hexagonal boron nitride (h-BN) powder and 100ml of Dimethylformamide (DMF) into a suspension of the two-dimensional material, carrying out water bath ultrasonic treatment on the suspension for 10 hours, and then carrying out centrifugal treatment at the rotating speed of 8000-20000 RPM for 1-2 hours to obtain a first suspension;
the metal substrate is made of copper foil, the container is made of a lower liquid drainage container (100ml), the copper foil is fixed in the lower liquid drainage container, the deionized water is poured into the lower liquid drainage container, the copper foil is submerged, and the liquid level of the deionized water is 0.5cm higher than that of the copper foil;
selecting 1/3 supernatant (10ml) of the first suspension, and pouring into a drainable container below;
treating the lower drainable container for 20min, and standing for 1 h;
opening a valve of the lower liquid drainage container to enable the liquid level of the mixed solution in the lower liquid drainage container to slowly descend, and enabling the copper foil to bear the two-dimensional material film on the liquid level of the mixed solution;
placing a copper foil on a display stand, using a single polished silicon wafer with an area slightly larger than that of the copper foil, with a polished surface facing downwards, covering the two-dimensional material film, covering the single polished silicon wafer with a plastic film, and sealing the periphery with wax to obtain a sample wafer;
baking the sample wafer at 50 ℃ for 1 hour, then pressurizing the sample wafer, and then annealing at 1200 ℃ for 3 hours in a nitrogen atmosphere to complete film formation on the copper foil.
The second embodiment is as follows:
preparing 1g of hexagonal boron nitride (h-BN) powder and 100ml of Dimethylformamide (DMF) into a suspension of the two-dimensional material, carrying out water bath ultrasonic treatment on the suspension for 10 hours, and then carrying out centrifugal treatment at the rotating speed of 8000-20000 RPM for 1-2 hours to obtain a first suspension;
the metal substrate is made of copper foil, the container is made of a beaker (100ml), an injector hose is fixed in the beaker, the copper foil is fixed in the beaker, the deionized water is poured into the beaker, the copper foil is submerged, and the liquid level of the deionized water is 0.5cm higher than that of the copper foil;
selecting 1/3 supernatant (10ml) of the first suspension, and pouring into a drainable container below;
treating the lower drainable container for 20min, and standing for 1 h;
connecting an injector to a hose, slowly sucking the mixed solution to enable the liquid level of the mixed solution to slowly descend, and enabling the copper foil to bear the two-dimensional material film on the liquid level of the mixed solution;
placing a copper foil on a display stand, using a single polished silicon wafer with an area slightly larger than that of the copper foil, with a polished surface facing downwards, covering the two-dimensional material film, covering the single polished silicon wafer with a plastic film, and sealing the periphery with wax to obtain a sample wafer;
baking the sample wafer at 50 ℃ for 1 hour, then pressurizing the sample wafer, and then annealing at 1250 ℃ for 1 hour in a nitrogen atmosphere to complete film formation on the copper foil.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A two-dimensional material film forming method is characterized by comprising the following steps:
preparing a suspension of a two-dimensional material, carrying out water-bath ultrasonic treatment on the suspension, and then carrying out centrifugal treatment to obtain a first suspension;
fixing a metal substrate in a container, pouring deionized water into the container, and submerging the metal substrate;
pouring the supernatant of the first suspension into the container to form a mixed solution;
carrying out ultrasonic treatment on the container, then standing, and forming a two-dimensional material film on the liquid surface of the mixed solution;
opening a drainage switch at the bottom of the container, and receiving the two-dimensional material film by the metal substrate when the liquid level of the mixed solution descends;
covering a single-polished silicon wafer on the two-dimensional material film, covering the single-polished silicon wafer with a plastic film, and sealing the periphery with wax to obtain a sample wafer;
and drying the sample wafer, then carrying out pressurization treatment, then removing the plastic film, and carrying out annealing treatment.
2. The two-dimensional material film forming method according to claim 1, wherein a suspension of the two-dimensional material is prepared, and the suspension is subjected to water bath ultrasonic treatment and then centrifugal treatment to obtain a first suspension, and the step of:
preparing a suspension of the two-dimensional material by using an organic solution;
the water bath ultrasonic treatment time is 6-12 h;
centrifuging at 8000-20000 RPM for 1-2 h.
3. The two-dimensional material film formation method according to claim 1, wherein the step of fixing a metal substrate in a container, pouring deionized water, and submerging the metal substrate:
the liquid level of the deionized water is 0.25 cm-0.5 cm higher than the metal substrate.
4. The two-dimensional material film forming method according to claim 1, wherein the step of pouring the supernatant of the first suspension into the container:
selecting 1/4-1/3 of supernatant of the first suspension, and pouring the supernatant into the container.
5. The two-dimensional material film forming method according to claim 1, wherein in the step of subjecting the container to ultrasonic treatment and then standing:
and carrying out ultrasonic treatment on the container for 10-30 min, and then standing for 0.5-1 h.
6. The two-dimensional material film forming method according to claim 1, wherein the step of subjecting the sample to the pressure treatment:
and pressurizing the single polished silicon wafer and the metal substrate to tightly press the two-dimensional material film and the metal substrate.
7. The two-dimensional material film formation method according to claim 1, wherein the annealing step includes:
the annealing temperature is the melting point of the metal substrate +/-50 ℃.
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