CN112938911A - Preparation method of boron nitride nanosheet - Google Patents
Preparation method of boron nitride nanosheet Download PDFInfo
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 50
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Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Abstract
The invention discloses a preparation method of a boron nitride nanosheet. Uniformly mixing a certain amount of boron source and a certain amount of nitrogen source according to a certain proportion, controlling the temperature, stirring and dissolving in a dispersion solution, evaporating and crystallizing to obtain a precursor, placing the precursor in a high-temperature sintering device with protective gas for sintering, and controlling the temperature rise speed, the heat preservation time and the sintering temperature to finally obtain the nano boron nitride powder. According to the invention, a precursor is prepared from a boron source and a nitrogen source, and the boron nitride nanosheet is prepared through a high-temperature reaction. The method overcomes the defects of low purity, low yield, uneven powder granularity, large particle size and the like of the existing boron nitride preparation process, can improve the yield as single-batch production, can effectively reduce the production cost of the hexagonal boron nitride, and expands the industrial application value of the hexagonal boron nitride.
Description
Technical Field
The invention discloses a preparation method of boron nitride nanosheets, and belongs to the technical field of nano ceramic materials.
Background
Hexagonal boron nitride (h-BN) is an excellent wide band gap semiconductor, has a graphite-like layered structure, is ivory-white in color, is called white graphite, has excellent physicochemical properties such as high temperature stability, low dielectric constant, high mechanical strength, high thermal conductivity, high corrosion resistance, high adsorbability and the like, and is widely researched and applied to the fields of ceramics, electricians, energy storage, lubricants, nano electronic devices, catalyst carriers, adsorption of pollutants, hydrogen storage, release of medicines, purification of water and the like.
The preparation method of the boron nitride nanosheet comprises the following steps: mechanical lift-off, multilayer boron nitride nanotube by laser etching, ultrasonic, solid-phase reaction synthesis, chemical vapor deposition, ionic liquid thermal, and chemical solvent lift-off. Compared with other methods, the liquid phase stripping method has mild reaction process and mature development, and is a universal, simple and environment-friendly method at present. A small amount of hexagonal boron nitride powder can form a single-layer or few-layer h-BNNSs low-concentration dispersion liquid in a corresponding organic solvent or water by direct liquid-phase ultrasound. Since the dispersion stability of two-dimensional materials such as hexagonal boron nitride nanosheets in a solution needs a surfactant to be improved, research directions of experiments in recent years gradually turn to research on reagents which have the effects of assisting h-BN liquid phase stripping and enhancing the stability of the nanosheets after stripping. Compared with water and organic solvents, the organic solvent has better economic benefit and ecological benefit, so the current experimental research mainly takes water as the solvent.
The chemical stripping method is to insert reactants into the hexagonal boron nitride layers in a solution system, perform chemical reaction, and overcome van der Waals force between the hexagonal boron nitride layers by using free movement of a product, thereby obtaining the few-layer h-BNNSs. Chemical stripping has the defect of difficult operation because most of the prepared products exist in acid or alkaline solution and need to be further treated to enable the products to be close to neutrality, and the yield of the monolayer hexagonal boron nitride nanosheet prepared by the method is low.
Ball milling is a well-established mechanical stripping method currently used in many applications. The interaction of the sphere with h-BN was utilized: on one hand, in the ball milling process, the hard balls and the edge of the h-BN laminated structure are subjected to friction collision to enable the h-BN sheet to wrinkle and peel off; on the other hand, the high energy generated during ball milling also provides energy for the separation between the h-BN layers. The longer the ball milling time is, the better the stripping effect is, but as the ball milling time is increased, the defects of the product are also greatly increased and cause certain environmental pollution.
The CVD method is one of the most guaranteed and most economical methods, and has advantages of simple design and operation, controllable reaction, and obtaining of high-quality and high-performance products, but has a disadvantage that it is difficult to realize industrialization. When the method is applied to preparation of hexagonal boron nitride nanosheets, boron-containing compounds and nitrogen-containing compounds such as B2O3/CH5N3 & HCl, H3BO3, B2H6, N2/NH3 and the like are generally adopted as precursors by a CVD method, and inert gas is used as carrier gas to generate H-BNNSs at high temperature. The substrate typically utilizes transition elements or oxides such as copper, nickel, platinum, iron, cobalt, iridium, ruthenium, rhodium, silver, silica, and the like. Also, combinations of two or more metals are used as the substrate, such as cobalt nickel combinations and copper nickel combinations. Optimizing h-BN growth by taking copper as a substrate is also a means which is researched more at present. The desire to improve the quality of h-BN films can generally be started from two aspects: firstly, the nucleation amount is inhibited, the CVD parameters are controlled, and other external factors such as substrate surface smoothing, Cu grain enlarging and the like are enhanced, and the defect that the nucleation amount is difficult to realize when the crystal size exceeds a millimeter range; and secondly, splicing the independent nucleation areas.
However, the method has many limitations, and is not beneficial to large-scale preparation and application of the boron nitride nanosheet. For example, the yield is low, the size of the boron nitride nanoplatelets is small, the reaction conditions are harsh, and the experimental cost is expensive. Therefore, in order to improve the yield and obtain thinner nano-sheets, the boron nitride nano-sheets are prepared by preparing a precursor from a boron source and a nitrogen source and carrying out high-temperature reaction. The method overcomes the defects of low purity, low yield, uneven powder granularity, large particle size and the like of the existing boron nitride preparation process, can improve the yield as single-batch production, can effectively reduce the production cost of the hexagonal boron nitride, and expands the industrial application value of the hexagonal boron nitride.
Disclosure of Invention
The invention aims to provide a preparation method of boron nitride nanosheets, which comprises the steps of firstly carrying out low-temperature chemical synthesis on cheap raw materials to obtain a precursor, then carrying out high-temperature sintering on the precursor to obtain nano boron nitride with higher purity, specifically, uniformly mixing a certain amount of boron source and nitrogen source according to a certain proportion, controlling the temperature, stirring, dissolving in a dispersion solution, evaporating and crystallizing to obtain the precursor, placing the precursor in a high-temperature sintering device with protective gas for sintering, and controlling the heating speed, the heat preservation time and the sintering temperature to finally obtain nano boron nitride powder. The method overcomes the defects of low purity, low yield, uneven powder granularity, large particle size and the like of the existing boron nitride preparation process, can effectively reduce the production cost of the boron nitride, and expands the industrial application value of the boron nitride.
The invention provides 1. a preparation method of boron nitride nanosheets, which is characterized in that a boron source and a nitrogen source are uniformly mixed, the temperature is controlled to stir and dissolve the mixture in a dispersion solution, a precursor is obtained after evaporation and crystallization, the precursor is placed in a high-temperature sintering device with protective gas to be sintered, the airflow speed range is 600mL/min with an air flow rate of 100-;
preferably, the boron source is boric acid (H3 BO 3) or boron oxide (B2O 3), the nitrogen source is urea (CON2H4) or melamine (C3N6H6), the molar ratio of boron atoms to urea is 1 (5-30), and the molar ratio of boron atoms to melamine is (2-6): 1.
preferably, the dispersion solution is formed by mixing methanol or ethanol with deionized water, and the volume ratio of the alcohol to the deionized water is (0.8-2): 1.
preferably, the evaporative crystallization is performed by a method comprising: one of a water bath type evaporative crystallization method, an air-drying oven evaporative crystallization method, a vacuum drying oven evaporative crystallization method or a freeze-drying type evaporative crystallization method.
Preferably, the evaporative crystallization method is to prepare a hot solution by heating the solution to 40-85 ℃ and stirring the solution to completely dissolve the solute before evaporative crystallization.
Preferably, the heating and heat preservation temperature of the evaporative crystallization method, the forced air drying oven evaporative crystallization method or the vacuum drying oven evaporative crystallization method is 45-90 ℃.
Preferably, the hot solution is rapidly solidified with liquid nitrogen in a vacuum freeze dryer, and then dried to evaporate under vacuum.
Preferably, the precursor high-temperature sintering device can be a traditional high-temperature furnace or laser sintering.
The invention has the beneficial effects that:
the method overcomes the defects of low purity, low yield, uneven powder granularity, large particle size and the like of the existing boron nitride preparation process, can improve the yield as single-batch production, can effectively reduce the production cost of the hexagonal boron nitride, and expands the industrial application value of the hexagonal boron nitride.
Drawings
In the figure 1, boric acid and urea are used as raw materials, a mixed solution of ethanol and deionized water is used as a dispersion liquid, and a white crystalline precursor is obtained by evaporation and crystallization.
FIG. 2 shows the boron nitride product prepared by using boric acid and urea as raw materials.
FIG. 3 is an XRD pattern of boron nitride product prepared by using boric acid and urea as raw materials.
Detailed Description
The invention is further described below by means of specific examples:
example 1
Boric acid and urea (CON2H4) were mixed as 1: uniformly mixing the components in a molar ratio of 30, dissolving the mixture in a dispersion solution (prepared by mixing ethanol and deionized water in a volume ratio of 1: 1) at 50 ℃, and stirring the mixture to completely dissolve the mixture, wherein the aqueous solution is in a transparent state. The solution was subjected to evaporative crystallization at a temperature controlled at 65 ℃ to give a white crystalline solid. And transferring the white crystalline solid to an alumina crucible, sintering at a high temperature in an argon protective atmosphere, heating at a flow rate of 250mL/min and a heating rate of 30 ℃/min to 1130 ℃ for 4.5h, and cooling to obtain the boron nitride sheet. Boric acid and urea are used as raw materials, ethanol and deionized water are mixed to form dispersion, and white crystalline precursors obtained by evaporation and crystallization are shown in figure 1.
Example 2
Boric acid and urea (CON2H4) were mixed as 1: uniformly mixing the components in a molar ratio of 30, dissolving the mixture in a dispersion solution (prepared by mixing ethanol and deionized water in a volume ratio of 1: 1) at 50 ℃, and stirring the mixture to completely dissolve the mixture, wherein the aqueous solution is in a transparent state. The solution was subjected to evaporative crystallization at a temperature controlled at 65 ℃ to give a white crystalline solid. And transferring the white crystalline solid to an alumina crucible, sintering at a high temperature in an argon protective atmosphere, wherein the flow rate of air flow is 250mL/min, the heating rate is 30 ℃/min, the temperature is raised to 1130 ℃, the heat preservation time is 4.5h, and cooling to obtain the boron nitride nanosheet. The boron nitride product prepared by using boric acid and urea as raw materials is shown in figure 2.
Example 3
Boric acid and urea (CON2H4) were mixed as 1: uniformly mixing the components in a molar ratio of 30, dissolving the mixture in a dispersion solution (prepared by mixing ethanol and deionized water in a volume ratio of 1: 1) at 50 ℃, and stirring the mixture to completely dissolve the mixture, wherein the aqueous solution is in a transparent state. The solution was subjected to evaporative crystallization at a temperature controlled at 65 ℃ to give a white crystalline solid. And transferring the white crystalline solid to an alumina crucible, sintering at a high temperature in an argon protective atmosphere, wherein the flow rate of air flow is 250mL/min, the heating rate is 30 ℃/min, the temperature is raised to 1130 ℃, the heat preservation time is 4.5h, and cooling to obtain the boron nitride nanosheet. The XRD pattern of the boron nitride product prepared by using boric acid and urea as raw materials is shown in figure 3.
Example 4
Boric acid and melamine (C3N6H6) were mixed as 3: 1 molar ratio, dissolving in 50 deg.C dispersion solution (ethanol and deionized water at a volume ratio of 1: 1), stirring to dissolve completely, and making the aqueous solution transparent. The solution was subjected to evaporative crystallization at a temperature controlled at 75 ℃ to give a white crystalline solid. And transferring the white crystalline solid to an alumina crucible, sintering at a high temperature in an argon protective atmosphere, wherein the flow rate of air flow is 250mL/min, the heating rate is 30 ℃/min, the temperature is increased to 1220 ℃, the heat preservation time is 4.5h, and cooling to obtain the boron nitride nanosheet.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A preparation method of boron nitride nanosheets is characterized by uniformly mixing a boron source and a nitrogen source, controlling the temperature, stirring and dissolving in a dispersion solution, evaporating and crystallizing to obtain a precursor, placing the precursor in a high-temperature sintering device with protective gas for sintering, wherein the flow rate of airflow ranges from 100-.
2. A method for preparing boron nitride nanosheets according to claim 1, wherein the source of boron is boric acid (H)3BO3) Or boron oxide (B)2O3) The nitrogen source is urea (CON)2H4) Or melamine (C)3N6H6) Wherein boron atomThe mol ratio of the boron atoms to the melamine is (2-6): 1.
3. the method for preparing boron nitride nanosheets according to claim 1, wherein the dispersion solution is formed by mixing methanol or ethanol with deionized water, and the volume ratio of the alcohol to the deionized water is (0.8-2): 1.
4. a method for preparing boron nitride nanosheets according to claim 1, wherein the evaporative crystallization extraction method comprises: one of a water bath type evaporative crystallization method, an air-drying oven evaporative crystallization method, a vacuum drying oven evaporative crystallization method or a freeze-drying type evaporative crystallization method.
5. A method for preparing boron nitride nanosheets according to claim 4, wherein the method for evaporative crystallization comprises heating the solution to 40-85 ℃ and stirring to completely dissolve the solute to prepare a hot solution before evaporative crystallization.
6. The method for preparing boron nitride nanosheets according to claim 4, wherein the heating and holding temperature of the evaporative crystallization method, the forced air oven evaporative crystallization method or the vacuum oven evaporative crystallization method is 45-90 ℃.
7. A method for preparing boron nitride nanosheets according to claim 5, wherein the hot solution is rapidly solidified with liquid nitrogen in a vacuum freeze dryer and then dried to evaporate under vacuum.
8. The method for preparing boron nitride nanosheets according to claim 1, wherein the precursor high-temperature sintering device can be a conventional high-temperature furnace or laser sintering.
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| CN202110310156.XA CN112938911A (en) | 2021-03-24 | 2021-03-24 | Preparation method of boron nitride nanosheet |
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