CN114293259A - Boron nitride crystal and preparation method thereof - Google Patents
Boron nitride crystal and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a boron nitride crystal, wherein the space group of the boron nitride crystal is IM-3, the lattice parameter a = b = c =14.034 (± 0.5%), and the crystal structure is a topological structure with a large-diameter nanopore. The boron nitride crystal has good physical properties. The invention also provides a preparation method of the boron nitride crystal, which has the advantages of low waste liquid generation rate, less impurities in the process, rich raw materials and low cost.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a boron nitride crystal and a preparation method thereof.
Background
Boron nitride is well known for its excellent thermal conductivity, electrical property, heat resistance, chemical stability and high hardness, and has a plurality of excellent physicochemical properties such as high heat resistance, high thermal conductivity, high chemical stability, non-wettability with various metals, and the like, so that it has a very wide application prospect in high-tech fields such as metallurgy, machinery, electronics, aerospace, and the like. Due to its special atomic bonding sp2 or sp3, boron nitride can exist in various crystal forms, such as hexagonal boron nitride (h-BN), Boron Nitride Nanotubes (BNNTs), wurtzite boron nitride (w-BN), and cubic zincblende BN (c-BN), among others. The current research on boron nitride is mainly focused on the research on the hexagonal phase and the cubic phase of the boron nitride. Hexagonal boron nitride is an analog of graphite and is mainly prepared by synthesizing and decomposing compounds containing boron and nitrogen, wherein the compounds containing boron mainly comprise halides, oxides, boric acid and the like of boron, and the compounds containing nitrogen mainly comprise ammonia, ammonia salts, urea and other organic ammonia. At present, a plurality of methods for preparing the nanometer boron nitride powder are available, and the method can be roughly divided into two categories according to the principle: one is a synthesis method, mainly including a high-temperature synthesis method, a solvothermal synthesis method, a template method, a Chemical Vapor Deposition (CVD) method, and the like; and the other is a peeling method including a liquid phase ultrasonic peeling method, a laser etching peeling method, a mechanical ball milling method, and the like. Cubic boron nitride (C-BN) is an artificially synthesized material, second only to diamond in hardness, and is a superhard material synthesized from hexagonal boron nitride and a catalyst at high temperature and high pressure. The Nanjing aerospace university discloses a three-dimensional boron nitride foam which is prepared by taking foam metal as a template and adopting chemical vapor deposition and chemical etching modes and has excellent performances such as low density, high thermal stability and the like. However, researches show that the network pores of the foam metal prepared by the method are as high as hundreds of micrometers, and the three-dimensional boron nitride foam prepared by using the method as a template has low volume density and is not beneficial to the macro preparation of the three-dimensional boron nitride foam. Currently, the prepared boron nitride mainly comprises cubic boron nitride and hexagonal boron nitride, and the preparation method of the novel boron nitride structure is not many.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects of cubic boron nitride and hexagonal boron nitride in the prior art, the invention provides a boron nitride crystal and a manufacturing method thereof.
The technical scheme is as follows: a boron nitride crystal comprising:
the space group of the boron nitride crystal is IM-3, the lattice parameter a = b = c =14.034 (± 0.5%), and the crystal structure is a topological structure with a large-diameter nanopore.
A method for producing the boron nitride crystal of claim 1, comprising the steps of:
(1) uniformly mixing ammonium chloride powder and borax, adding distilled water, and stirring at a controlled temperature to obtain a solution A;
(2) uniformly heating the solution A in the step (1) in an ammonia atmosphere to 900-1000K at a constant speed, carrying out constant temperature treatment for 2-3 h, and standing to obtain a white solid B;
(3) mixing hexagonal boron nitride powder with the solid B in the step (2), adding the mixture into hot water, stirring, soaking, precipitating, and washing for more than three times to obtain a mixture containing boron nitride single crystals;
(4) and (4) mixing the mixture obtained in the step (3) with a catalyst, performing high-temperature and high-pressure treatment at the temperature of 1200-1400 ℃ and the pressure of 10-15 GPa, then performing acid treatment and alkali treatment, washing with water, filtering, and drying in vacuum to obtain the boron nitride crystal.
Further, in the step (1), ammonium chloride powder and borax (NH)4Cl、Na2B4O7) The mass ratio of (A) to (B) is 2: 1.
Further, the mass concentration of the solution A in the step (2) is 0.06-0.10 g/mL.
Further, the mass ratio of the hexagonal boron nitride powder to the white solid B used in the step (3) is 3: 2.
Further, the catalyst in the step (4) is one or a combination of more of metal magnesium, nitride, boronitride and magnesium-based alloy.
Further, the mass percent of the catalyst in the step (4) is 15-20%.
Further, in the step (2), the constant temperature rise rate is 15-25K/min;
further, the step (4) of performing acid treatment and alkali treatment includes the steps of:
firstly, placing the mixture containing boron nitride single crystals in acid liquor, heating for 1-2 hours at the temperature of 450-550K, and then washing and drying. And then placing the obtained mixture in alkali liquor, and heating for 1-2 hours at the temperature of 450-600K.
Further, in the step (3), the hot water temperature is 300-400K.
Has the advantages that: the invention takes ammonium chloride powder and borax as nitrogen source and boron source, heats in ammonia atmosphere, mixes and stirs with hexagonal boron nitride powder, and carries out high-temperature high-pressure treatment. Finally, the novel boron nitride crystal is prepared by acid treatment, alkali treatment, water washing, filtration, vacuum drying and other steps. The method has the advantages of low waste liquid generation rate, less impurities in the process, rich raw materials and low cost.
Drawings
FIG. 1 is a diagram of the structure of novel boron nitride for the IM-3 space group;
FIG. 2 is an X-ray diffraction pattern of the novel boron nitride structure of the IM-3 space group of example 1;
FIG. 3 is an X-ray diffraction pattern of the novel boron nitride structure of the IM-3 space group of example 2;
FIG. 4 is an X-ray diffraction pattern of the novel boron nitride structure of the IM-3 space group of example 3;
FIG. 5 is an X-ray diffraction pattern of the novel boron nitride structure of the IM-3 space group of example 4.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a boron nitride crystal, the space group of the boron nitride crystal is IM-3, the lattice parameter a = b = c =14.034 (± 0.5%), and the crystal structure is a topological structure with a large-diameter nanometer hole.
The invention also provides a method for preparing the boron nitride crystal, which comprises the following steps:
(1) uniformly mixing ammonium chloride powder and borax, adding distilled water, and stirring at a controlled temperature to obtain a solution A;
(2) uniformly heating the solution A in the step (1) in an ammonia atmosphere to 900-1000K at a constant speed, carrying out constant temperature treatment for 2-3 h, and standing to obtain a white solid B;
(3) mixing hexagonal boron nitride powder with the solid B in the step (2), adding the mixture into hot water, stirring, soaking, precipitating, and washing for more than three times to obtain a mixture containing boron nitride single crystals;
(4) and (4) mixing the mixture obtained in the step (3) with a catalyst, performing high-temperature and high-pressure treatment at the temperature of 1200-1400 ℃ and the pressure of 10-15 GPa, then performing acid treatment and alkali treatment, washing with water, filtering, and drying in vacuum to obtain the boron nitride crystal.
The invention takes ammonium chloride powder and borax as nitrogen source and boron source, heats in ammonia atmosphere, mixes and stirs with hexagonal boron nitride powder, and carries out high-temperature high-pressure treatment. Finally, the novel boron nitride crystal is prepared by acid treatment, alkali treatment, water washing, filtration, vacuum drying and other steps. The method has the advantages of low waste liquid generation rate, less impurities in the process, rich raw materials and low cost.
Further, in the step (1), ammonium chloride powder and borax (NH)4Cl、Na2B4O7) The mass ratio of (A) to (B) is 2: 1.
Further, the mass concentration of the solution A in the step (2) is 0.06-0.10 g/mL.
Further, the mass ratio of the hexagonal boron nitride powder to the white solid B used in the step (3) is 3: 2.
Further, the catalyst in the step (4) is one or a combination of more of metal magnesium, nitride, boronitride and magnesium-based alloy.
Further, the mass percent of the catalyst in the step (4) is 15-20%.
Further, in the step (2), the constant temperature rise rate is 15-25K/min;
further, the step (4) of performing acid treatment and alkali treatment includes the steps of:
firstly, placing the mixture containing boron nitride single crystals in acid liquor, heating for 1-2 hours at the temperature of 450-550K, and then washing and drying. And then placing the obtained mixture in alkali liquor, and heating for 1-2 hours at the temperature of 450-600K.
Further, in the step (3), the hot water temperature is 300-400K.
The invention is further described below with reference to specific examples:
example 1:
novel boron nitride space group ofIM-3, lattice parametera=b=c=14.034 (± 0.5%), crystal structure is a topology with large diameter nanopores (see fig. 1);
a preparation method of novel boron nitride comprises the following specific steps:
(1) mixing ammonium chloride powder and borax (NH)4Cl、Na2B4O7) Uniformly mixing, adding distilled water, controlling the temperature and stirring to obtain a solution A; the concentration of the solution A is 0.06g/mL, and the mass ratio of the ammonium chloride powder to the borax is 2: 1.
(2) And (2) uniformly heating the solution A in the step (1) in a tubular furnace at a heating rate of 20K/min in an ammonia atmosphere to 900K, carrying out constant temperature treatment for 1h, uniformly heating at a heating rate of 20K/min to 1200K, and standing at a constant temperature for 3h to obtain a solid B.
(3) And (3) mixing the hexagonal boron nitride powder with the solid B in the step (2), adding the mixture into 350K hot water, stirring, soaking, precipitating, and washing for more than three times to obtain a mixture containing boron nitride single crystals. The mass ratio of the hexagonal boron nitride powder to the white solid B was 6: 4.
(4) And (4) mixing and stirring the mixture obtained in the step (3) with a catalyst, wherein the mass percent of the catalyst is 15%, and performing high-temperature high-pressure treatment at the temperature of 1200 ℃ and under the pressure of 10 GPa. Then carrying out acid treatment and alkali treatment, washing with water, filtering and vacuum drying to obtain the productIM-3 space groups of novel boron nitrides.
The acid treatment and the alkali treatment comprise the following steps:
firstly, placing the mixture containing boron nitride single crystals in acid liquor, heating for 1-2 hours at the temperature of 450K, and then washing and drying. The mixture obtained is then placed in an alkaline solution and heated at a temperature of 600K for 1 hour.
This exampleIMThe X-ray diffraction pattern of the novel boron nitride in the-3 space group is shown in FIG. 2, the lattice parameter of whicha=b=c=14.034；
This exampleIMThe density of the novel boron nitride structure of the-3 space group is 1.7891g/cm3。
Example 2:
a preparation method of a novel boron nitride crystal comprises the following specific steps:
(1) mixing ammonium chloride powder and borax (NH)4Cl、Na2B4O7) Uniformly mixing, adding distilled water, controlling the temperature and stirring to obtain a solution A; the concentration of the solution A is 0.06g/mL, and the mass ratio of the ammonium chloride powder to the borax is 2: 1;
(2) and (3) uniformly heating the solution A in the step (1) in a tubular furnace at a heating rate of 15K/min in an ammonia atmosphere to 900K, carrying out constant temperature treatment for 1h, and standing to obtain a white solid B. Then the temperature is raised to 1200K at a constant speed at the temperature rise rate of 20K/min and kept standing for 3.0h at a constant temperature to obtain a solid B.
(3) And (3) mixing the hexagonal boron nitride powder with the solid B in the step (2), adding the mixture into 350K hot water, stirring, soaking, precipitating, and washing for more than three times to obtain a mixture containing boron nitride single crystals. The mass ratio of the hexagonal boron nitride powder to the white solid B is 6:4
(4) And (4) mixing and stirring the mixture obtained in the step (3) with a catalyst, wherein the mass percent of the catalyst is 20%, and performing high-temperature high-pressure treatment at the temperature of 1200 ℃ and the pressure of 12 GPa. Then carrying out acid treatment and alkali treatment, washing with water, filtering and vacuum drying to obtain the productIM-3 space groups of novel boron nitrides.
The acid treatment and the alkali treatment comprise the following steps:
firstly, placing the mixture containing the boron nitride single crystal in acid liquor, heating for 1-2 hours at the temperature of 550K, and then washing and drying. The mixture obtained is then placed in an alkaline solution and heated at a temperature of 450K for 1.5 hours.
This exampleIMThe X-ray diffraction pattern of the novel boron nitride in the-3 space group is shown in FIG. 3, the lattice parameter of whicha=b=c=13.820；
This exampleIMThe density of the novel boron nitride structure of the-3 space group is 1.8168g/cm3。
Example 3:
a preparation method of a novel boron nitride crystal comprises the following specific steps:
(1) mixing ammonium chloride powder and borax (NH)4Cl、Na2B4O7) Uniformly mixing, adding distilled water, controlling the temperature and stirring to obtain a solution A; the concentration of the solution A is 0.06g/mL, and the mass ratio of the ammonium chloride powder to the borax is 2: 1;
(2) and (3) uniformly heating the solution A in the step (1) to 900K at a constant temperature in an ammonia atmosphere at a heating rate of 25K/min in a tubular furnace, carrying out constant temperature treatment for 1h, and standing to obtain a white solid B. Then the temperature is raised to 1200K at a constant speed at the temperature rise rate of 20K/min and kept standing for 3.0h at a constant temperature to obtain a solid B.
(3) And (3) mixing the hexagonal boron nitride powder with the solid B in the step (2), adding the mixture into 400K hot water, stirring, soaking, precipitating, and washing for more than three times to obtain a mixture containing boron nitride single crystals. The mass ratio of the hexagonal boron nitride powder to the white solid B was 6: 4.
(4) And (4) mixing and stirring the mixture obtained in the step (3) with a catalyst, wherein the mass percent of the catalyst is 18%, and performing high-temperature high-pressure treatment at 1300 ℃ and under the pressure of 10 GPa. Then carrying out acid treatment and alkali treatment, washing with water, filtering and vacuum drying to obtain the productIM-3 space groups of novel boron nitrides.
The acid treatment and the alkali treatment comprise the following steps:
firstly, placing the mixture containing boron nitride single crystals in acid liquor, heating for 1-2 hours at the temperature of 500K, and then washing and drying. The mixture obtained is then placed in an alkaline solution and heated at a temperature of 500K for 2 hours.
This exampleIMThe X-ray diffraction pattern of the novel boron nitride in the-3 space group is shown in FIG. 4, the lattice parameter of whicha=b=c=14.522；
This exampleIMThe density of the novel boron nitride structure of the-3 space group is 1.7289g/cm3。
Example 4:
a preparation method of a novel boron nitride crystal comprises the following specific steps:
(1) mixing ammonium chloride powder and borax (NH)4Cl、Na2B4O7) Uniformly mixing, adding distilled water, controlling the temperature and stirring to obtain a solution A; the concentration of the solution A is 0.06g/mL, and the mass ratio of the ammonium chloride powder to the borax is 2: 1;
(2) and (3) uniformly heating the solution A in the step (1) in a tubular furnace at a heating rate of 20K/min in an ammonia atmosphere to 900K, carrying out constant temperature treatment for 1h, and standing to obtain a white solid B. Then the temperature is raised to 1200K at a constant speed at the temperature rise rate of 20K/min and kept standing for 3.0h at a constant temperature to obtain a solid B.
(3) And (3) mixing the hexagonal boron nitride powder with the solid B in the step (2), adding the mixture into hot water, stirring, soaking, precipitating, and washing for more than three times to obtain a mixture containing boron nitride single crystals. The mass ratio of the hexagonal boron nitride powder to the white solid B is 6:4
(4) And (4) mixing and stirring the mixture obtained in the step (3) with a catalyst, and performing high-temperature high-pressure treatment at the temperature of 1300 ℃ and the pressure of 12 GPa. Then carrying out acid treatment and alkali treatment, washing with water, filtering and vacuum drying to obtain the productIM-3 space groups of novel boron nitrides.
This exampleIMThe X-ray diffraction pattern of the novel boron nitride in the-3 space group is shown in FIG. 5, the lattice parameter of whicha=b=c=13.682；
This exampleIMThe density of the novel boron nitride structure of the-3 space group is 1.7891g/cm3。
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (10)
1. A boron nitride crystal characterized by: the space group of the boron nitride crystal is IM-3, the lattice parameter a = b = c =14.034 (± 0.5%), and the crystal structure is a topological structure with a large-diameter nanopore.
2. A method for producing the boron nitride crystal according to claim 1, comprising the steps of:
(1) uniformly mixing ammonium chloride powder and borax, adding distilled water, and stirring at the temperature of 300-350K to obtain a solution A;
(2) uniformly heating the solution A in the step (1) in an ammonia atmosphere to 900-1000K at a constant speed, carrying out constant temperature treatment for 2-3 h, and standing to obtain a white solid B;
(3) mixing hexagonal boron nitride powder with the solid B in the step (2), adding the mixture into hot water, stirring, soaking, precipitating, and washing for more than three times to obtain a mixture containing boron nitride single crystals;
(4) and (4) mixing the mixture obtained in the step (3) with a catalyst, performing high-temperature and high-pressure treatment at the temperature of 1200-1400 ℃ and the pressure of 10-15 GPa, then performing acid treatment and alkali treatment, washing with water, filtering, and drying in vacuum to obtain the boron nitride crystal.
3. The method for producing a boron nitride crystal according to claim 2, characterized in that: in the step (1), ammonium chloride powder and borax (NH)4Cl、Na2B4O7) The mass ratio of (A) to (B) is 2: 1.
4. The method for producing a boron nitride crystal according to claim 3, characterized in that: the mass concentration of the solution A in the step (2) is 0.06-0.10 g/mL.
5. The method for producing a boron nitride crystal according to claim 4, characterized in that: the mass ratio of the hexagonal boron nitride powder used in the step (3) to the white solid B is 3: 2.
6. The method for producing a boron nitride crystal according to claim 1, characterized in that: the catalyst in the step (4) is one or a combination of more of metal magnesium, nitride, boronitride and magnesium-based alloy.
7. The method for producing a boron nitride crystal according to claim 6, characterized in that: the mass percentage of the catalyst in the step (4) is 15-20%.
8. The method for producing a boron nitride crystal according to claim 2, characterized in that: in the step (2), the constant temperature rise rate is 15-25K/min.
9. The method for producing a boron nitride crystal according to claim 2, characterized in that: in the step (4), the acid treatment and the alkali treatment include the following steps:
firstly, placing a mixture containing boron nitride single crystals in acid liquor, heating for 1-2 hours at the temperature of 450-550K, and then washing and drying; and then placing the obtained mixture in alkali liquor, and heating for 1-2 hours at the temperature of 450-600K.
10. The method for producing a boron nitride crystal according to claim 2, characterized in that: in the step (3), the hot water temperature is 300-400K.
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