CN114293259A - Boron nitride crystal and preparation method thereof - Google Patents
Boron nitride crystal and preparation method thereof Download PDFInfo
- Publication number
- CN114293259A CN114293259A CN202111472054.4A CN202111472054A CN114293259A CN 114293259 A CN114293259 A CN 114293259A CN 202111472054 A CN202111472054 A CN 202111472054A CN 114293259 A CN114293259 A CN 114293259A
- Authority
- CN
- China
- Prior art keywords
- boron nitride
- nitride crystal
- temperature
- producing
- crystal according
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 75
- 239000013078 crystal Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000000203 mixture Substances 0.000 claims description 33
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 25
- 239000007787 solid Substances 0.000 claims description 24
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 20
- 239000003513 alkali Substances 0.000 claims description 18
- 239000003054 catalyst Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 17
- 235000019270 ammonium chloride Nutrition 0.000 claims description 16
- 229910021538 borax Inorganic materials 0.000 claims description 16
- 239000004328 sodium tetraborate Substances 0.000 claims description 16
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 16
- 238000010306 acid treatment Methods 0.000 claims description 15
- 229910021529 ammonia Inorganic materials 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 229910004835 Na2B4O7 Inorganic materials 0.000 claims description 7
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 239000011777 magnesium Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 150000004767 nitrides Chemical class 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 17
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 230000000704 physical effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 238000001291 vacuum drying Methods 0.000 description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 5
- 239000006260 foam Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000012670 alkaline solution Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- -1 comprise halides Chemical compound 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000010329 laser etching Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical compound [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Images
Landscapes
- Catalysts (AREA)
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111472054.4A CN114293259A (en) | 2021-12-06 | 2021-12-06 | Boron nitride crystal and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111472054.4A CN114293259A (en) | 2021-12-06 | 2021-12-06 | Boron nitride crystal and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114293259A true CN114293259A (en) | 2022-04-08 |
Family
ID=80966550
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111472054.4A Pending CN114293259A (en) | 2021-12-06 | 2021-12-06 | Boron nitride crystal and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114293259A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244812A (en) * | 2008-02-26 | 2008-08-20 | 武汉理工大学 | Method for manufacturing flying saucer shaped nano-hexagonal boron nitride powder |
| CN101891165A (en) * | 2010-07-15 | 2010-11-24 | 丹东市化工研究所有限责任公司 | Production method of macrocrystalline hexagonal boron nitride |
| CN106586980A (en) * | 2016-12-16 | 2017-04-26 | 富耐克超硬材料股份有限公司 | Preparation method of cubic boron nitride |
| CN109825880A (en) * | 2019-03-07 | 2019-05-31 | 信阳市德隆超硬材料有限公司 | A kind of cubic boron nitride monocrystal and preparation method thereof |
| CN110016719A (en) * | 2019-04-30 | 2019-07-16 | 吉林大学 | A kind of bismuth sulfide compound crystal and preparation method thereof |
| CN110759327A (en) * | 2019-10-12 | 2020-02-07 | 宁波海秀丰科技有限公司 | Preparation method of metal carbon crystal |
-
2021
- 2021-12-06 CN CN202111472054.4A patent/CN114293259A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244812A (en) * | 2008-02-26 | 2008-08-20 | 武汉理工大学 | Method for manufacturing flying saucer shaped nano-hexagonal boron nitride powder |
| CN101891165A (en) * | 2010-07-15 | 2010-11-24 | 丹东市化工研究所有限责任公司 | Production method of macrocrystalline hexagonal boron nitride |
| CN106586980A (en) * | 2016-12-16 | 2017-04-26 | 富耐克超硬材料股份有限公司 | Preparation method of cubic boron nitride |
| CN109825880A (en) * | 2019-03-07 | 2019-05-31 | 信阳市德隆超硬材料有限公司 | A kind of cubic boron nitride monocrystal and preparation method thereof |
| CN110016719A (en) * | 2019-04-30 | 2019-07-16 | 吉林大学 | A kind of bismuth sulfide compound crystal and preparation method thereof |
| CN110759327A (en) * | 2019-10-12 | 2020-02-07 | 宁波海秀丰科技有限公司 | Preparation method of metal carbon crystal |
Non-Patent Citations (1)
| Title |
|---|
| "关于以硼砂和氯化铵为原料制备六方氮化硼方法中若干问题的试验探讨", 四川大学学报(自然科学版), no. 01, pages 65 - 70 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108275663B (en) | Method for preparing uniform-pore mesoporous boron nitride by melt bubble template method | |
| CN104724685A (en) | Preparation method of nano aluminium nitride powder | |
| CN110980664A (en) | Porous few-layer h-BN nanosheet and preparation method thereof | |
| CN107640751A (en) | One-dimensional boron nitride nano material and preparation method thereof | |
| CN104944391A (en) | Preparing method of hexagonal boron nitride with high specific surface area | |
| CN111484334B (en) | High alpha-phase silicon nitride powder and preparation method thereof | |
| CN107161960B (en) | A kind of high pressure vapor prepares the method and apparatus of boron nitride spherical powder | |
| CN108483414B (en) | Low-temperature synthesis diamond boron nitride powder based on molten salt growth method and preparation method thereof | |
| WO2019232765A1 (en) | Preparation method for ultrathin boron nitride nanosheet | |
| CN109574014B (en) | B4C fiber felt and preparation method thereof | |
| Xu et al. | Combustion synthesis of MgSiN2 powders and Si3N4‐MgSiN2 composite powders: Effects of processing parameters | |
| Tan et al. | Low temperature synthesis of 2H-SiC powders via molten-salt-mediated magnesiothermic reduction | |
| CN103496679B (en) | A kind of beta-silicon nitride powder and preparation method thereof | |
| CN111268656A (en) | Preparation method of boron nitride nanotube | |
| Liu et al. | Facile growth of oriented SiC nanowires arrays on carbon fiber cloth via CVD | |
| Soltys et al. | Synthesis and Properties of Silicon Carbide | |
| CN110386593A (en) | The method that the induction of amorphous precursor body synthesizes spherical boron nitride (BN) nano-powder | |
| CN1603238A (en) | Preparation method of titanium carbide and titanium nitride one dimension nanometer construction material | |
| CN104071760B (en) | The preparation method of the bar-shaped hexagonal boron nitride stupalith of a kind of porous | |
| US7192644B2 (en) | Non-aqueous borate routes to boron nitride | |
| CN114293259A (en) | Boron nitride crystal and preparation method thereof | |
| CN103030120B (en) | Fabrication method of boron-carbon-nitrogen nanotube | |
| CN105314609A (en) | Preparation method of AIN nano-powder material | |
| US7060237B1 (en) | Non-aqueous borate routes to boron nitride | |
| CN104828792B (en) | A kind of preparation method of lamellar aluminium nitride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |