CN111204720A - Batch preparation method of boron nitride nanotubes - Google Patents
Batch preparation method of boron nitride nanotubes Download PDFInfo
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- CN111204720A CN111204720A CN202010085419.7A CN202010085419A CN111204720A CN 111204720 A CN111204720 A CN 111204720A CN 202010085419 A CN202010085419 A CN 202010085419A CN 111204720 A CN111204720 A CN 111204720A
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 43
- 239000002184 metal Substances 0.000 claims abstract description 43
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000012043 crude product Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 24
- 229910052582 BN Inorganic materials 0.000 claims abstract description 23
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052796 boron Inorganic materials 0.000 claims abstract description 20
- 239000002071 nanotube Substances 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- 238000004321 preservation Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims description 23
- 229910052810 boron oxide Inorganic materials 0.000 claims description 18
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 13
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 10
- 229910052744 lithium Inorganic materials 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- PZKRHHZKOQZHIO-UHFFFAOYSA-N [B].[B].[Mg] Chemical group [B].[B].[Mg] PZKRHHZKOQZHIO-UHFFFAOYSA-N 0.000 claims description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 4
- 238000005554 pickling Methods 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- 238000010923 batch production Methods 0.000 claims 4
- 239000000047 product Substances 0.000 abstract description 2
- 239000000843 powder Substances 0.000 description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 238000001816 cooling Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 description 4
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses a batch preparation method of boron nitride nanotubes. The preparation method comprises the steps of respectively arranging active metal and/or active metal boride and a boron source in a reaction system of a nitrogen source atmosphere; heating the reaction system to 1200-1700 ℃, and carrying out heat preservation reaction to obtain a crude product; and carrying out post-treatment on the crude product to obtain the boron nitride nanotube. Compared with the prior art, the method has the advantages of low cost, high production efficiency, high product purity, and good reproducibility and stability.
Description
Technical Field
The invention belongs to the technical field of inorganic nano materials, and particularly relates to a batch preparation method of boron nitride nanotubes.
Background
The hexagonal Boron Nitride (BN) nano material is a material formed by alternating covalent bonds of B atoms and N atoms, wherein both the B atoms and the N atoms adopt sp2 hybridization, and the covalent bonds between the B atoms and the N atoms have the property of partial ionic bonds due to the difference of electronegativity of the B atoms and the N atoms. BN with different structures can be divided into one-dimensional Boron Nitride Nanotubes (BNNTs) and two-dimensional nanosheets (BNNSs), both have the advantages of super-good high-temperature stability, good thermal conductivity, excellent electrical insulation, excellent lubricating property, good mechanical strength, good chemical stability and the like, and have great application potential in the fields of thermal interface materials, biomedicine, aerospace and national defense industry. General methods for preparing boron nitride nanotubes include, but are not limited to, ball milling annealing, arc discharge, chemical vapor deposition, laser ablation, etc., but these methods have the disadvantages of high cost, long time consumption, complex experimental apparatus, low production efficiency, etc. Therefore, the mass preparation of boron nitride nanotubes is a very challenging problem, and therefore, the development of a preparation method for synthesizing BNNTs at low cost has important significance in promoting the application of boron nitride nanomaterials in important fields.
The synthesis method disclosed in the related patent document CN109825880A is a cubic boron nitride preparation method, and it needs to be mentioned that the preparation method of the patent document is too simple and does not relate to the control and design of product morphology; CN109252202A discloses an electrolyte only containing nano boron nitride magnesium alloy micro-arc oxidation, and relates to the technical field of electrolytes; CN107673318A discloses a boron nitride nanotube and a method for preparing the same in bulk, which is relatively low in cost, easy to scale up and easy to mass-produce, but requires catalyst loading and handling of the precursor, and is complicated in process, and moreover, the diameter of the prepared boron nitride nanotube is relatively large.
Disclosure of Invention
In order to solve the above technical problems, the present invention aims to provide a method for preparing boron nitride nanotubes with low cost and simple process, and suitable for mass production.
An embodiment of the present invention provides a method for preparing a boron nitride nanotube, including:
respectively arranging active metal and/or active metal boride and a boron source in a reaction system of a nitrogen source atmosphere;
heating the reaction system to 1200-1700 ℃, and carrying out heat preservation reaction to obtain a crude product;
and carrying out post-treatment on the crude product to obtain the boron nitride nanotube.
One embodiment includes:
disposing an active metal and/or an active metal boride and a boron source, respectively, in a chemical vapor deposition system;
and heating the chemical vapor deposition system to 700-1100 ℃ in a protective atmosphere, and introducing a nitrogen source to obtain the reaction system.
In one embodiment, the temperature of the chemical vapor deposition system is increased to 700-1100 ℃ at a rate of 2-30 ℃/min.
In one embodiment, the active metal is selected from one or a combination of magnesium and lithium; and/or, the active metal boride is selected from magnesium boride; and/or the active metal and the active metal boride are in the form of particles, strips or belts; and/or, the boron source is selected from one or a combination of boron oxide, boric acid or borate; the nitrogen source is selected from one or a combination of ammonia gas and nitrogen gas.
One embodiment includes:
and (3) carrying out heat preservation reaction on the reaction system at 1200-1700 ℃ for 1-4 h to obtain a crude product.
In one embodiment, the post-processing comprises: and carrying out acid washing and drying treatment on the crude product to obtain the boron nitride nanotube.
One embodiment includes: and (3) pickling the crude product at the temperature of 40-90 ℃ for 1-2 h, and drying at the temperature of 50-100 ℃ for 3-9 h to obtain the boron nitride nanotube.
In one embodiment, the active metal and/or the active metal boride and the boron source are respectively carried in a high-temperature reaction boat, and the material of the high-temperature reaction boat is one selected from alumina, silicon nitride and zirconia.
In one embodiment, in the direction of introducing the nitrogen source into the reaction system, the active metal and/or the active metal boride is located at the front end of the boron source, and the distance between the active metal and/or the active metal boride and the boron source is 5-10 cm.
The boron nitride nanotube prepared by the method has the tube diameter of 20-40 nm and the tube length of 80-180 mu m.
The invention obtains a large amount of high-purity boron nitride nanotubes by using cheap and easily-obtained materials such as active metal, boron source and the like, adjusting the placing condition between the two raw materials, using a simple and convenient chemical vapor deposition preparation process and a subsequent treatment and purification procedure.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be 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 described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 a: optical photographs of the boron nitride nanotubes obtained in this example;
FIG. 1 b: scanning electron micrographs of the boron nitride nanotubes obtained in this example;
FIG. 1 c: scanning electron micrographs of the boron nitride nanotubes obtained in this example;
FIG. 1 d: TEM image of the boron nitride nanotubes obtained in this example;
Detailed Description
The present invention will be more fully understood from the following detailed description, which should be read in conjunction with the accompanying drawings. Detailed embodiments of the present invention are disclosed herein; however, it is to be understood that the disclosed embodiments are merely exemplary of the invention, which can be embodied in various forms. Therefore, specific functional details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present invention in virtually any appropriately detailed embodiment.
The embodiment of the invention provides a batch preparation method of boron nitride nanotubes, which comprises the following steps:
and S1, respectively arranging the active metal and/or the active metal boride and the boron source in a reaction system of a nitrogen source atmosphere.
The active metal is selected from one or a combination of magnesium and lithium; the active metal boride is selected from magnesium boride; the active metal and the active metal boride are in the forms of particles, strips, sheets or belts; the boron source is selected from one or a combination of boron oxide, boric acid or borate; the nitrogen source is selected from one or a combination of ammonia gas and nitrogen gas. Of course, in alternate embodiments, the boron source may be any substance that decomposes to boron oxide vapor at high temperatures.
In a specific reaction process, firstly, respectively loading an active metal and/or an active metal boride and a boron source into a high-temperature reaction boat, and then sequentially arranging the active metal and/or the active metal boride and the boron source in a normal pressure/low pressure chemical vapor deposition system (CVD, specifically, for example, a normal pressure chemical vapor deposition system, a low pressure chemical vapor deposition system and the like) according to the direction of introducing a nitrogen source into a reaction system; and then heating the chemical vapor deposition system to 700-1100 ℃ in a protective atmosphere, and introducing a nitrogen source to obtain the reaction system.
In one embodiment, the temperature of the chemical vapor deposition system is raised to 800-1000 ℃.
In one embodiment, the material of the high temperature reaction boat is selected from one of alumina, silicon nitride and zirconia.
In one embodiment, the distance between the active metal and/or the active metal boride and the boron source is 5-8 cm.
The protective atmosphere may be inert gas such as argon, nitrogen, etc. introduced into the chemical vapor deposition system to remove the original atmosphere (e.g., air) in the chemical vapor deposition system. The temperature rise rate of the chemical vapor deposition system is 2-30 ℃/min, and preferably 10 ℃/min.
S2, heating the reaction system to 1200-1700 ℃, and carrying out heat preservation reaction to obtain a crude product.
The temperature of the heat preservation reaction is preferably 1300 ℃; the reaction time is 1-4 h, preferably 2 h.
And S3, carrying out post-treatment on the crude product to obtain the boron nitride nanotube.
The post-processing here includes: and carrying out acid washing and drying treatment on the crude product to obtain the boron nitride nanotube. Specifically, the crude product is subjected to acid washing for 1-2 hours at the temperature of 40-90 ℃, and is dried for 3-9 hours at the temperature of 50-100 ℃ to obtain the boron nitride nanotube.
The pickling solution can be 1-4 mol/L hydrochloric acid, nitric acid and sulfuric acid, and the pickling temperature can be preferably 50-85 ℃; the temperature of the drying may be preferably 60 deg.c, and the drying time may be preferably 6 hours.
In one embodiment, the boron nitride nanotubes prepared by the above method have a tube diameter of about 20 to 40nm and a tube length of about 80 to 180 μm.
The technical solution of the present invention is further explained with reference to the drawings and the embodiments.
Example 1: weighing 1g of magnesium powder and 2g of boron oxide powder, separately placing in an alumina ceramic boat, placing magnesium at about 6cm in the front section of the boron oxide powder, placing in CVD (chemical vapor deposition) furnace, removing air in the furnace chamber with argon, heating to 800 deg.C, and introducing 100sccm of NH3Programmed heating to 1300 ℃ and keeping the temperature for 90min, and closing NH after the reaction is finished3And cooling to room temperature in Ar atmosphere to obtain a white crude product. FIG. 1(a) is an optical photograph of the collected boron nitride nanotubes, which shows that a large amount of boron nitride nanotubes are produced. And then treating the obtained crude product with 1-4 mol/L hydrochloric acid at 85 ℃ for 1-2 h, filtering, washing with deionized water and ethanol for several times, and drying in a 60 ℃ oven for 6h to obtain the pure boron nitride nanotube. Fig. 1(b) and 1(c) are scanning electron micrographs of the prepared boron nitride nanotubes, respectively, and fig. 1(d) is a TEM image of the prepared boron nitride nanotubes, showing that the prepared boron nitride nanotubes have better crystallization properties.
Example 2: 0.5g of lithium piece and 4g of boron oxide powder are weighed and respectively put into an alumina boat, the lithium piece is positioned at about 5cm in the front section of the boron oxide powder and is put into a CVD furnace. Removing air in the furnace chamber by Ar, heating to 700 ℃, and introducing NH of 50sccm3The temperature is programmed to 1200 ℃ and kept for 120min, NH is closed after the reaction is finished3And cooling to room temperature in Ar atmosphere to obtain a white crude product. Then treating the obtained crude product with 1-4 mol/L hydrochloric acid at 85 ℃ for 1-2 h, filtering, and cleaning with deionized water and ethanolWashing for several times, and then drying in an oven at 60 ℃ for 6h to obtain the pure boron nitride nanotube.
Example 3: weighing 2g of magnesium boride powder and 1g of boron oxide powder, respectively placing the magnesium boride powder and the boron oxide powder into an alumina boat, wherein the magnesium boride powder is positioned in the front section of the boron oxide powder by about 10cm, and placing the magnesium boride powder and the boron oxide powder into a CVD (chemical vapor deposition) furnace. Removing air in the furnace chamber by Ar, heating to 1000 ℃, and introducing 300sccm of NH3The temperature is programmed to 1400 ℃ and kept for 180min, NH is closed after the reaction is finished3And cooling to room temperature in Ar atmosphere to obtain a white crude product. And then treating the obtained crude product with 1-4 mol/L hydrochloric acid at 85 ℃ for 1-2 h, filtering, washing with deionized water and ethanol for several times, and drying in a 60 ℃ oven for 6h to obtain the pure boron nitride nanotube.
Example 4: 0.5g of lithium piece and 4g of boron oxide powder are weighed and respectively put into an alumina boat, the lithium piece is positioned at about 5cm in the front section of the boron oxide powder and is put into a CVD furnace. Removing air in the furnace chamber by Ar, heating to 700 ℃, and introducing 300sccm of NH3The temperature is programmed to 1200 ℃ and kept for 4h, and NH is closed after the reaction is finished3And cooling to room temperature in Ar atmosphere to obtain a white crude product. And then treating the obtained crude product with 1-4 mol/L hydrochloric acid at 85 ℃ for 1-2 h, filtering, washing with deionized water and ethanol for several times, and drying in a 60 ℃ oven for 9h to obtain the pure boron nitride nanotube.
Example 5: 2g of magnesium boride powder and 1g of boron oxide powder are weighed and respectively placed in an alumina boat, and a lithium plate is positioned in the front section of the boron oxide powder by about 10cm and is placed in a CVD furnace. Removing air from the furnace chamber with Ar, heating to 1100 deg.C, introducing 300sccm N2The temperature is programmed to 1700 ℃ and kept for 240min, and N is closed after the reaction is finished2And cooling to room temperature in Ar atmosphere to obtain a white crude product. And then treating the obtained crude product with hydrochloric acid with the concentration of 1-4 mol/L for 1-2 h at 40 ℃, filtering, washing with deionized water and ethanol for several times, and drying in an oven at 70 ℃ for 4h to obtain the pure boron nitride nanotube.
Example 6:0.5g of lithium piece and 4g of boron oxide powder are weighed and respectively put into an alumina boat, the lithium piece is positioned at about 6cm in the front section of the boron oxide powder and is put into a CVD furnace. Removing air in the furnace chamber by Ar, heating to 900 ℃, and introducing 100sccm of NH3The temperature is programmed to 1500 ℃ and kept for 100min, NH is closed after the reaction is finished3And cooling to room temperature in Ar atmosphere to obtain a white crude product. And then treating the obtained crude product with 1-4 mol/L hydrochloric acid at 85 ℃ for 1-2 h, filtering, washing with deionized water and ethanol for several times, and drying in a 60 ℃ oven for 6h to obtain the pure boron nitride nanotube.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
Throughout this specification, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the composition of the present teachings also consist essentially of, or consist of, the recited components, and the process of the present teachings also consist essentially of, or consist of, the recited process steps.
Claims (10)
1. A method for batch preparation of boron nitride nanotubes, the method comprising:
respectively arranging active metal and/or active metal boride and a boron source in a reaction system of a nitrogen source atmosphere;
heating the reaction system to 1200-1700 ℃, and carrying out heat preservation reaction to obtain a crude product;
and carrying out post-treatment on the crude product to obtain the boron nitride nanotube.
2. The method for mass production of boron nitride nanotubes according to claim 1, comprising: disposing an active metal and/or an active metal boride, respectively, a boron source in a chemical vapor deposition system;
and heating the chemical vapor deposition system to 700-1100 ℃ in a protective atmosphere, and introducing a nitrogen source to obtain the reaction system.
3. The method for batch production of boron nitride nanotubes according to claim 2, wherein the temperature of the chemical vapor deposition system is raised to 700-1100 ℃ at a temperature raising rate of 2-30 ℃/min.
4. The batch production method of boron nitride nanotubes according to claim 1, wherein the active metal is selected from one or a combination of magnesium and lithium; and/or, the active metal boride is selected from magnesium boride;
and/or the active metal and the active metal boride are in the form of particles, strips, sheets or strips;
and/or, the boron source is selected from one or a combination of boron oxide, boric acid or borate; the nitrogen source is selected from one or a combination of ammonia gas and nitrogen gas.
5. The method for mass production of boron nitride nanotubes according to claim 1, comprising: and (3) carrying out heat preservation reaction on the reaction system at 1200-1700 ℃ for 1-4 h to obtain a crude product.
6. The batch production method of boron nitride nanotubes according to claim 1, wherein the post-treatment comprises: and carrying out acid washing and drying treatment on the crude product to obtain the boron nitride nanotube.
7. The method for mass production of boron nitride nanotubes according to claim 6, comprising: and (3) pickling the crude product at the temperature of 40-90 ℃ for 1-2 h, and drying at the temperature of 50-100 ℃ for 3-9 h to obtain the boron nitride nanotube.
8. The method of claim 1, wherein the active metal and/or the active metal boride and the boron source are respectively carried in a high temperature reaction boat, and the high temperature reaction boat is made of one material selected from the group consisting of alumina, silicon nitride, and zirconia.
9. The batch production method of boron nitride nanotubes according to claim 1, wherein the active metal and/or active metal boride is located at the front end of the boron source in the direction of introducing the nitrogen source into the reaction system, and the distance between the active metal and/or active metal boride and the boron source is 5-10 cm.
10. The boron nitride nanotubes prepared by the method of any one of claims 1 to 9, wherein the tube diameter of the boron nitride nanotubes is 20 to 40nm and the tube length is 80 to 180 μm.
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Cited By (2)
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| CN113353899A (en) * | 2021-05-24 | 2021-09-07 | 上海硼矩新材料科技有限公司 | Preparation method of boron nitride nanotube, boron nitride nanotube and application of boron nitride nanotube |
| CN115259111A (en) * | 2022-05-09 | 2022-11-01 | 上海交通大学 | Preparation method of boron nitride nanotube |
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| Publication number | Priority date | Publication date | Assignee | Title |
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