CN114524418B - Preparation method of hammer-shaped short boron nitride nanotube - Google Patents

Preparation method of hammer-shaped short boron nitride nanotube Download PDF

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CN114524418B
CN114524418B CN202210141952.XA CN202210141952A CN114524418B CN 114524418 B CN114524418 B CN 114524418B CN 202210141952 A CN202210141952 A CN 202210141952A CN 114524418 B CN114524418 B CN 114524418B
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boron nitride
hammer
nitride nanotube
shaped short
iron content
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CN114524418A (en
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李艳娇
郭剑锋
吕秋娟
王学仁
芦静
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Rocket Force University of Engineering of PLA
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    • 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
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract

The invention discloses a preparation method of a hammer-shaped short boron nitride nanotube, which comprises the following steps: 1. boron oxide and magnesium metalMixing and ball milling the powder to obtain solid powder; 2. placing the solid powder into a porcelain boat, placing a nickel-chromium alloy silk screen with low iron content on the porcelain boat, heating to 1250-1350 ℃ under the protection of argon, introducing high-purity ammonia gas for heat preservation, and depositing to obtain the hammer-shaped short boron nitride nanotube. The invention carries out ball milling activation on boron oxide and magnesium powder and then carries out catalysis at high temperature to generate B 2 O 2 The gas is diffused on the nichrome wire mesh and reacts with ammonia gas to generate BN nano tubes, the growth speed of the BN nano tubes generated by catalysis is controlled through the low iron content of the nichrome wire mesh, and the short boron nitride nano tubes in the shape of a stick are ensured to be obtained by combining a gas-liquid-solid growth mechanism.

Description

Preparation method of hammer-shaped short boron nitride nanotube
Technical Field
The invention belongs to the technical synthesis field of hexagonal boron nitride micro-nano materials, and particularly relates to a preparation method of a hammer-shaped short boron nitride nanotube.
Background
Boron nitride has the molecular formula BN, and is a graphite-like layered structure material composed of nitrogen (N) atoms and boron (B) atoms. BN nanomaterial refers to BN material having at least one dimension in the nanoscale range in three dimensions. Because of the small-size effect, the BN nano material has the advantages of high specific surface area, good adsorptivity and the like on the basis of having good mechanical property, higher thermal conductivity, remarkable electrical insulation, excellent chemical stability and excellent oxidation resistance of the bulk BN material. The unique properties enable the BN nano material to have good application prospects in the fields of biological probes, photoelectric instruments, humidity sensing, hydrogen storage media and the like, and particularly can show the advantages in high temperature and corrosive environments.
The research on BN nano materials relates to BN nano materials with various morphologies such as nano tubes, nano wires, nano sheets, nano spheres and the like, wherein the BN nano materials are the earliest and most mature. The BN nanotubes reported in the prior literature are bamboo joint type, cylinder type, ripple type and the like. The length is generally longer, more than about ten micrometers. Short BN nanotubes with a length below 5 μm have not been reported nor are hammer-like BN nanotubes. The BN nanotubes of different sizes and morphologies will have different properties and will have different application areas. Therefore, it is very necessary to prepare boron nitride nanotubes with different lengths and morphologies.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a hammer-shaped short boron nitride nanotube aiming at the defects in the prior art. The method comprises the steps of ball milling and activating boron oxide and magnesium powder to generate B in an annealing process 2 O 2 The gas is diffused on the nichrome silk screen and reacts with ammonia gas to generate BN nano tubes, the growth speed of the BN nano tubes generated by catalysis is controlled through the low iron content of the nichrome silk screen, and the B atoms and the N atoms are combined with a gas-liquid-solid growth mechanism which is formed by reaction after the B atoms and the N atoms are absorbed into nichrome small liquid drops to be saturated, so that the length of the BN nano tubes is effectively ensured to be shorter, a club-shaped structure is formed, and the club-shaped short boron nitride nano tubes are obtained.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the hammer-shaped short boron nitride nanotube is characterized by comprising the following steps of:
firstly, mixing boron oxide and metal magnesium powder according to a molar ratio of 1:1.5-1:2.5, and then adopting a planetary ball mill to ball-mill for 2-12 hours in a protective atmosphere to obtain solid powder with a particle size of 2-10 mu m;
and step two, placing the solid powder obtained in the step one in a porcelain boat, placing a nickel-chromium alloy screen with low iron content at the central position of the upper part of the porcelain boat, then closing an argon valve when the temperature is raised to 1250-1350 ℃ from room temperature at a speed of 10 ℃/min under the protection of argon, introducing high-purity ammonia gas, preserving heat for 2-8 hours, naturally cooling to room temperature under a protective atmosphere after stopping introducing the high-purity ammonia gas, and depositing the obtained gray-white substance on the nickel-chromium alloy screen to obtain the club-shaped short boron nitride nanotube.
The invention oxidizesThe boron and the metal magnesium powder are mixed and ball-milled to obtain solid powder, the forming process and the production quantity of the BN nano tube are effectively regulated by controlling the mole ratio of raw material boron oxide to catalyst metal magnesium powder, and the morphology of the BN nano tube is further controlled, so that the hammer-shaped short boron nitride nano tube is obtained; then placing the solid powder in a porcelain boat, placing a nickel-chromium alloy silk screen with low iron content at the upper part of the porcelain boat, firstly introducing argon to remove air, heating to 1250-1350 ℃, then introducing high-purity ammonia gas, and carrying out heat preservation annealing, wherein in the process, magnesium powder is used as a catalyst to be mixed with raw material boron oxide in a ball milling mode for activation, and then B is generated at a high temperature 2 O 2 And the gas is diffused to the low-iron-content nichrome wire mesh, and the nichrome wire mesh forms BN nanotubes through vapor deposition and grows slowly under the slow catalysis of iron in the low-iron-content nichrome wire mesh and the synergistic combined catalysis of nickel and chromium, so that the short boron nitride nanotubes with shorter length are obtained. According to the invention, a low catalytic speed is formed by adopting the nickel-chromium alloy wire mesh with low iron content, so that the BN nano tube grows slowly, the short boron nitride nano tube is prepared, the defects of too high growth speed of the BN nano tube and longer boron nitride nano tube prepared due to too strong catalytic performance of the nickel-chromium alloy wire mesh with high iron content are avoided, and the nickel-chromium alloy wire mesh with low iron content is generally placed at the central position of the upper part of the porcelain boat so as to facilitate the circulation of reaction gas; meanwhile, the surface layer of the nichrome wire mesh forms nichrome small liquid drops at high temperature, and the nichrome small liquid drops are diffused to B on the nichrome wire mesh 2 O 2 B atoms in the gas and N atoms in the ammonia gas of the reaction gas are absorbed and dissolved in the nichrome small liquid drops, as the concentration of the B atoms and the N atoms increases and gradually reach a saturated state, BN generated by the reaction is separated out from the small liquid drops and forms a capsule-shaped BN, the capsule-shaped BN is one section of the bamboo-shaped nanotube, the diameter of the capsule-shaped BN is larger, a plurality of bamboo joints are connected together along with the extension of the reaction time to form the bamboo-shaped BN nanotube, meanwhile, the formed bamboo-shaped BN nanotube is gradually elongated and has a smaller diameter under the action of internal stress, and the first section diameter of the bamboo-shaped nanotube is minimum and the last section of internal stress action time is prolonged due to the longest action time of the internal stressThe diameter is the largest, thus forming the short BN nano tube with thick end and thin end.
The preparation method of the hammer-shaped short boron nitride nanotube is characterized in that the protective atmosphere in the first step and the second step is nitrogen, helium, neon, argon, krypton, xenon or radon.
The preparation method of the hammer-shaped short boron nitride nanotube is characterized in that the flow rate of argon in the second step is 20-100 mL/min, and the flow rate of high-purity ammonia is 50-200 mL/min. The invention can quickly and fully exhaust the air in the reaction device by controlling the flow of the argon; by controlling the flow of the high-purity ammonia gas, the reaction speed is effectively controlled, and the problem that the reaction speed is too high due to the overlarge amount of the high-purity ammonia gas is avoided, so that the diameter of the BN nanotube generated by the reaction is large, and the club-shaped short boron nitride nanotube cannot be obtained.
The preparation method of the hammer-shaped short boron nitride nano tube is characterized in that the nickel-chromium alloy wire mesh with low iron content in the second step is replaced by a wire mesh with low iron content, a metal porous material, a metal and ceramic solid sheet, a ceramic wire mesh and a ceramic porous material.
The preparation method of the hammer-shaped short boron nitride nanotube is characterized in that the solid powder in the first step contains catalyst metal magnesium powder and iron powder produced by ball milling. During the mixing ball milling process of boron oxide and metal magnesium powder, a very small amount of iron powder is introduced due to the friction and collision effect of grinding balls (usually stainless steel grinding balls), and the iron powder also has the catalytic effect, thereby being beneficial to catalyzing the boron oxide reaction to generate B 2 O 2 And (3) gas.
The preparation method of the hammer-shaped short boron nitride nanotube is characterized in that the iron content in the nickel-chromium alloy wire mesh with low iron content in the second step is lower than 1wt%. The nickel-chromium alloy wire mesh with the iron content effectively controls the growth speed of the BN nano tube and is beneficial to obtaining the hammer-shaped short boron nitride nano tube.
The preparation method of the hammer-shaped short boron nitride nanotube is characterized in that the diameter of the thick end of the hammer-shaped short boron nitride nanotube in the second step is 100-300 nm, the diameter of the thin end of the hammer-shaped short boron nitride nanotube is 20-60 nm, and the length of the hammer-shaped short boron nitride nanotube is 2-3 mu m.
Compared with the prior art, the invention has the following advantages:
1. the invention carries out ball milling activation on raw material boron oxide and catalyst magnesium powder and then carries out catalysis at high temperature to generate B 2 O 2 The gas is diffused to a nichrome wire mesh, and ammonia gas and B are catalyzed by iron, nickel and chromium in the nichrome wire mesh 2 O 2 The BN nano tube is generated by gas reaction, the growth speed of the BN nano tube is controlled by the low iron content of the nichrome silk screen, and the B atoms and N atoms are absorbed into the nichrome droplet to be saturated, and then the gas, liquid and solid growth mechanism of the BN nano tube is separated out by reaction, so that the length of the BN nano tube is effectively ensured to be short, a club-shaped structure is formed, and the club-shaped short boron nitride nano tube is obtained.
2. The thick end diameter of the hammer-shaped short boron nitride nano tube prepared by the invention is 100 nm-300 nm, the diameter of the thin end is 20 nm-60 nm, the length is 2 mu m-3 mu m, and the length is shorter, so that the hammer-shaped short boron nitride nano tube is not easy to wind and agglomerate and easy to disperse uniformly when being used as a composite material additive, and plays a role in improving the mechanical property, heat transfer property, high temperature resistance, corrosion resistance and other properties of a matrix material.
3. The hammer-shaped short boron nitride nanotube prepared by the invention is used as a composite material additive, effectively increases the mechanical property, heat transfer property, high temperature resistance and corrosion resistance of a composite material matrix, and is suitable for the fields of high-performance structural materials and functional materials for equipment and machinery.
4. The raw materials of boron oxide powder, metal magnesium powder, nickel-chromium alloy silk screen, argon and high-purity ammonia gas adopted by the preparation method of the invention belong to common chemical raw materials which are industrially produced, and the raw materials are wide in source, low in cost, easy to obtain, nontoxic and harmless.
5. According to the invention, the reaction precursor is prepared through a ball milling activation process, and then the final product can be prepared through heating through a conventional tubular atmosphere protection annealing furnace, so that the requirement on preparation equipment is low, and the reaction temperature is reduced through ball milling activation, so that the energy consumption and the production cost of the whole preparation process are reduced.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
Fig. 1 is an XRD pattern of a short boron nitride nanotube in the form of a hammer prepared in example 1 of the present invention.
Fig. 2a is an SEM image of a short boron nitride nanotube in the form of a hammer prepared in example 1 of the present invention.
Fig. 2b is an EDS spectrum of the surface of a nichrome wire mesh with a hammer-like short boron nitride nanotube deposited thereon in example 1 of the present invention.
Fig. 3 is a TEM image of a short boron nitride nanotube in the form of a hammer prepared in example 1 of the present invention.
FIG. 4 is a selected area diffraction pattern of a short boron nitride nanotube in the form of a hammer prepared in example 1 of the present invention.
FIG. 5 is a high resolution transmission electron micrograph of a single hammer-like short boron nitride nanotube prepared in example 1 of the present invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
firstly, mixing boron oxide and metal magnesium powder according to a molar ratio of 1:2, placing the mixture in a planetary ball mill, and then ball milling for 4 hours in a protective atmosphere nitrogen in a positive and negative alternate operation mode to obtain solid powder with a particle size of 2-10 mu m;
placing the solid powder obtained in the first step in a porcelain boat, placing a nickel-chromium alloy wire mesh with the length of 30mm and the width of 30mm and the iron content of 0.7wt% at the central position of the upper part of the porcelain boat, then closing an argon valve when the temperature is raised to 1300 ℃ from room temperature at the speed of 10 ℃/min under the protection of argon with the flow of 20mL/min, introducing ammonia with the mass purity of 99.99% at the flow of 150mL/min, preserving the temperature for 6 hours, stopping introducing ammonia, naturally cooling to the room temperature under the protection of argon atmosphere, and depositing the obtained gray-white substance on the nickel-chromium alloy wire mesh to obtain the club-shaped short boron nitride nanotube.
The nitrogen in the protective atmosphere in the first step of the embodiment can be replaced by helium, neon, argon, krypton, xenon or radon; the protective atmosphere argon in the second step can be replaced by nitrogen, helium, neon, krypton, xenon or radon; the flow rate of the argon gas which is introduced in the second step can be a value ranging from 20mL/min to 100mL/min except 20 mL/min.
Fig. 1 is an XRD pattern of the short boron nitride nanotubes prepared in this example, and as can be seen from fig. 1, sharp and clear BN phase diffraction peaks exist in the XRD pattern of the short boron nitride nanotubes, which indicates that the product in this example is boron nitride and has good crystallization, and meanwhile, since the short boron nitride nanotubes grow on the nichrome wire mesh, there are strong nickel peaks and chromium peaks in the figure.
Fig. 2a is an SEM image of a short hammer-shaped boron nitride nanotube prepared in this example, and as can be seen from fig. 2a, the short hammer-shaped boron nitride nanotube prepared in this example is uniform and dense on the surface of a nichrome wire mesh, and has a thick end, a thin end, a uniform length and diameter, a length of about 2 μm to 3 μm, a thick end diameter of about 100nm to 300nm, and a thin end diameter of about 20nm to 60nm.
Fig. 2B is an EDS spectrum of the surface of a nichrome wire mesh for depositing a hammer-like short boron nitride nanotube in this embodiment, and as can be seen from fig. 2B, the nichrome wire mesh mainly contains B, N, O, al, mg, cr, ni and other elements, wherein Al is caused by a porcelain boat, O is derived from magnesium oxide, mg is derived from magnesium oxide, cr and Ni are derived from the wire mesh, the rest elements are B and N, and the atomic ratio is approximately 1:1, and accords with the stoichiometric characteristics of BN material, which illustrates that the rod-like structure obtained by depositing the method in this embodiment on the surface of the nichrome wire mesh is BN.
Fig. 3 is a TEM image of a short boron nitride nano tube in the shape of a hammer prepared in this example, and as can be seen from fig. 3, the short boron nitride nano tube in the shape of a bamboo joint hollow tubular structure has a thick end, a thin end, a thick end with a diameter of about 200nm, a thin end with a diameter of about 50nm, and both the thick end and the thin end are closed structures.
Fig. 4 is a selective area diffraction pattern of the short boron nitride nanotubes of the mallet shape prepared in this example, and it can be seen from fig. 4 that the product component of this example is hexagonal boron nitride.
Fig. 5 is a high resolution transmission electron microscope photograph of the single hammer-shaped short boron nitride nanotube prepared in this embodiment, and as can be seen from fig. 5, the interplanar spacing of the single hammer-shaped short boron nitride nanotube is about 0.334nm, which accords with the interplanar spacing of hexagonal boron nitride, further illustrating that the nanotube is a well crystallized boron nitride nanotube.
As can be seen from fig. 1 to 5, the product prepared by the method of this example is a hexagonal boron nitride nanotube with good crystallization.
Example 2
This embodiment differs from embodiment 1 in that: in the second step, the temperature is raised to 1250 ℃.
Example 3
This embodiment differs from embodiment 1 in that: and in the second step, the temperature is raised to 1350 ℃.
Example 4
This embodiment differs from embodiment 1 in that: in the first step, the mol ratio of the boron oxide to the metal magnesium powder is 1:1.5.
Example 5
This embodiment differs from embodiment 1 in that: in the first step, the mol ratio of the boron oxide to the metal magnesium powder is 1:2.5.
Example 6
This embodiment differs from embodiment 1 in that: the ball milling time in the first step is 2 hours.
Example 7
This embodiment differs from embodiment 1 in that: the ball milling time in the first step is 6 hours.
Example 8
This embodiment differs from embodiment 1 in that: the ball milling time in the first step is 8 hours.
Example 9
This embodiment differs from embodiment 1 in that: the ball milling time in the first step is 10 hours.
Example 10
This embodiment differs from embodiment 1 in that: the ball milling time in the first step is 12 hours.
Example 11
This embodiment differs from embodiment 1 in that: and in the second step, the heat preservation time is 2 hours.
Example 12
This embodiment differs from embodiment 1 in that: and in the second step, the heat preservation time is 4 hours.
Example 13
This embodiment differs from embodiment 1 in that: and in the second step, the heat preservation time is 8 hours.
Example 14
This embodiment differs from embodiment 1 in that: the flow of the high-purity ammonia gas in the second step is 50mL/min.
Example 15
This embodiment differs from embodiment 1 in that: the flow of the high-purity ammonia gas in the second step is 200mL/min.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.

Claims (5)

1. The preparation method of the hammer-shaped short boron nitride nanotube is characterized by comprising the following steps of:
firstly, mixing boron oxide and metal magnesium powder according to a molar ratio of 1:1.5-1:2.5, and then adopting a planetary ball mill to ball-mill for 2-12 hours in a protective atmosphere to obtain solid powder with a particle size of 2-10 mu m;
placing the solid powder obtained in the first step in a porcelain boat, placing a nickel-chromium alloy screen with low iron content at the central position of the upper part of the porcelain boat, then closing an argon valve when the temperature is raised to 1250-1350 ℃ from room temperature at a speed of 10 ℃/min under the protection of argon, introducing high-purity ammonia gas, preserving heat for 2-8 hours, naturally cooling to room temperature in a protective atmosphere after stopping introducing the high-purity ammonia gas, and depositing an off-white substance on the nickel-chromium alloy screen to obtain the club-shaped short boron nitride nanotube; the iron content in the nickel-chromium alloy silk screen with low iron content is lower than 1wt%; the diameter of the thick end of the hammer-shaped short boron nitride nanotube is 100-300 nm, the diameter of the thin end of the hammer-shaped short boron nitride nanotube is 20-60 nm, and the length of the hammer-shaped short boron nitride nanotube is 2-3 mu m.
2. The method for preparing the hammer-like short boron nitride nanotube according to claim 1, wherein the protective atmosphere in the first and second steps is nitrogen, helium, neon, argon, krypton, xenon or radon.
3. The method for preparing the hammer-shaped short boron nitride nanotube according to claim 1, wherein the flow rate of argon in the second step is 20-100 mL/min, and the flow rate of high-purity ammonia is 50-200 mL/min.
4. The method for preparing a hammer-like short boron nitride nanotube according to claim 1, wherein the nichrome wire mesh with low iron content in the second step is replaced by a wire mesh with low iron content and a metal porous material, a metal and ceramic solid sheet, a ceramic wire mesh and a ceramic porous material.
5. The method for preparing the hammer-like short boron nitride nanotubes according to claim 1, wherein in the step one, the solid powder contains catalyst metal magnesium powder and iron powder produced by ball milling.
CN202210141952.XA 2022-02-16 2022-02-16 Preparation method of hammer-shaped short boron nitride nanotube Active CN114524418B (en)

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* Cited by examiner, † Cited by third party
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CH490271A (en) * 1966-03-09 1970-05-15 Lonza Werke Gmbh Process for the production of hexagonal boron nitride
DE2461821C3 (en) * 1974-12-30 1984-10-18 Elektroschmelzwerk Kempten GmbH, 8000 München Process for the production of hexagonal boron nitride
JPS61215203A (en) * 1985-03-21 1986-09-25 Toshiba Tungaloy Co Ltd Synthesis of cubic boron nitride
CN100369806C (en) * 2006-06-27 2008-02-20 华南理工大学 Method for synthesizing single shape boron nitride nano tube
CN108545708B (en) * 2018-03-14 2021-08-24 中国人民解放军火箭军工程大学 Preparation method of coralline hexagonal boron nitride micro-nano tube sheet composite structure
CN111569530B (en) * 2020-05-26 2021-11-23 中国人民解放军火箭军工程大学 Super-hydrophobic filter screen and preparation method thereof

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