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Small-diameter boron nitride nanotube and preparation method thereof

A boron nitride nanotube and small-diameter technology, which is applied in the field of nanomaterials, can solve the problems of complex preparation process, high reaction temperature, and high cost of raw materials, and achieve the effects of lower reaction temperature, simple preparation method, and improved matrix performance

Active Publication Date: 2022-04-01
ROCKET FORCE UNIV OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are very few reports on the preparation of boron nitride nanotubes with small diameters. The only reports have the disadvantages of high raw material cost, expensive equipment, complicated preparation process, and high reaction temperature.

Method used

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  • Small-diameter boron nitride nanotube and preparation method thereof
  • Small-diameter boron nitride nanotube and preparation method thereof
  • Small-diameter boron nitride nanotube and preparation method thereof

Examples

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Effect test

preparation example Construction

[0026] The preparation method of the small-diameter uniform boron nitride nanotube of the present invention comprises the following steps:

[0027] Step (1), put the weighed boron oxide powder in the zirconia ball milling tank, and add an appropriate amount of zirconia grinding balls, vacuumize and introduce an inert protective atmosphere, adopt the mode of forward and reverse alternating operation, ball mill 0.5~ After 12 hours, a uniformly mixed solid powder with a particle size of about 2-10 microns was obtained.

[0028] In step (2), the solid powder obtained in step (1) is placed in a porcelain boat, and the porcelain boat is placed in a tubular atmosphere protection annealing furnace, and the temperature is raised from normal temperature under the protection of 20-100mL / min inert protection atmosphere, The heating rate is 5-10°C / min. When the temperature rises to 300-500°C, the inert protective atmosphere valve is closed, and high-purity ammonia gas is introduced at a fl...

Embodiment 1

[0032] In step (1), put the weighed boron oxide powder in a zirconia ball mill jar, and add an appropriate amount of zirconia grinding balls, vacuumize and feed nitrogen gas, and use the forward and reverse alternate operation mode, and ball mill for 12 hours to obtain Mixed uniform solid powder, the particle size is about 2-10 microns.

[0033] Step (2), the solid powder obtained in step (1) is placed in Al 2 o 3 In the porcelain boat, the porcelain boat was placed in a tubular atmosphere protection annealing furnace, and the temperature was raised from room temperature under the protection of 100mL / min argon gas at a rate of 10°C / min. When the temperature rose to 300°C, the argon valve was closed, and the Inject high-purity ammonia gas with a flow rate of 50mL / min. When the temperature further rises to 1300°C, keep warm for 8 hours, then stop feeding ammonia gas, and then cool down to room temperature naturally under a protective atmosphere, and a beige substance is obtaine...

Embodiment 2

[0040] Change the reaction temperature of step (2) in Example 1 to 1250°C, and the other operations are the same as in Example 1. A large amount of beige substance grows in the porcelain boat, and the SEM photo shows that its morphology and structure are the same as those in Example 1. same, only slightly smaller in number.

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Abstract

The invention discloses a small-diameter boron nitride nanotube and a preparation method thereof, and the preparation method comprises the following steps: step 1, carrying out ball-milling activation on boron oxide powder by adopting a zirconium oxide ball-milling tank and zirconium oxide grinding balls, and putting the ball-milled powder into a container; step 2, heating from normal temperature at the heating rate of 5-10 DEG C / min under the condition of introducing the inert protective atmosphere, stopping introducing the inert protective atmosphere when the temperature is raised to 300-500 DEG C, then introducing high-purity ammonia gas, keeping the temperature for 2-8 hours after the temperature is raised to 1250-1350 DEG C, stopping introducing the high-purity ammonia gas, introducing the inert protective atmosphere, and naturally cooling to the room temperature, so as to obtain the high-purity ammonia-nitrogen composite material. And obtaining a white substance in the container, namely the small-diameter boron nitride nanotube. The required raw materials are low in price, equipment is simple, and cost is low. The diameter of the boron nitride nanotube prepared at a low temperature through a simple ball-milling annealing process is about 10-15 nm, and the size is uniform.

Description

technical field [0001] The invention belongs to the field of nanometer materials, and relates to a small-diameter boron nitride nanotube and a preparation method thereof. Background technique [0002] The molecular formula of boron nitride is BN, which is a graphite-like layered structure material composed of nitrogen (N) atoms and boron (B) atoms. BN nanomaterials refer to BN materials with at least one dimension in the nanoscale range in three-dimensional space. In 1995, Chopra and others successfully prepared boron nitride nanotubes (boron nitrideanotubes, abbreviated as BNNTs) by the plasma arc discharge method, which opened the prelude to the research on boron nitride nanotubes. For a long time, the research work on boron nitride nanotubes has mainly focused on the preparation, purification and application. However, most of the boron nitride nanotubes reported in the literature have a diameter of more than 50 nm, and there is a problem of non-uniform size. This will ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/064B82Y40/00
Inventor 李艳娇王鑫峰杜海霞王涵
Owner ROCKET FORCE UNIV OF ENG
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