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Preparation method for SiBCN nano ceramic fiber

A nano-ceramic fiber and nano-fiber technology, applied in the field of nano-ceramic fiber, can solve the problems of complex process, difficult synthesis of raw materials, high requirements of spinning process, etc., and achieve the effect of simple process and easy operation

Active Publication Date: 2019-05-24
NAT UNIV OF DEFENSE TECH
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The invention provides a preparation method of SiBCN nano ceramic fiber, which is used to overcome the defects of difficult synthesis of raw materials, high requirements on spinning process and complicated process in the prior art, and realize the preparation of SiBCN nano ceramic fiber with simple process and easy operation

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  • Preparation method for SiBCN nano ceramic fiber
  • Preparation method for SiBCN nano ceramic fiber
  • Preparation method for SiBCN nano ceramic fiber

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[0024] The present invention proposes a kind of preparation method of SiBCN nano ceramic fiber (refer to figure 1 ), including the following steps:

[0025] S1: Place polyacrylonitrile nanofibers in a container, and then replace the air atmosphere in the container with an inert atmosphere; use polyacrylonitrile nanofibers as a template.

[0026] S2: Inject a tetrahydrofuran solution of lithium aluminum hydride into the container after step S1, add methanol after reaction at room temperature; use lithium aluminum hydride to reduce the nitrile group to amino group.

[0027] S3: Take out the product fiber of step S2, place it in a tube furnace, raise the temperature from room temperature to 100°C under an inert atmosphere and keep it warm. Chlorosilane and boron trichloride; in the second stage, methylamine is introduced; trichlorosilane and boron trichloride are used to react with amino groups to introduce silicon and boron atoms, and then remove residual chlorine through methy...

Embodiment 1

[0045] The present embodiment proposes a kind of preparation method of SiBCN nano-ceramic fiber, comprises the following steps:

[0046] S1: Place 2g of polyacrylonitrile nanofibers in a sealed glass Erlenmeyer flask, and then replace the air atmosphere in the container with nitrogen;

[0047] S2: Inject 40 mL of lithium aluminum hydride tetrahydrofuran solution with a concentration of 1 mol / L into the container after step S1, and add 40 mL of methanol after 2 hours of reaction at room temperature;

[0048] S3: Take out the product fiber of step S2, place it in a tube furnace, raise the temperature from room temperature to 100°C under a nitrogen atmosphere and keep it warm for 2 hours; during the first 1 hour of keeping warm, feed trichlorosilane and Boron trichloride; During the last 1h of the heat preservation period, feed methylamine at a flow rate of 100mL / min;

[0049] S4: After step S3, raise the temperature from 100°C to 1500°C at a heating rate of 5°C / min in a nitroge...

Embodiment 2

[0054] The present embodiment proposes a kind of preparation method of SiBCN nano-ceramic fiber, comprises the following steps:

[0055] S1: Place 10 g of polyacrylonitrile nanofibers in a sealed glass Erlenmeyer flask, and then replace the air atmosphere in the container with nitrogen;

[0056] S2: Inject 100 mL of a tetrahydrofuran solution of lithium aluminum hydride with a concentration of 1 mol / L into the container after step S1, and add 100 mL of methanol after 2 hours of reaction at room temperature;

[0057] S3: Take out the product fiber of step S2, place it in a tube furnace, raise the temperature from room temperature to 100°C under a nitrogen atmosphere and keep it warm for 2 hours; during the first 1 hour of keeping warm, feed trichlorosilane and Boron trichloride; during the last 1h of the heat preservation period, feed methylamine at a flow rate of 500mL / min;

[0058] S4: After step S3, the temperature was raised from 100° C. to 1600° C. at a rate of 8° C. / min ...

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Abstract

The invention discloses a preparation method for a SiBCN nano ceramic fiber. The preparation method comprises the following steps: 1) using a polyacrylonitrile fiber as a nanofiber template; 2) reducing a nitrile group into an amino group by using lithium aluminum hydride; 3) using trichlorosilane and boron trichloride to react with the amino group and introducing silicon and boron atoms, and removing residual chlorine through methylamine; 4) acquiring the SiBCN nano ceramic fiber through high-temperature ceramics. Compared with an existing ceramic fiber preparation method, the provided preparation method for the SiBCN nano ceramic fiber is capable of solving problems that a raw material polymer used by the existing SiBCN nano ceramic fiber preparation method is difficultly synthesized, the requirement to a spinning technology is high, the preparation technology is complicated and the like. The provided SiBCN nano ceramic fiber is 50-500 nm in monofilament diameter, 0.1-0.2 mg / cm<3> indensity, 20-40 W / m*k in heat conductivity, and 7-15 in dielectric constant, and can be used as good high-temperature heat-insulating material and high-temperature wave-absorbing material.

Description

technical field [0001] The invention relates to the technical field of nano ceramic fibers, in particular to a preparation method of SiBCN nano ceramic fibers. Background technique [0002] Nanofibers can be formed by a variety of methods, such as electrospinning, melt blown and flash spinning, etc., which can be directly made into non-woven fabrics or three-dimensional nano stacks to obtain aerogels. However, these commonly used methods are generally used for carbon nanofibers, oxide nanofibers, etc., and currently only literatures have reported the preparation of SiBCN nanoceramic fibers by electrospinning. Because the raw materials of SiBCN nanofibers are sensitive to air and moisture, harsh raw material synthesis and spinning forming equipment are required, especially an anhydrous and oxygen-free spinning environment, the process is complex, and it is difficult to operate and prepare in a conventional laboratory. Contents of the invention [0003] The invention provid...

Claims

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Application Information

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IPC IPC(8): D01F9/08C04B35/622
Inventor 邵长伟张帅纪小宇
Owner NAT UNIV OF DEFENSE TECH
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