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Method and device for preparing BN fiber through electron beam irradiation crosslinking

An electron beam irradiation, electron beam technology, applied in the directions of irradiation device, fiber treatment, fiber chemical characteristics, etc., can solve the problem of lack of infusible treatment methods for BN fibrils, and achieve improved mechanical properties, excellent dielectric properties, and crystallinity. good effect

Active Publication Date: 2017-05-31
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing patents and literature reports on the preparation of BN fibers, there is a lack of non-melting treatment methods for BN fibrils.

Method used

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  • Method and device for preparing BN fiber through electron beam irradiation crosslinking
  • Method and device for preparing BN fiber through electron beam irradiation crosslinking
  • Method and device for preparing BN fiber through electron beam irradiation crosslinking

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The first step of melt spinning: heat the polyborazane precursor to 170°C in the feed tank, stand still for 4 hours, exhaust, then lower the temperature to 150°C, and control the spinning pressure to 0.5MPa to obtain Polyborazane fibrils 100g. The diameter of the spinneret hole is 0.4 mm, and the spinning speed is 600 m / min.

[0040] The second step of electron beam irradiation: the fiber precursors obtained in the first step are placed in a crosslinking box and protected by nitrogen gas. Then carry out cross-linking by electron beam irradiation, the energy is 1.5 MeV, the beam current is 2.5 mA, and the irradiation is 3.0 hours. During the irradiation process, first pass the cooling water to the cross-linking box to cool down, so as to prevent the temperature from being too high during the cross-linking process, resulting in the melting of the filaments; secondly, by adjusting the tension of the filaments, the shrinkage of the fibrils is controlled at 2%- 5%.

[004...

Embodiment 2

[0044] The first step of melt spinning: heat the polyborazane precursor to 170°C in the feed tank, stand still for 4 hours, exhaust, then lower the temperature to 150°C, and control the spinning pressure to 0.5MPa to obtain Polyborazane fibrils 100g. The diameter of the spinneret hole is 0.4 mm, and the spinning speed is 600 m / min.

[0045] The second step of electron beam irradiation: the fiber precursors obtained in the first step are placed in a crosslinking box and protected by nitrogen gas. Then carry out cross-linking by electron beam irradiation, the energy is 2.5 MeV, the beam current is 1.5 mA, and the irradiation is 2.5 hours. During the irradiation process, first pass the cooling water to the cross-linking box to cool down, so as to prevent the temperature from being too high during the cross-linking process, resulting in the melting of the filaments; secondly, by adjusting the tension of the filaments, the shrinkage of the fibrils is controlled at 2%- 5%.

[004...

Embodiment 3

[0049] The first step of melt spinning: heat the polyborazane precursor to 170°C in the feed tank, stand still for 4 hours, exhaust, then lower the temperature to 150°C, and control the spinning pressure to 0.5MPa to obtain Polyborazane fibrils 100g. The diameter of the spinneret hole is 0.4 mm, and the spinning speed is 600 m / min.

[0050] The second step of electron beam irradiation: the fiber precursors obtained in the first step are placed in a crosslinking box and protected by nitrogen gas. Then carry out cross-linking by electron beam irradiation, the energy is 2.5 MeV, the beam current is 2.5 mA, and the irradiation is 2.0 hours. During the irradiation process, first pass the cooling water to the cross-linking box to cool down, so as to prevent the temperature from being too high during the cross-linking process, resulting in the melting of the filaments; secondly, by adjusting the tension of the filaments, the shrinkage of the fibrils is controlled at 2%- 5%.

[005...

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Abstract

The invention discloses a method and a device for preparing a BN fiber through electron beam irradiation crosslinking. The method comprises the following steps: (1) taking an organic polyborazine precursor as a raw material and performing melt spinning, thus obtaining a proto fiber; (2) irradiating the proto fiber with electron beam, thus obtaining BN non-melting fiber through electron beam irradiation crosslinking; (3) heating the beam treated in the last step, causing the residual free radical to further react to lose activity; (4) performing inorganic and ceramic treatment on the non-melting fiber, thus obtaining the BN fiber. According to the invention, a new non-melting treating technique is applied to the BN fiber; the proto fiber obtained after the treatment according to the technique can maintain the fiber morphology in the subsequent treatment processes, such as, low-temperature de-carbonization and high-temperature nitridation; the solid BN fiber with excellent crystallinity and dielectric property can be obtained; the mechanical property of the BN fiber can be greatly improved.

Description

technical field [0001] The present invention generally relates to a method and a device for preparing inorganic fibers, in particular to a method and a device for preparing BN fibers by electron beam irradiation crosslinking. Background technique [0002] BN fiber is an ideal high-temperature-resistant ceramic material with excellent corrosion resistance and electrical insulation. Its dielectric properties are especially outstanding in high-temperature and harsh environments. It can be used in oxidizing atmospheres below 900°C and inert atmospheres below 2800°C. used in . [0003] The preparation process of BN fiber mainly includes inorganic precursor method and organic precursor method. The inorganic precursor method is based on boric acid or B 2 o 3 As a raw material, B is obtained through high-temperature melting 2 o 3 fiber, then in NH 3 / N 2 After low-temperature nitriding and high-temperature treatment in the atmosphere, it is transformed into BN ceramic fiber. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/10D06M10/00G21K5/10
CPCD01F9/10D06M10/00G21K5/10
Inventor 张伟刚卢振西戈敏张金鹏乌琪琪
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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