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Chemical vapor crosslinking method for polyborosilazane fiber

A polyborosilazane, gas-phase cross-linking technology, applied in the chemical characteristics of fibers, chemical post-treatment of synthetic polymer rayon filaments, textiles and papermaking, etc. problem, to achieve the effect of being suitable for large-scale production, reducing the reaction temperature, and the process is simple

Active Publication Date: 2013-05-01
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the chemical cross-linking atmosphere used has a strong corrosive effect, which is unfavorable to the cross-linking equipment (see Chinese Patent No. ZL 200910311781.5)

Method used

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  • Chemical vapor crosslinking method for polyborosilazane fiber
  • Chemical vapor crosslinking method for polyborosilazane fiber
  • Chemical vapor crosslinking method for polyborosilazane fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) The FT IR spectrum of PBSZ fibrils is as follows figure 1 shown. The main characteristic peaks in the figure belong to: 3429 cm -1 、3383 cm -1 、1179 cm -1 : N-H; 2955 cm -1 、2858 cm -1 : C-H; 2125 cm -1 : Si-H; 1472 cm -1 、1386 cm -1 : B-N; 913 cm -1 : Si-N; 1252 cm -1 : Si-C.

[0041] Put the PBSZ fibrils in the tube furnace of the existing chemical vapor phase cross-linking system, and evacuate to 6×10 -2 Pa, then replace the gas in the system with nitrogen to normal pressure, repeat three times; (2) vacuum to 6×10 -2 After Pa, inject diborane gas to normal pressure; (3) program temperature rise to 50°C, reaction time 24h; (4) program temperature rise to 400°C, hold time 2h, cool to room temperature, and serve.

[0042] The FT IR spectrogram of gained crosslinked fiber is as figure 2 shown.

[0043] The obtained polyborosilazane crosslinked fiber gel content is 100%. Oxygen content analysis showed that the oxygen content of PBSZ fibrils was 0.84wt%...

Embodiment 2

[0047] Place the PBSZ fibrils in the existing chemical vapor phase cross-linking system equipment, vacuumize and replace the gas in the system with high-purity nitrogen or high-purity argon to normal pressure, repeat three times; Gas to normal pressure; (3) Program temperature rise to 80°C, reaction time 12h; (4) Program temperature rise to 350°C, holding time 6h, cool to room temperature, ready to serve.

[0048] The FT IR spectrogram of gained PBSZ cross-linked fiber and figure 2 Basically the same, only the intensity of the absorption peak is slightly different.

Embodiment 3

[0050] Put the PBSZ fibrils in the existing chemical vapor phase cross-linking system equipment, vacuumize and replace the gas in the system with high-purity nitrogen or high-purity argon to normal pressure, repeat three times; Pentaborane to normal pressure; (3) Program temperature rise to 100°C, reaction time 8h; (4) Program temperature rise to 400°C, holding time 2h. Let cool to room temperature and serve.

[0051] FT IR spectra of PBSZ cross-linked fibers and figure 2 Basically the same, only the intensity of the absorption peak is slightly different.

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Abstract

The invention discloses a chemical vapor crosslinking method for a polyborosilazane fiber, which comprises the following operation steps of (1) placing a polyborosilazane fibril in a chemical vapor crosslinking system, vacuumizing, displacing system gas with high-purity nitrogen or high-purity argon to a normal pressure, and repeating for three times, (2) introducing boron hydride compound gas to the normal pressure after vacuumizing, (3) conducting temperature programming to 50-100 DEG C for reaction for 0.5-25h, and (4) conducting temperature programming to 350-500 DEG C, keeping warm for 0.5-12h, and cooling to a room temperature. The method has the following advantages that (1) no catalyst is needed, no oxygen is needed, and a dehydrogenation coupled reaction can be conducted at a temperature below a melting point of polyborosilazane, so that crosslinking of the polyborosilazane fiber is realized; (2) no equipment change on the existing chemical vapor crosslinking system is needed; and (3) the method is simple in technology and is suitable for large-scale production.

Description

technical field [0001] The invention relates to a crosslinking method of polyborosilazane fibers, in particular to a chemical vapor phase crosslinking method of polyborosilazane fibers. Background technique [0002] Silicon-based nitride ceramic fiber is a kind of ceramic fiber with excellent comprehensive properties. Ceramic fiber-reinforced ceramic matrix composites prepared with it have important application prospects in the fields of aviation and aerospace. [0003] There are many types of silicon-based nitride ceramic fibers, mainly including SiBNC ceramic fibers, SiCN ceramic fibers, Si 3 N 4 Ceramic fiber, SiBN ceramic fiber, etc. [0004] SiBNC ceramic fiber has received more and more attention, mainly because it is different from pure SiC and Si 3 N 4 Compared with ceramics, the introduction of B or BN can significantly improve the thermal and mechanical properties of the material. The Siboramic fiber—SiBCN ceramic fiber produced by Bayer Company in Germany has...

Claims

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Application Information

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IPC IPC(8): D01F11/08D01F9/10C04B35/58C04B35/56
Inventor 谢征芳王军宋永才王浩邵长伟
Owner NAT UNIV OF DEFENSE TECH
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