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Preparation method of SiBN(C) ceramic fiber

A ceramic fiber and fiber technology, which is applied in the field of high-performance non-oxide ceramic fiber, can solve the problems of reducing the performance of ceramic fiber, increasing production cost, and complicated operation, and achieves the effects of reliable source, convenient synthesis, and simple process

Inactive Publication Date: 2011-11-23
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the obtained polyborosilazane precursor is easily hydrolyzed, and the precursor obtained by melt spinning is hydrolyzed in the air, which affects the subsequent heat treatment and reduces the performance of the ceramic fiber.
Therefore, the entire melt spinning device needs to be placed under an inert atmosphere, which makes the operation complicated and increases the production cost
In addition, it is necessary to feed BCl in the non-melting process 3 , causing pollution to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Vacuumize and dry the reactor equipped with a stirring device three times with nitrogen to remove the air and water in it. Use a syringe to add the toluene solution of trichloroborazine (TCB) into the reactor. Cool to -20°C;

[0023] (2) The molar ratio of isopropylamine and TCB is 3:1, and the excess ratio of triethylamine is added to the reactor;

[0024] Add the isopropylamine into the reactor with stirring device pre-cooled to -20°C by means of syringe injection, and keep stirring. The reaction proceeds rapidly, and a large amount of heat is released, the temperature of the chamber system rises and a white precipitate is produced;

[0025] (3) When the temperature of the system no longer rises and no more white precipitates are produced, keep the temperature of the system at room temperature, filter the obtained product under the protection of dry nitrogen, and place the obtained filtrate in a reaction chamber with a condenser, a cracking column, and a reflux d...

Embodiment 2

[0032] (1) Vacuumize and dry the reactor with nitrogen three times to remove the air and moisture in it, add the xylene solution of TCB into the reactor with a syringe, and pre-cool the reactor to -20°C;

[0033] (2) The molar ratio of n-propylamine and TCB is 2:1, and the excess ratio of triethylamine is added to the reactor;

[0034] Add n-propylamine into the reactor with stirring device pre-cooled to -20°C by syringe injection, and keep stirring. The reaction proceeds rapidly, and a large amount of heat is released, the temperature of the chamber system rises and a white precipitate is produced;

[0035] (3) When the temperature of the system no longer rises and no more white precipitates are produced, continue to stir for 5 hours, then pass the molar ratio of methylamine gas and TCB into the reaction system at a ratio of 1:1, and react until no more white precipitates are produced. The temperature of the system was kept at room temperature, and the reaction was carried o...

Embodiment 3

[0042] (1) Vacuumize and dry the reactor with nitrogen three times to remove the air and moisture in it, add the xylene solution of TCB into the reactor with a syringe, and pre-cool the reactor to -20°C;

[0043] (2) The molar ratio of n-propylamine and TCB is 2:1, and the excess ratio of triethylamine is added to the reactor;

[0044] Add n-propylamine into the reactor with stirring device pre-cooled to -20°C by syringe injection, and keep stirring. The reaction proceeds rapidly, and a large amount of heat is released, the temperature of the chamber system rises and a white precipitate is produced;

[0045] (3) When the temperature of the system no longer rises and no more white precipitates are produced, continue to stir for 5 hours, then pass the molar ratio of methylamine gas and TCB into the reaction system at a ratio of 1:1, and react until no more white precipitates are produced. The temperature of the system was kept at room temperature, and the reaction was carried o...

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PUM

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Abstract

The invention discloses a preparation method of a SiBN(C) ceramic fiber. The method comprises the following steps of: using alkyl amine and B-trichloroborazine as initial raw materials, and triethylamine as a precipitating agent; adding alkyl amine and TCB in a mo;ar ratio of 3:1, and an excess amount of triethylamine into a reactor for reaction; filtering products after the reaction and obtaining a filtrate which is an alkyl amino borazine monomer; carrying out polymerization to the monomer with heating; cooling to obtain a poly alkyl amino borazine precursor; adding the poly alkyl amino borazine precursor and polycarbosilane in a mass ratio of 1:15-15:1 into a toluene or a xylene solution; depriving a solvent by reduced pressure distillation and carrying out melt spinning to a hybrid precursor; and carrying out curing treatment and pyrolysis to obtain a SiBN(C) ceramic fiber. The method of the invention has a high synthesis yield and a technology thereof is simple; and the melt spinning of the precursor is completed in a general melt spinning equipment environment and without protection of expensive inert atmosphere, and has low coats and high efficiency; so as to realize large scale production.

Description

technical field [0001] The invention relates to a method for preparing high-temperature-resistant and anti-oxidation ceramic fibers, in particular to a method for preparing SiBN (C) fibers from organosilicon polymers and organoboron polymers through high-temperature cracking conversion. It belongs to the field of high-performance non-oxide ceramic fiber. Background technique [0002] literature (see J. Euro. Ceram. Soc , 20, 2655 (2000)) showed that: when the content of B element is 5~16 wt%, Si 3 N 4 The effect of crystallization is more obvious, and its effect is not obvious outside this range. Based on this, the SiBNC multi-component ceramics and its fibers have shown good high temperature resistance. SiBN fibers both have Si 3 N 4 The advantages of fiber and BN fiber make up for the shortcomings of the two. It is a new type of structure-functional ceramic fiber, which has broad application prospects in hypersonic aircraft and new high-speed precision guided weapons...

Claims

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Application Information

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IPC IPC(8): C04B35/58C04B35/622
Inventor 王应德雷永鹏
Owner NAT UNIV OF DEFENSE TECH
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