Method for preparing SiBN(C) ceramic fibre

A technology of ceramic fiber and halosilane, which is applied in the field of preparation of high-temperature-resistant ceramic fiber, can solve problems such as unfavorable popularization and application, high activity of intermediate products, complicated process, etc., and achieve the effect of low raw material cost, reliable source, and convenient spinning

Inactive Publication Date: 2008-09-24
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method has high cost, complex process, and high activity of intermediate products, which is not conducive to popularization and application.

Method used

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  • Method for preparing SiBN(C) ceramic fibre
  • Method for preparing SiBN(C) ceramic fibre
  • Method for preparing SiBN(C) ceramic fibre

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038](1) boron trichloride and trichlorosilane are dissolved and preserved in normal hexane; (2) vacuumize repeatedly in the 250ml there-necked flask reactor with stirring, distillation unit and constant pressure funnel, fill dry nitrogen three times, Exclude the air and moisture in it, and cool the reactor to minus 15°C; (3) Take 0.15 mol of trichlorosilane and 0.15 mol of boron trichloride into a three-necked flask protected by dry nitrogen with a syringe, and then use a syringe to Take 0.9 mol of heptamethyldisilazane and inject it into the constant pressure funnel, while stirring, add heptamethyldisilazane to the mixed solution of the first two monomers in a dropwise manner; (4) drop After the addition, the temperature was raised to 260°C at a rate of 0.5°C / min, and the temperature was kept at 260°C for 10 hours; (5) the system was cooled to 150°C, and vacuum distillation was carried out for 0.5 hours to obtain the solid polyborosilazane precursor 12.2 g; (6) Place the po...

Embodiment 2

[0045] (1) Methyl boron dichloride and silicon tetrachloride are dissolved and stored in n-hexane; (2) Repeatedly vacuumize and dry in the 500ml three-necked flask reactor with stirring, distillation device and constant pressure funnel Nitrogen four times to remove the air and moisture, and cool the reactor to minus 10°C; (3) Take 0.15 mol of silicon tetrachloride and 0.3 mol of methyl boron dichloride with a syringe and inject them into the dry nitrogen-protected In the three-necked flask, use a syringe to take 1.5 mol of N-ethylhexamethyldisilazane and inject it into the constant pressure funnel. While stirring, add N-ethylhexamethyldisilazane dropwise into the mixture of the first two monomers; (4) after the dropwise addition, the temperature was raised to 300°C at a rate of 0.5°C / min, and kept at 300°C for 12 hours; (5) the system was lowered to 165°C, and the pressure was reduced Distill for 0.5 hour to obtain 14.6 g of solid polyborosilazane precursor; (6) place the poly...

Embodiment 3

[0047] (1) phenyl dichloroborane and ethyl trichlorosilane are dissolved and stored in n-hexane; (2) before the synthesis, the 250ml three-necked flask reactor with stirring, distillation device and constant pressure funnel is repeatedly extracted Vacuum and dry nitrogen for three times to remove the air and moisture, and cool the reactor to minus 10°C; (3) Take 0.15mol of butyltrichlorosilane and 0.15mol of phenyldichloroborane into the In a three-necked flask protected by dry nitrogen, inject 1 mol of N-methylhexaethyldisilazane with a syringe into a constant pressure funnel, and while stirring, add N-methylhexaethyldisilazane dropwise (4) After the dropwise addition, the temperature was raised to 320°C at a rate of 0.3°C / min, and kept at 320°C for 12 hours; (5) The system was cooled to 182°C , Distilled under reduced pressure for 1 hour to obtain 10.8 g of solid polyborosilazane precursor; (6) place the polyborosilazane precursor obtained in step (5) in a melt spinning devi...

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Abstract

The present invention provides a preparation method of SiBN(C) ceramic fiber. In the preparation method, silicon haloganide, boron halide and disilazane of small molecules are used as starting materials and are mixed according to a certain ratio; the temperature is raised to be between 150 and 500 DEG C and is maintained for a certain period; after the temperature is lowered, the mixture is processed through vacuum distillation and is cooled to be at the room temperature; thus the precursory of solid boron-containing polysilazane can be prepared and is then used for fusing filature to prepare precursor fiber of SiBN(C) ceramic fiber. Compared with the existing method, the preparation method has the advantages of low costs in raw materials, reliable source, higher synthetic yield, simple process and one-step preparation of the precursor; the fiber of the precursor is treated through chemical crosslinking that has high efficiency and is conducive to the integrative operation of spinning, non-melting treatment and sintering.

Description

technical field [0001] The invention relates to a method for preparing high-temperature-resistant ceramic fibers, in particular to a method for preparing SiBN (C) fibers from organosilicon polymers through high-temperature pyrolysis conversion. Background technique [0002] Due to its high strength, high modulus, excellent high temperature oxidation resistance, high temperature thermal shock resistance and high temperature creep resistance, SiBN(C) fibers require high strength, high modulus, high temperature resistance, and high temperature resistance in aviation and aerospace. It has important application prospects in the fields of oxidation, thermal shock resistance and creep resistance materials. [0003] At present, the preparation of SiBN(C) ceramic fibers can be divided into polymer route and monomer route from the perspective of precursor synthesis route. [0004] The polymer route refers to modifying Si-N bond-containing polymers such as polysilazane with boron-cont...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/515C04B35/622
Inventor 王军唐云李效东王浩王小宙李文华王义
Owner NAT UNIV OF DEFENSE TECH
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