Method for preparing nitride ceramic fibre

A technology for nitride ceramics and fibers, which is applied in the field of high-temperature thermal cracking and transformation to prepare multi-component nitride ceramic fibers, can solve the problems of unfavorable popularization and application, high cost, complicated process, etc., and achieves low cost, reliable source and high synthesis yield. Effect

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

[0006] The above-mentioned preparation method is complicated in process and relatively high in cost, which is unfavorable for popularization and application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: SiAlNC fiber preparation example ①

[0029] (1) Dichloromethylsilane and aluminum trichloride are dissolved in xylene, meanwhile, vacuumize repeatedly in the three-necked flask reactor of 250ml with stirring, dripping, distillation device, fill dry nitrogen at least three times, (2) Take 0.15mol of dichloromethylsilane and 0.15mol of aluminum trichloride into a three-necked flask protected by dry nitrogen, and then inject 0.9mol of hexamethyldisilazane into a constant pressure In the funnel, add hexamethyldisilazane dropwise to the mixed solution of dichloromethylsilane and aluminum trichloride, and stir while adding; Raise the temperature of the reactor to 280°C at a rate of / min, and keep it warm at this temperature for 10 hours; (4) Lower the temperature of the reactor to 150°C, distill under reduced pressure for 0.5 hours, and cool naturally to room temperature to obtain solid polyaluminum silicon Azane precursor 12.2g; (5) Place the precursor obtaine...

Embodiment 2

[0030] Embodiment 2: SiAlNC fiber preparation example ②

[0031] (1) Dissolve aluminum trichloride in toluene, at the same time, repeatedly vacuumize and fill dry nitrogen at least three times in a 250ml three-necked flask reactor with stirring, dropping, and distillation devices to get rid of air and moisture therein (2) Take 0.15mol of aluminum trichloride and add it to a three-necked flask protected by dry nitrogen, then take 0.6mol of hexamethyldisilazane and add it to a constant pressure funnel, then add hexamethyldisilazane dropwise Add it into the aluminum chloride solution in the way of adding, and stir while adding it dropwise; (3) after the dropwise addition is completed, the reactor is heated to 300°C at a rate of 0.5°C / min, and is kept at 290°C for 8 hours; (4) ) The temperature of the reactor was lowered to 105° C., and the vacuum distillation was performed for 0.5 hour to obtain 19.2 g of polyaluminosilazane precursor. (5) Place the polyaluminosilazane precursor...

Embodiment 3

[0032] Embodiment 3: SiBAlNC fiber preparation example ①

[0033] (1) boron trichloride, aluminum trichloride are dissolved in normal hexane, meanwhile, repeatedly vacuumize in the there-necked flask reactor of 250ml with stirring, dropwise, distillation unit, fill dry nitrogen at least three times, with Exclude the air and moisture therein; (2) Take 0.15mol of boron trichloride and 0.3mol of aluminum trichloride successively into a three-necked flask protected by dry nitrogen, then take 0.6mol of heptamethyldisilazane and add to constant pressure In the funnel, heptamethyldisilazane was added dropwise to the mixed solution of the first two monomers, and stirred while adding; (3) after the dropwise addition was completed, the The reactor was heated up to 320°C, and kept at this temperature for 12 hours; (4) the temperature of the reactor was lowered to 165°C, and after vacuum distillation for 0.5 hours, it was naturally cooled to room temperature to obtain the solid polysilabo...

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Abstract

The present invention provides a preparation method of nitrogen ceramic fiber. In the preparation method, the halides of the target element and small molecules disilazane are used as starting materials and are mixed according to a certain ratio; the temperature is raised to be between 125 and 500 DEG C and is maintained for 2 to 30 hours; after the temperature is lowered, the mixture is processed through vacuum distillation and is cooled to be at the room temperature; thus the nitrogen ceramics precursor of the target element can be prepared; the nitrogen ceramics precursor is fused for spinning to prepare the precursor fiber of nitride that is not treated through fusing; the non-molten fiber is dispersed at high temperature; after the fiber is cooled, the product of nitride ceramic fiber can be prepared. The preparation method has the advantages of low costs of raw materials, reliable source, higher synthetic yield, simple process and one-step preparation of the precursor. The efficiency is high and the preparation method is conducive to the integrative operation of spinning, non-melting treatment and sintering of the precursor.

Description

technical field [0001] The invention relates to a method for preparing nitride ceramic fibers, in particular to a method for preparing multi-element nitride ceramic fibers from organic nitride polymers through high-temperature pyrolysis conversion. Background technique [0002] Nitride ceramic fiber has the characteristics of high thermal conductivity, low expansion coefficient and high temperature resistance. It is a kind of ceramic fiber with excellent comprehensive performance. It has important application prospects in the fields of high temperature resistance, oxidation resistance, thermal shock resistance, and high temperature creep resistance materials. [0003] At present, the preparation of multi-component nitride ceramic fibers mainly focuses on silicon-based nitride ceramic fibers such as SiCN and SiBNC. For the preparation of these ceramic fibers, the precursor conversion method is mainly used. From the perspective of the synthesis route of the precursor, the pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C04B35/622
Inventor 王军唐云李效东王浩王小宙
Owner NAT UNIV OF DEFENSE TECH
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