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Method for synthesizing tantalum-containing SiC ceramic precursor

A technology of ceramic precursor and synthesis method, which is applied in the field of preparation of SiC ceramic precursor, can solve the problems of poor oxidation resistance, poor ultra-high temperature resistance, and single function of fibers, and achieves easy control of the reaction process and re-formability. Good, wide-ranging effects

Inactive Publication Date: 2008-05-28
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to overcome the shortcomings of poor oxidation resistance, poor ultra-high temperature resistance and single function of SiC ceramics and fibers prepared by the existing precursor conversion method, and provide a kind of good oxidation resistance and better ultra-high temperature resistance. Preparation process of SiC ceramic precursor containing heterogeneous element tantalum to diversify the functions of SiC ceramics

Method used

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  • Method for synthesizing tantalum-containing SiC ceramic precursor
  • Method for synthesizing tantalum-containing SiC ceramic precursor
  • Method for synthesizing tantalum-containing SiC ceramic precursor

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Using PSCS and tantalum tetraethoxy acetylacetonate as raw materials, the mass ratio of the two (the proportions described below are all mass ratios) is: tantalum tetraethoxy acetylacetonate: PSCS = 8: 100, and the reaction temperature is 450°C , pyrolysis temperature 500°C, heat preservation reaction for 6 hours, dissolved in xylene, filtered, and the filtrate was distilled under reduced pressure at 390°C to obtain PTCS with a softening point of 215°C and tantalum content of 4.11wt%, with a precursor yield of 70.9%. N 2 Heat preservation at 1200°C for 1 hour under the atmosphere, and the ceramic yield is 75.3%.

[0031] The tantalum-containing SiC ceramic fiber is prepared by using the PTCS precursor through melt spinning, non-melting in air and firing at high temperature. The fiber diameter is 20μm, and the tensile strength is 1.9GPa. The fiber has good ultra-high temperature resistance. After treatment at 1450°C and 1600°C, the fiber strength retention rate is 47% ...

Embodiment 2

[0034] Using PCS and tetraethoxy tantalum as raw materials, tetraethoxy tantalum: PCS = 1: 100, the reaction temperature is 400 ° C, the cracking temperature is 450 ° C, and after the reaction time of 2 hours, it is dissolved in xylene and filtered, and the filtrate is at 350 °C for vacuum distillation to obtain PTCS with a softening point of 210 °C and a tantalum content of 0.72 wt%, with a precursor yield of 78.2%. N 2 The temperature was kept at 1200° C. for 1 hour under the atmosphere, and the ceramic yield was 76.5%.

[0035] The tantalum-containing SiC ceramic fiber is prepared by using the PTCS precursor through melt spinning, non-melting in air and firing at high temperature. The fiber diameter is 18μm, and the tensile strength is 2.1GPa. The fiber has good ultra-high temperature resistance. After treatment at 1450°C and 1600°C, the fiber strength retention rate is 51% and 36% respectively; the fiber has good oxidation resistance. After heat treatment at 1000°C in ai...

Embodiment 3

[0037] Using PSCS and tantalum pentachloride as raw materials, the mass ratio of the two is: tantalum pentachloride:PSCS=20:100, the reaction temperature is 420°C, the cracking temperature is 500°C, and after 4 hours of heat preservation reaction, it is dissolved in xylene and filtered. The filtrate was distilled under reduced pressure at 350° C. to obtain PTCS with a softening point of 179° C. and a tantalum content of 9.26 wt%, with a precursor yield of 52.9%. N 2 The temperature was kept at 1200° C. for 1 hour under the atmosphere, and the ceramic yield was 72.2%.

[0038] The tantalum-containing SiC ceramic fiber is prepared by using the PTCS precursor through melt spinning, non-melting in air and firing at high temperature. The fiber diameter is 21μm, and the tensile strength is 1.8GPa. The fiber has good ultra-high temperature resistance. After treatment at 1450°C and 1600°C, the fiber strength retention rate is 45% and 35% respectively; the fiber has good oxidation re...

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Abstract

The invention discloses a synthesis method of an SiC-containing ceramics precursor, which comprises the steps that: 1. low molecular weight polymer with main chain containing silicon is sent into a three-mouth flask, and is added with 0.5wt% - 20wt% of tantalum organic compounds or chloride; 2. under the protection of Ar or N2 or compound of the Ar or N2, the temperature of the three-mouth flask is raised to 350 to 500 DEG C, and the temperature of a cracking column is controlled within 450 DEG C to 550 DEG C; then thermal decomposition rearrangement reaction is carried out for 0.5 to 25 hours, and then cooling is done; 3. the obtained rough product is dissolved by xylene and filtered; the filtrate solution is distilled by reducing temperature to between 250 to 390 DEG C, then the obtained material is cooled. The invention has the advantages of wide raw material source, reaction process being easy to be controlled, simple equipment, high purity of product, good formability, and good performance of super-high temperature and absorbing property; in addition, the ceramics fiber produced in the method has good oxidation resistance performance and is easy to realize large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of a SiC ceramic precursor containing a heterogeneous element tantalum, in particular to a SiC ceramic precursor containing a heterogeneous element tantalum with a main chain silicon-containing polymer and an organometallic compound containing tantalum as main raw materials body preparation method. Background technique [0002] With the development of science and technology, national defense, aerospace, energy and other fields have put forward higher and higher requirements for materials such as light weight, high strength, high modulus, high temperature resistance, corrosion resistance, oxidation resistance, and wear resistance. The development of high-performance ceramics and their composite materials to replace traditional high-temperature alloys and refractory metal materials has become the main research direction in the future. High-performance ceramics are also used in the fields of advanced aerospac...

Claims

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Application Information

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IPC IPC(8): C04B35/571
Inventor 谢征芳曹淑伟王军王浩薛金根牛加新
Owner NAT UNIV OF DEFENSE TECH
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