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A hafnium-tantalum-silicon ternary composite ceramic precursor, carbon/hafnium-tantalum-carbon solid solution-silicon carbide ceramic matrix composite material and preparation method thereof

A technology of composite ceramics and precursors, applied in the field of composite materials, can solve the problems of difficult hafnium-tantalum-carbon solid solution dispersion of silicon carbide, unsolved hafnium-tantalum-carbon solid solution dispersion, impregnated fiber prefabrication, etc., to achieve easy industrial implementation , Excellent oxidation resistance, excellent ablation resistance

Active Publication Date: 2021-10-08
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there have been no reports on composite materials such as carbon / silicon carbide modified by hafnium-tantalum-carbon solid solution. The reason is that based on the high melting point and good stability of hafnium-tantalum-carbon solid solution, it is difficult to uniformly dispersed in SiC
Although patents CN201611051813.9 and CN201611053755.3 prepared Hf x Ta 1-x C alloy, but the method is to use hafnium and tantalum alkoxide to make the alloy precursor and directly sinter the preparation, which does not involve the dispersion of hafnium-tantalum-carbon solid solution in the silicon carbide matrix, that is, it does not solve the problem of hafnium-tantalum-carbon solid solution in the silicon carbide matrix. Dispersion problem; in addition, the viscosity of the hafnium-tantalum alloy precursors prepared in these two patent applications is as high as 20,000-30,000mPa·s, which cannot be used to impregnate fiber preforms, so it is not suitable for composite materials such as modified carbon / silicon carbide

Method used

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  • A hafnium-tantalum-silicon ternary composite ceramic precursor, carbon/hafnium-tantalum-carbon solid solution-silicon carbide ceramic matrix composite material and preparation method thereof

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preparation example Construction

[0031] In a second aspect, the present invention provides a method for preparing the hafnium-tantalum-silicon ternary composite ceramic precursor described in the first aspect of the present invention, the method comprising the following steps:

[0032] (1) Mix pentavalent tantalum salt, tetravalent hafnium salt and small molecule alcohol evenly to obtain a mixture, then place the mixture in an ice bath at 0°C and add a catalyst for co-hydrolysis reaction to obtain hafnium tantalum alkoxide Solution; in the present invention, the addition of the catalyst can accelerate the reaction speed of the pentavalent tantalum salt, tetravalent hafnium salt and small molecule alcohol;

[0033] (2) adding the ligand to the hafnium-tantalum alkoxide solution obtained in step (1) to carry out a polymerization reaction to obtain a hafnium-tantalum coordination copolymer resin; and

[0034] (3) Mix the hafnium-tantalum coordination copolymer resin, the polycarbosilane, and the carbon source pr...

Embodiment 1

[0055] A method for preparing a hafnium-tantalum-silicon ternary composite ceramic precursor, the specific steps of which are:

[0056] ① In molar parts, mix 1 part of hafnium tetrachloride, 4 parts of tantalum pentachloride and 5 parts of n-propanol, place in an ice-water bath at 0°C, and drop an appropriate amount of diethylamine (the dosage of diethylamine is 0.3% of the mass sum of the pentavalent tantalum salt and the tetravalent hafnium salt), reacted for 3 hours, then added 5 parts of acetylacetone, polymerized at 80°C for 4 hours, and distilled at atmospheric pressure for 5 hours to remove excess n-propanol to obtain hafnium-tantalum coordination copolymer resin.

[0057] ② In terms of molar parts, mix 1 part of the hafnium-tantalum coordination copolymer resin obtained in step ①, 1 part of polycarbosilane, 2 parts of allyl phenolic resin and 4 parts of xylene, stir mechanically for 6 hours, and let stand for 8 hours. hours, and filtered to obtain a uniform hafnium-ta...

Embodiment 2

[0061] A method for preparing a hafnium-tantalum-silicon ternary composite ceramic precursor, the specific steps of which are:

[0062] ① In molar parts, mix 1 part of hafnium tetrachloride, 4 parts of tantalum pentachloride and 5 parts of n-propanol, place in an ice-water bath at 0°C, and drop an appropriate amount of diethylamine (the dosage of diethylamine is 0.3% of the mass sum of the pentavalent tantalum salt and the tetravalent hafnium salt), reacted for 3 hours, then added 5 parts of acetylacetone, polymerized at 80°C for 4 hours, and distilled at atmospheric pressure for 5 hours to remove excess n-propanol to obtain hafnium-tantalum coordination copolymer resin.

[0063] ② In terms of molar parts, mix 4 parts of the hafnium-tantalum coordination copolymer resin obtained in step ①, 1 part of polycarbosilane, 5 parts of allyl phenolic resin and 7 parts of xylene, stir mechanically for 6 hours, and let stand for 8 hours. hours, and filtered to obtain a uniform hafnium-t...

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Abstract

The invention relates to a hafnium-tantalum-silicon ternary composite ceramic precursor, a carbon / hafnium-tantalum-carbon solid solution-silicon carbide ceramic matrix composite material and a preparation method thereof. The hafnium-tantalum-silicon ternary composite ceramic precursor comprises a hafnium-tantalum coordination copolymer resin, polycarbosilane and a carbon source precursor in a molar ratio of 1:(0.25-4):(1.1-5). The preparation method of the ceramic precursor is as follows: mixing pentavalent tantalum salt, tetravalent hafnium salt and small molecular alcohol uniformly, then placing in ice bath condition and adding catalyst to carry out co-hydrolysis reaction, and then adding ligand to carry out polymerization reaction, The hafnium-tantalum coordination copolymer resin is obtained; the hafnium-tantalum coordination copolymer resin, polycarbosilane and carbon source precursor are mixed with an organic solvent, then stirred, left standing and filtered to prepare the ceramic precursor. The invention solves the problem of uniform dispersion of hafnium, tantalum and silicon, and the ceramic matrix composite material with good toughness, ultra-high temperature resistance, excellent oxidation resistance and excellent ablation resistance can be prepared by using the ceramic precursor.

Description

technical field [0001] The invention belongs to the technical field of composite materials, and in particular relates to a hafnium-tantalum-silicon ternary composite ceramic precursor, a carbon / hafnium-tantalum-carbon solid solution-silicon carbide ceramic matrix composite material and a preparation method thereof. Background technique [0002] Carbon fiber toughened silicon carbide ceramic matrix composites (C f / SiC composite material) is a high-performance thermal structural material. It overcomes the Achilles heel of brittleness of single-phase ceramic materials, and has excellent characteristics such as low density, high temperature resistance, high strength, oxidation resistance and ablation resistance. The rudder has been applied. However, long-term research has shown that traditional C f The long-term anti-oxidation service temperature of SiC composite materials does not exceed 1650 °C. When the Mach number of a hypersonic vehicle exceeds 6, its high-temperature ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/80C04B35/56C04B35/622
CPCC04B35/5607C04B35/622C04B2235/3839C04B2235/3826C04B2235/96C04B2235/9607C04B35/6325
Inventor 裴雨辰赵彤刘伟浑丙利刘俊鹏于艺宋环君金鑫孙同臣
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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