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Preparation method of carbon fiber-reinforced ultra high-temperature ceramic-base composite material capable of being repeatedly ablated for use

A technology of ultra-high temperature ceramics and composite materials, which is applied in the field of preparation of carbon fiber reinforced ultra-high temperature ceramic matrix composite materials, can solve the problems of difficult to withstand repeated ablation, lack of protective layer, and volatile loss of protective layer, etc. protective effect

Active Publication Date: 2014-06-18
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, under the action of high temperature and strong air flow, the ultra-high temperature ceramic matrix composite material SiO 2 The protective layer is extremely volatile and lost, and ZrO 2 , HfO 2 In the process of temperature changes, the oxidation products are accompanied by the transformation of the crystal form, and the volume changes to form a loose and porous structure. The lack of an effective protective layer on the surface of the material makes it difficult for the above-mentioned materials to withstand repeated ablation, which greatly reduces the reusability of the material.

Method used

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  • Preparation method of carbon fiber-reinforced ultra high-temperature ceramic-base composite material capable of being repeatedly ablated for use
  • Preparation method of carbon fiber-reinforced ultra high-temperature ceramic-base composite material capable of being repeatedly ablated for use

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Effect test

Embodiment 1

[0025] Preparation of composite material preform: CVI process is used to pyrolyze propylene at 960°C to deposit a pyrolytic carbon interface phase on the surface of carbon fibers, and MTS is loaded into a deposition furnace using hydrogen gas, and MTS is cracked at 1000°C under a pressure of 5KPa to deposit SiC For the matrix, a C / SiC composite material preform with an open porosity of 20vol% was cleaned by ultrasonic cleaning for at least 30 minutes, and dried in an oven at 80° C. to obtain a clean and dry preform.

[0026] Slurry preparation: Dissolve phenolic resin and hexamethylenetetramine in absolute ethanol, then add La(NO 3 ) 3 ·xH 2 O and ball milled for more than 24 hours to obtain the slurry; the ratio of phenolic resin and nitrate is 1:3, and the quality of hexamethylenetetramine is 0.1 times of the quality of the phenolic resin; the viscosity of the slurry is controlled by the content of absolute ethanol to be 50~ 100mPa·s.

[0027] Vacuum pressure impregnation...

Embodiment 2

[0031] Preparation of composite material preform: CVI process is used to pyrolyze propylene at 960°C to deposit a pyrolytic carbon interface phase on the surface of carbon fibers, and MTS is loaded into a deposition furnace using hydrogen gas, and MTS is cracked at 1000°C under a pressure of 5KPa to deposit SiC The matrix, the obtained C / SiC composite preform with an open porosity of 20vol%, was cleaned by ultrasonic waves for at least 30 minutes, and dried in an oven at 80°C to obtain a clean and dry preform.

[0032] Slurry preparation: La 2 o 3 The powder was added to 0.5% cellulose sodium CMC aqueous solution and ball milled for more than 24 hours, La 2 o 3 Mass fraction is 30%, obtains slurry a; Phenolic resin, hexamethylenetetramine are dissolved in dehydrated alcohol, obtain slurry b, hexamethylenetetramine quality is 0.1 times of phenolic resin quality, pass through The content of water ethanol controls the viscosity of the slurry to be 50-100 mPa·s.

[0033] Vacuu...

Embodiment 3

[0037] Preparation of composite material prefabricated body: In the carbon fiber prefabricated body, the phenolic resin slurry is pressure-impregnated, the vacuum degree is -0.08MPa, the pressure is 0.8MPa, and the resin is cracked at 900°C after curing at 150°C to obtain an open porosity of 30vol%. The C / C composite material preform was cleaned by ultrasonic waves for at least 30 minutes, and dried in an oven at 80° C. to obtain a clean and dry preform.

[0038] Slurry preparation: dissolve furan resin and hexamethylenetetramine in absolute ethanol, then add Y(NO 3 ) 3 ·xH 2 O and ball milled for more than 24 hours to obtain the slurry; the ratio of furan resin and nitrate is 1:4, and the quality of hexamethylenetetramine is 0.1 times of the quality of furan resin; the viscosity of the slurry is controlled by the content of absolute ethanol to be 50~ 100mPa·s.

[0039] Vacuum pressure impregnation: Put the C / C preform and the slurry into the vacuum tank at the same time, b...

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Abstract

The invention relates to a preparation method of a carbon fiber-reinforced ultra high-temperature ceramic-base composite material capable of being repeatedly ablated for use. Vacuum pressure is adopted to soak and combine reaction melt, the reaction melt is permeated in the conventional carbon fiber-reinforced ultra high-temperature ceramic-base composite material, and rear-earth metal elements such as La, Y, Yb, Sc, and the like are added to achieve effects of reducing volatilization of SiO2 at a high temperature, stabilizing a ZrO2 / HfO2 crystal form and generating rare-earth zirconate or rear-earth hafnate. After ablation, glass-state SiO2 is formed on the material surface and filled between ZrO2 and HfO2; and a compaction layer of the rare-earth zirconate / the rear-earth hafnate is mixed to protect the material very well, so that repeatable ablation of the ultra high-temperature ceramic-base composite material is possible.

Description

technical field [0001] The invention relates to a method for preparing a carbon fiber reinforced ultra-high temperature ceramic matrix composite material that can be repeatedly ablated. Rare earth metal compounds such as La, Y, Yb, Sc, etc. are introduced into the carbon fiber reinforced ultra high temperature ceramic matrix composite material in situ, and a An ultra-high temperature ceramic matrix composite with repeatable ablation properties. Background technique [0002] Continuous fiber toughened silicon carbide ceramic matrix composite (C / SiC) is an ideal high-temperature structural material, which has a series of advantages such as high temperature resistance, low density, high strength, and thermal shock resistance, and has broad application prospects in the aerospace field , but when the temperature exceeds 1700°C, C / SiC actively oxidizes and loses the SiO on the surface 2 The protective layer, anti-ablation and anti-oxidation properties drop sharply leading to comp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/80C04B35/565C04B35/56C04B35/622
Inventor 王一光刘俊朋罗磊段刘阳张立同成来飞
Owner NORTHWESTERN POLYTECHNICAL UNIV
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