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Preparation method of Cf/SiC-ZrC-ZrB2 ultrahigh-temperature ceramic-based composite material

A technology of ultra-high temperature ceramics and composite materials, which is applied in the field of improving material ablation resistance, oxidation resistance and mechanical properties. It can solve problems such as uneven distribution and low phase content of ultra-high temperature ceramics, achieve uniform distribution, improve The effect of phase content and high content

Active Publication Date: 2017-05-31
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention is aimed at C f / SiC-ZrC and C f / SiC-ZrC-ZrB 2 Due to the insufficient preparation methods of materials such as ultra-high temperature ceramics, the phase content is low and the distribution is uneven, and an improved C f / SiC-ZrC-ZrB 2 Preparation method of ultra-high temperature ceramic matrix composite material

Method used

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  • Preparation method of Cf/SiC-ZrC-ZrB2 ultrahigh-temperature ceramic-based composite material
  • Preparation method of Cf/SiC-ZrC-ZrB2 ultrahigh-temperature ceramic-based composite material
  • Preparation method of Cf/SiC-ZrC-ZrB2 ultrahigh-temperature ceramic-based composite material

Examples

Experimental program
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Effect test

Embodiment 1

[0054] (1) Prefabricated body treatment: carry out alcohol ultrasonic cleaning on the carbon fiber prefabricated body with an open porosity of 30vol% (the interface is a PyC / SiC composite multilayer interface with a thickness of 500nm), and the cleaning time is 2 hours;

[0055] (2) Preparation of sol solution: H 3 BO 3 , PVA were dissolved in glycerin and deionized water respectively, and 8.0mol / L H 3 BO 3 solution and 2.0mol / L PVA solution, with NH 3 ·H 2 O solution to H 3 BO 3 The pH of the solution was adjusted to 4, and the two solutions were mixed in a molar ratio of H 3 BO 3 / PVA=4 / 10 ratio mixing, reacting at 80°C oil bath temperature for 4-8 hours to obtain a sol solution;

[0056] (3) Vacuum impregnation sol: Under the vacuum condition of -0.08MPa~-0.10MPa, introduce the sol solution in (2) into the C in (1) fIn the preform, heat it at 100°C for 24 hours to obtain C f / polyethyl borate, take it out and put it in an oven to dry at 60°C for 48 hours;

[0057...

Embodiment 2

[0063] Similar to the steps in Example 1, the difference is that the open porosity of the fiber preform is 40% (the interface is a PyC / SiC composite multilayer interface with a thickness of 1000nm), H 3 BO 3 The pH of the solution was adjusted to 5, the molar ratio H 3 BO 3 / PVA=5 / 10, the temperature of the sol-oil bath is 100°C, the gel condition is 110°C for 20 hours, and the gel is dried at 70°C for 36 hours.

Embodiment 3

[0065] Similar to the steps in Example 1, the difference is that the open porosity of the fiber preform is 50% (the interface is a PyC / SiC composite multilayer interface with a thickness of 1500nm), H 3 BO 3 The pH of the solution was adjusted to 6, the molar ratio H 3 BO 3 / PVA=6 / 10, the temperature of the sol-oil bath is 120°C, the gel condition is 120°C for 18 hours, and the gel is dried at 80°C for 24 hours.

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Abstract

The invention relates to a preparation method of a Cf / SiC-ZrC-ZrB2 ultrahigh-temperature ceramic-based composite material. The preparation method comprises the following steps: (1) preparing a sol solution containing H3BO3 and polyvinyl alcohol; (2) introducing the sol solution into a carbon fiber preform by utilizing vacuum impregnation, and performing gelatinization to obtain Cf / polyethyl borate; (3) cracking the Cf / polyethyl borate in the presence of an inert gas to obtain Cf / B2O3-C; (4) performing a carbothermal reduction reaction on the obtained Cf / B2O3-C in the presence of the inert gas to obtain Cf / B4C-C; and (5) infiltrating fused ZrSi2 into the Cf / B4C-C to perform an infiltration reaction to generate SiC, ZrC, ZrB2 in situ, thereby obtaining the Cf / SiC-ZrC-ZrB2 ultrahigh-temperature ceramic-based composite material. The method provided by the invention is simple and feasible, the prepared Cf / SiC-ZrC-ZrB2 has high contents of ultrahigh-temperature phases (ZrC and ZrB2) and is uniformly distributed, and the method significantly improves ablation resistance, oxidation resistance and mechanical properties of the material.

Description

technical field [0001] The present invention relates to a C f / SiC-ZrC-ZrB 2 A method for preparing ultra-high temperature ceramic matrix composites, especially a B 4 C-C Porous Structure Combined with Reactive Infiltration ZrSi 2 A method for in-situ generation of ultra-high temperature phases to improve material ablation resistance, oxidation resistance and mechanical properties. Background technique [0002] Known as the "next-generation flight technology", the hypersonic (speed up to 5-20 times the speed of sound) flight technology has attracted great attention from the world's major military powers. When the hypersonic vehicle re-enters the atmosphere, it rubs against the air violently, causing some tip parts to withstand the severe erosion of high temperature and high-pressure airflow of ≥2000°C. Such a harsh service environment can easily lead to catastrophic accidents such as deformation or even fracture of components. Therefore, one of the keys to ensure the saf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/624C04B35/565C04B35/58C04B35/56C04B35/622
Inventor 董绍明陈小武阚艳梅胡建宝周海军
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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