Composite material and method for preparing the same

Patent metadata

Field	Value
Publication number	US-10364194-B2
Application number	US-201815985736-A
Country	US
Kind code	B2
Filing date	May 22, 2018
Priority date	May 22, 2017
Publication date	Jul 30, 2019
Grant date	Jul 30, 2019

Abstract

A method for preparing a ceramic-modified carbon-carbon composite material. The method includes preparing and thermally treating a carbon fiber preform, and depositing pyrolytic carbon on the carbon fiber preform in a chemical vapor infiltration furnace, to yield a porous carbon-carbon composite material; placing the carbon-carbon composite material deposited with the pyrolytic carbon on a zirconium-titanium powder mixture, and performing a reactive melt infiltration, to yield a carbon-carbon composite material modified by non-stoichiometric zirconium titanium carbide; and placing the carbon-carbon composite material modified by non-stoichiometric zirconium titanium carbide in a powder mixture including carbon, boron carbide, silicon carbide, silicon, and an infiltration enhancer, and performing an embedding method, to form a ceramic-modified carbon-carbon composite material.

First claim

What is claimed is:

1. A method, comprising:
1) preparing and thermally treating a carbon fiber preform, and depositing pyrolytic carbon on the carbon fiber preform in a chemical vapor infiltration furnace, to yield a porous carbon-carbon composite material;
2) placing the carbon-carbon composite material deposited with the pyrolytic carbon on a zirconium-titanium powder mixture, and performing a reactive melt infiltration, to yield a carbon-carbon composite material modified by non-stoichiometric zirconium titanium carbide; and
(3) placing the carbon-carbon composite material modified by non-stoichiometric zirconium titanium carbide in a powder mixture comprising carbon, boron carbide (B 4 C), silicon carbide (SiC), silicon, and an infiltration enhancer, and performing an embedding method, to form a ceramic-modified carbon-carbon composite material.

2. The method of claim 1 , wherein the prepared ceramic-modified carbon-carbon composite material comprises, in percentages by volume, 20-80% of a carbon matrix material, 15-78% of a Zr 0.8 Ti 0.2 C 0.74 B 0.26 ceramic material, and 2-5% of a silicon carbide ceramic material; and the carbon matrix material is the carbon-carbon composite material deposited with the pyrolytic carbon.

3. The method of claim 1 , wherein the carbon fiber preform has a density of 0.1-0.9 g·cm −3 , and comprises a needled felt or a three-dimensional braided body; in 1), the thermal treatment of the carbon fiber preform comprising placing the carbon fiber preform in a graphite furnace, and incubating at a temperature of between 2000 and 2300° C. for between 1 and 3 hrs.

4. The method of claim 1 , wherein in 1), depositing pyrolytic carbon on the carbon fiber preform in a chemical vapor infiltration furnace comprises charging nitrogen, hydrogen, and propylene or methane to the chemical vapor infiltration furnace, and controlling a furnace temperature of between 1000 and 1300° C., a furnace pressure of between 0.3 and 1.3 kPa and a reaction time of between 10 and 60 hrs; and the prepared porous carbon-carbon composite material has a porosity of between 20 and 40%.

5. The method of claim 1 , wherein the zirconium-titanium powder mixture is prepared by: sieving a zirconium power having a purity of ≥99.9% using a 325-mesh screen, sieving a titanium powder having a purity of ≥99.9% using a 325-mesh screen, mixing the zirconium power and the titanium powder in a molecular ratio of 0.8:0.2, ball milling the power mixture using a planetary ball mill, and drying a ball-milled mixed powder for 3-8 hrs under vacuum at 80-90° C.; a ball-milling speed is 200-300 rpm, a ball-milling time is 10-25 hrs, a ball-to-powder ratio is 4-10, and a ball-milling medium is alcohol.

6. The method of claim 1 , wherein in 2), the reactive melt infiltration is implemented as follows: weighing the zirconium-titanium powder mixture in an amount that is 3-5 times the weight of the porous carbon-carbon composite material, compacting the zirconium-titanium powder mixture in a graphite can, placing the porous carbon-carbon composite material on the zirconium-titanium powder mixture, and placing the graphite can in an infiltration furnace which is heated to a temperature of between 1900 and 2300° C. in a heating rate of 10-20° C./min for between 0.5 and 2 hours in the presence of argon.

7. The method of claim 1 , wherein in 3), the infiltration enhancer is alumina (Al 2 O 3 ), boron oxide (B 2 O 3 ), silica (SiO 2 ), or a mixture thereof; and the embedding method is implemented at a temperature of between 1600 and 1800° C. for between 0.5 and 2 hrs in the presence of argon.

8. The method of claim 1 , wherein the embedding method is implemented as follows:
a) weighing and mixing, on the basis of a total weight of a resulting mixture, 30%-70% by weight (wt. %) of silicon, 5-10 wt. % of alumina (Al 2 O 3 ), 10-20 wt. % of carbon, and 10-40 wt. % of silicon carbide (SiC), to yield a mixture; uniformly mixing the mixture with alcohol in a planetary ball mill, and drying, to yield a first powder mixture A;
b) weighing, on the basis of a total weight of a resulting mixture, 30-80 wt. % of boron carbide (B 4 C) and 20-70 wt. % of boron oxide (B 2 O 3 ), and uniformly mixing in a planetary ball mill, and drying, to yield a second powder mixture B;
c) weighing and mixing 20-50 wt. % of the first powder mixture A and 50-80 wt. % of the second powder mixture B, to yield a first power for modifying the carbon-carbon composite material modified by non-stoichiometric zirconium titanium carbide;
d) weighing and mixing 50-80 wt. % of the first powder mixture A and 20-50 wt. % of the second powder mixture B, to yield a second powder for modifying carbon-carbon composite material modified by non-stoichiometric zirconium titanium carbide;
e) weighing the first power and the second powder in a weight ratio of 0.2-1:1, a weight ratio of the carbon-carbon composite material modified by non-stoichiometric zirconium titanium carbide to a mixture of the first power and the second powder being 0.05-0.2:1; and
f) respectively embedding the first power and the second powder on the carbon-carbon composite material modified by non-stoichiometric zirconium titanium carbide at a temperature of between 1600 and 1800° C. for between 0.5 and 2 hrs in the presence of argon.

9. A material, comprising, in percentage amounts by volume: 20-80% of a carbon matrix material, 15-78% of a Zr 0.8 Ti 0.2 C 0.74 B 0.26 ceramic material, and 2-5% of a silicon carbide ceramic material.

Assignees

• Univ Central South

Inventors

• Zeng Yi
• Xiong Xiang
• Wang Dini
• Sun Wei
• Chen Zhaoke
• Wang Yalei

Classifications

• C04B2235/614

  Gas infiltration of green bodies or pre-forms · CPC title

• C04B41/87

  Ceramics · CPC title

• C04B41/4523

  applied from the molten state (vitreous materials C04B41/5022); Thermal spraying, e.g. plasma spraying · CPC title

• C04B35/83 Primary

  Carbon fibres in a carbon matrix · CPC title

• C04B2235/3821

  Boron carbides · CPC title