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Si-B-C gradient anti-oxidation coating of carbon/carbon composite material and preparation method of Si-B-C gradient anti-oxidation coating

A carbon composite material and anti-oxidation coating technology, applied in the field of Si-B-C gradient anti-oxidation coating and preparation, can solve the problems of limited service life of the coating system, unsatisfactory oxidation protection effect, high volatility of boric acid glass, etc. , to achieve the effect of improving antioxidant performance, short experimental period and small fiber damage

Active Publication Date: 2022-01-18
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007]However, boric acid glass produced after boron oxidation becomes more volatile and less viscous at temperatures above 1000°C, resulting in a larger oxygen diffusion coefficient, which makes the coating system more than 1000 The service life is limited at high temperature of ℃, and the oxidation protection effect is not ideal

Method used

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  • Si-B-C gradient anti-oxidation coating of carbon/carbon composite material and preparation method of Si-B-C gradient anti-oxidation coating
  • Si-B-C gradient anti-oxidation coating of carbon/carbon composite material and preparation method of Si-B-C gradient anti-oxidation coating
  • Si-B-C gradient anti-oxidation coating of carbon/carbon composite material and preparation method of Si-B-C gradient anti-oxidation coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1): Using a two-dimensional C / C composite material with a density of 1.7g / cm3 as the matrix, cut samples with a size of 10mm×10mm×10mm from the C / C composite material, and use 400 mesh SiC sandpaper for all samples Polish, then ultrasonically clean with ethanol, and dry in an oven at a temperature of 60-100°C for 2-4 hours.

[0038] 2): Suspend the C / C substrate in the deposition area of ​​the vertical resistance furnace, evacuate to below -0.09Mpa, pass Ar as the protective gas, and raise the furnace temperature to 950°C at a heating rate of 3-10°C / min , when the temperature in the furnace reaches the deposition temperature, the diluted Ar, the reaction H2 and the boron source BCl3 are first introduced, and then the bubbling method is used to bring methyltrichlorosilane (MTS) into the reaction zone for deposition. During this process, the gas flow rate The control range is: dilute Ar: 500-600ml / min, react H 2 : 900-1000ml / min, boron source BCl 3 : 500ml / min, MTS: 0.1...

Embodiment 2

[0042] 1): Using a two-dimensional C / C composite material with a density of 1.7g / cm3 as the matrix, cut samples with a size of 10mm×10mm×10mm from the C / C composite material, and use 400 mesh SiC sandpaper for all samples Polish, then ultrasonically clean with ethanol, and dry in an oven at a temperature of 60-100°C for 2-4 hours.

[0043] 2): Suspend the C / C substrate in the deposition area of ​​the vertical resistance furnace, evacuate to below -0.09Mpa, pass Ar as the protective gas, and raise the furnace temperature to 1050°C at a heating rate of 3-10°C / min , when the temperature in the furnace reaches the deposition temperature, the diluted Ar is first introduced, and the reaction H 2 and boron source BCl 3 , and then use the bubbling method to bring methyltrichlorosilane (MTS) into the reaction zone for deposition. The gas flow control range during this process is: dilute Ar: 500-600ml / min, react H 2 : 900-1000ml / min, boron source BCl 3 : 500ml / min, MTS: 0.1-0.2g / min;...

Embodiment 3

[0047] 1): Using a two-dimensional C / C composite material with a density of 1.7g / cm3 as the matrix, cut samples with a size of 10mm×10mm×10mm from the C / C composite material, and use 400 mesh SiC sandpaper for all samples Polish, then ultrasonically clean with ethanol, and dry in an oven at a temperature of 60-100°C for 2-4 hours.

[0048] 2): Suspend the C / C substrate in the deposition area of ​​the vertical resistance furnace, evacuate to below -0.09Mpa, pass Ar as the protective gas, and raise the furnace temperature to 1150°C at a heating rate of 3-10°C / min , when the temperature in the furnace reaches the deposition temperature, the diluted Ar is first introduced, and the reaction H 2 and boron source BCl 3 , and then use the bubbling method to bring methyltrichlorosilane (MTS) into the reaction zone for deposition. The gas flow control range during this process is: dilute Ar: 500-600ml / min, react H 2 : 900-1000ml / min, boron source BCl 3 : 500ml / min, MTS: 0.1-0.2g / min;...

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Abstract

The invention relates to a Si-B-C gradient anti-oxidation coating of a carbon / carbon composite material and a preparation method. A self-healing coating is composed of SiC and B4C phases, has a gradient structure, and comprises a boron-rich layer, a transition layer and a silicon-rich layer from inside to outside; a Si-B-C coating with different B contents is deposited by adopting a chemical vapor deposition method, so that the gradient coating is successfully prepared on the surface of the C / C composite material. The invention aims to improve the oxidation resistance of the coating in a wide temperature range. The coating has the advantages of low reaction temperature and small damage to fibers; the bonding capacity of the coating and a matrix is good; in a low-temperature area of 700-1000 DEG C, boron oxide glass is generated on the inner boron-rich layer, and oxygen is prevented from entering the coating; in a high-temperature region of 1000-1300 DEG C, the outer silicon-rich layer generates a borosilicate glass phase, volatilization of boron oxide on the inner layer is prevented, the C / C composite material is protected at the same time; and thus, oxidation protection of the C / C composite material in a wide temperature range is achieved. The preparation method has the advantages of simple technological process, short experimental period and high experimental efficiency; and the coating has good oxidation resistance in a wide temperature range and the like.

Description

technical field [0001] The invention belongs to a Si-B-C gradient anti-oxidation coating and a preparation method thereof, and relates to a Si-B-C gradient anti-oxidation coating of a carbon / carbon composite material and a preparation method thereof. Background technique [0002] C / C composite material is a carbon-based composite material with carbon fiber as the reinforcing phase, and its composition is all carbon elements. It is a high-performance composite material with both structural and functional properties. The material has a series of unique physical and chemical properties: low density, high specific strength and specific modulus, good fracture toughness, small thermal expansion coefficient, high temperature resistance, ablation resistance, thermal shock resistance and stable chemical properties. These advantages make it unique in the application of aviation, aerospace and military high-tech fields. However, in an oxidizing atmosphere, the C / C composite material w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B41/89
CPCC04B41/89C04B41/52C04B41/009C04B35/83C04B41/5062C04B41/4531
Inventor 张雨雷盖文涵张鹏飞陈国辉孔竟安
Owner NORTHWESTERN POLYTECHNICAL UNIV
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