Method for preparing SiO2-SiC mosaic structure microporous antioxidant coating on surface of carbon/carbon composite material

A carbon composite material and anti-oxidation coating technology, which is applied in the field of carbon/carbon composite material anti-oxidation coating, can solve the problems of SiC coating failure, poor anti-oxidation performance, and no mitigation of oxide film cracking, etc., so as to inhibit cracking. , the effect of hindering the diffusion of oxygen

Active Publication Date: 2020-12-29
NORTHWESTERN POLYTECHNICAL UNIV
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Problems solved by technology

[0003] Document 1 "Xin Yang, Qi-zhong Huang, Zhe-an Su, Li-yuan Chai, Xiu-fei Wang, Le-ping Zhou. A double layer nanostructure SiC coating for anti-oxidation protection of carbon / carbon composites prepared by chemical vapor reaction and chemical vapor deposition[J].Ceramics International,39(2013):5053-5062."A double-layer silicon carbide coating prepared by liquid phase infiltration and vapor deposition, during the anti-oxidation process, the coating surface The crystallization of the amorphous silicon dioxide film produces cristobalite. The CTE of this crystal phase is larger than that of amorphous silicon dioxide, and a crack with a width of 16.08um is generated on the silicon dioxide film, which leads to the failure of the SiC coating.
Literature 2 "Yan-hui Chu, He-junLi, Qiang-ang Fu, Le-hua Qi, Xu Zou. Toughening by SiC Nanowires in a Dense SiC-Si Ceramic Coating for Oxidation Protection of C / C Composites[J].Journal ofthe American Ceramic Society, 95(2012) 3691-3697." announced a method for preparing a SiC nanowire toughened SiC ceramic coating on the surface of a carbon / carbon composite material. The method introduces SiC nanowires in the SiC coating To a certain extent, the cracking of SiC coating was inhibited, but the cracking of SiC and surface SiO was not alleviated. 2 The problem of cracking of the oxide film caused by crystallization and thermal mismatch of the glass, and the final oxidation resistance is not good

Method used

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  • Method for preparing SiO2-SiC mosaic structure microporous antioxidant coating on surface of carbon/carbon composite material
  • Method for preparing SiO2-SiC mosaic structure microporous antioxidant coating on surface of carbon/carbon composite material
  • Method for preparing SiO2-SiC mosaic structure microporous antioxidant coating on surface of carbon/carbon composite material

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Experimental program
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Embodiment 1

[0041] Grind the carbon / carbon composite material with No. 400 and No. 800 sandpaper, wash it with absolute ethanol, and dry it in an oven at 70°C for 12 hours for later use; weigh 80g of silicon powder and 10g of graphite powder and place them in a turpentine ball mill jar for ball milling Mixing treatment for 5 hours, put the powder mixed by the ball mill into the graphite crucible, embed the dried carbon / carbon composite material into the mixed powder, so that the mixed powder completely covers the C / C composite material; put the graphite crucible into In the vacuum reaction furnace, after the vacuum treatment of the vacuum furnace, the argon gas is passed to normal pressure, and the furnace temperature is raised from room temperature to 2000 °C at a temperature increase rate of 5 °C / min, and the temperature is kept for 3 hours, and then the power is turned off and naturally cooled to room temperature. Argon protection was used throughout the process. Weigh 7g of silicon ca...

Embodiment 2

[0043] Grind the carbon / carbon composite material with No. 400 and No. 800 sandpaper, wash it with absolute ethanol, and dry it in an oven at 70°C for 12 hours for later use; weigh 77g of silicon powder and 15g of graphite powder and place them in a turpentine ball mill jar for ball milling Mixing treatment for 8 hours, put the powder mixed by the ball mill into the graphite crucible, embed the dried carbon / carbon composite material into the mixed powder, so that the mixed powder completely covers the C / C composite material; put the graphite crucible into In the vacuum reaction furnace, after the vacuum treatment of the vacuum furnace, the argon gas is passed to the normal pressure, and the furnace temperature is raised from room temperature to 2050 °C at a heating rate of 7 °C / min, and the temperature is kept for 2 hours, and then the power is turned off and naturally cooled to room temperature. Argon protection was used throughout the process. Weigh 8g of silicon carbide pow...

Embodiment 3

[0045] Grind the carbon / carbon composite material with No. 400 and No. 800 sandpaper, wash it with absolute ethanol, and dry it in an oven at 70°C for 12 hours for later use; weigh 70g of silicon powder and 13g of graphite powder and place them in a turpentine ball mill jar for ball milling Mixing treatment for 8 hours, put the powder mixed by the ball mill into the graphite crucible, embed the dried carbon / carbon composite material into the mixed powder, so that the mixed powder completely covers the C / C composite material; put the graphite crucible into In the vacuum reaction furnace, after the vacuum treatment of the vacuum furnace, the argon gas was passed to normal pressure, and the furnace temperature was raised from room temperature to 2100 °C at a heating rate of 9 °C / min, and kept for 1 hour, and then the power was turned off and naturally cooled to room temperature. Argon protection was used throughout the process. Weigh 9g of silicon carbide powder and 1g of silicon...

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Abstract

The invention relates to a method for preparing a SiO2-SiC mosaic structure microporous antioxidant coating on the surface of a carbon/carbon composite material, which is used for relieving the problem that a ceramic coating is easy to crack due to thermal mismatch and improving the oxidation resistance of the carbon/carbon composite material. According to the technical scheme, a compact SiC-Si inner coating is prepared on the surface of a carbon/carbon composite material through an embedding method, then a porous SiC-Si outer coating is prepared through a slurry method and heat treatment, finally, through high-temperature pre-oxidation, oxygen is rapidly diffused in the porous outer coating, SiC particles are oxidized, and the SiO2-SiC mosaic structure microporous anti-oxidation coating is formed. The structure has very good oxygen diffusion resistance, the existence of micropores also has an inhibition effect on crack propagation generated in the oxidation process, and the coating shows good thermal shock resistance in a 1500 DEG C air environment.

Description

technical field [0001] The invention belongs to the field of anti-oxidation coatings for carbon / carbon composite materials, and relates to a method for preparing SiO on the surface of carbon / carbon composite materials 2 -A method for SiC mosaic structure microporous anti-oxidation coating. Background technique [0002] Carbon / carbon composite materials have excellent properties such as low density, high specific strength, impact resistance and friction resistance, especially the mechanical properties at high temperature are higher than those at room temperature, making them extremely useful as ultra-high temperature thermal structural materials in aerospace and other fields prospect. However, carbon / carbon composites are prone to oxidation in a high-temperature aerobic environment, causing damage to the carbon matrix and carbon fibers, resulting in a significant decline in the mechanical properties of carbon / carbon composites. In order to protect carbon / carbon composites f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B41/89
CPCC04B41/89C04B41/52C04B41/009C04B35/83C04B41/5096C04B41/5059C04B41/4545C04B41/5035C04B41/456
Inventor 张雨雷朱肖飞张建陈慧
Owner NORTHWESTERN POLYTECHNICAL UNIV
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