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Hf (Ta) C ultra-high-temperature composite coating and preparation method thereof

An ultra-high temperature coating technology, applied in the field of HfC ultra-high temperature multi-phase coating and its preparation, can solve the problems that are difficult to meet the ablation environment of solid rocket engine throat lining, and achieve excellent ablation resistance and thermal shock resistance Superior performance and anti-ablation performance, combined with good effect

Active Publication Date: 2012-12-12
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The application of a single coating for anti-ablation protection of carbon / carbon composites has its limitations, and it is difficult to meet the complex ablation environment of solid rocket motor throat linings

Method used

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  • Hf (Ta) C ultra-high-temperature composite coating and preparation method thereof
  • Hf (Ta) C ultra-high-temperature composite coating and preparation method thereof
  • Hf (Ta) C ultra-high-temperature composite coating and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0037] First, the C / C composite material was polished and polished with SiC sandpaper, cleaned with ultrasonic alcohol for 30 minutes, and dried in vacuum at 120°C for 2 hours before use; the hafnium tetrachloride and tantalum pentachloride powders were placed in a vacuum glove box, and placed under argon protection. The two powders are mechanically mixed at a molar ratio of 4 / 1; the obtained multi-component precursor mixed powder is placed in a mechanical powder feeding device, and the surface-treated carbon / carbon composite material substrate is placed in a low-pressure chemical vapor deposition furnace.

[0038] Turn on the vacuum system to keep the vapor deposition furnace at low pressure (lower than 100Pa); turn on the argon protection, turn on the heating system, and heat up to 1300°C at a heating rate of 5°C / min; after the temperature rises to 1300°C, put in hydrogen . After the temperature in the furnace is stabilized, methane is introduced, and the CH 4 / H 2 =1 / 8、CH...

Embodiment 2

[0042] Firstly, the graphite was polished and polished with SiC sandpaper, cleaned with ultrasonic alcohol for 30 min, and vacuum-dried at 120°C for 2 h for later use; the powders of hafnium tetrachloride and tantalum pentachloride were placed in a vacuum glove box, and the two powders were separated under the protection of argon. The molar ratio is 1 / 1 mechanical mixing; the obtained multi-component precursor mixed powder is placed in a mechanical powder feeding device, and the surface-treated carbon / carbon composite material substrate is placed in a low-pressure chemical vapor deposition furnace.

[0043] Turn on the vacuum system to keep the vapor deposition furnace at low pressure (lower than 100Pa); turn on the argon gas protection, turn on the heating system, and heat up to 1650°C at a heating rate of 8°C / min; after the temperature rises to 1650°C, put in hydrogen . After the temperature in the furnace is stabilized, methane is introduced, and the CH 4 / H 2 =1 / 20,CH 4...

Embodiment 3

[0047] Firstly, the ZrC ceramics were polished and polished with SiC sandpaper, cleaned with ultrasonic alcohol for 30 minutes, and then vacuum-dried at 120°C for 2 hours for later use. Physical mixing at a molar ratio of 10 / 1; the obtained multi-component precursor mixed powder is placed in a mechanical powder feeding device, and the surface-treated carbon / carbon composite material substrate is placed in a low-pressure chemical vapor deposition furnace.

[0048] Turn on the vacuum system to keep the vapor deposition furnace at low pressure (lower than 100Pa); turn on the argon gas protection, turn on the heating system, and heat up to 1400°C at a heating rate of 10°C / min; after the temperature rises to 1400°C, put in hydrogen . After the temperature in the furnace is stabilized, methane is introduced, and the CH 4 / H 2 =1 / 1,CH 4 / (HfCl 4 +TaCl 5 ) = 5 / 1, and at the same time turn on the mechanical powder feeding device, control the internal pressure of the reaction furna...

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Abstract

The invention discloses a Hf (Ta) C ultra-high-temperature composite coating, which consists of HFC with HfTaC2, wherein the molar fraction of HfTaC2 is 6-50 percent, and the HfTaC2 is distributed in the coating uniformly or in a gradient way. The preparation method comprises the steps of: placing a surface-treated substrate material into a low-voltage chemical vapor deposition furnace, and usingmixed powder of hafnium tetrachloride and tantalum pentachloride as a hafnium source and a tantalum source, methane as a carbon source, argon as a diluent gas and hydrogen as a reducing gas; and delivering the mixed powder into a reactor of the deposition furnace, and preparing the Hf (Ta) C ultra-high-temperature composite coating by surface deposition on the substrate material. Limitations of asingle coating in ablation can be overcome, advantages of all phases of the coating can be fully utilized, and requirements for long-time high-temperature protection of the substrate material can be satisfied. The process is simple and convenient to operate, the prepared coating is well combined with the substrate, no interlayer cracks or penetrating cracks can be produced, and the thermal shock resistance and ablation resistance are excellent. The Hf (Ta) C ultra-high-temperature composite coating is suitable for surface coating and high-temperature protection of carbon / carbon composite materials, carbon / ceramic composite materials, graphite, carbide ceramics and other materials.

Description

technical field [0001] The invention relates to a Hf(Ta)C ultra-high temperature multi-phase coating and a preparation method thereof, which belongs to the technical field of chemical vapor deposition and is suitable for carbon / carbon composite materials, carbon / ceramic composite materials, graphite, carbide ceramics and other materials Surface coating and high temperature protection. technical background [0002] Carbon / carbon composites have excellent high-temperature mechanical properties, low thermal expansion coefficient, high thermal conductivity, and good thermal shock resistance. They are ideal ablation structural materials for throat linings of solid rocket motors. The rapid oxidation of carbon / carbon composite throat lining in the high temperature aerobic environment above 500 ℃ will lead to the rapid attenuation of its mechanical properties. If the throat lining is severely ablated during operation, it will be difficult to maintain a stable aerodynamic shape, whi...

Claims

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Application Information

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IPC IPC(8): C04B41/85C04B35/66
Inventor 熊翔王雅雷李国栋孙威陈招科赵学嘉
Owner CENT SOUTH UNIV
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