Method for preparing carbon/carbon composite material nanometer silicon carbide-mullite composite external coating

A carbon composite material and nano-silicon carbide technology, which is applied in the field of preparing carbon/carbon composite material composite outer coating, can solve the problems of easy cracking coating thickness, instant noodles cracking, shortage, etc., and achieves improved high-temperature oxidation resistance, high heat Effects of stability and antioxidant properties, good physicochemical compatibility

Inactive Publication Date: 2012-05-23
SHAANXI UNIV OF SCI & TECH
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  • Abstract
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Problems solved by technology

The surface of the outer coating prepared by the sol-gel method is easy to crack and the coating thickness is insufficient [Huang Jian-Feng, Zeng Xie-Rong, Li He-Jun, Xiong Xin-Bo, Sun Guo-ling.Surf.coat. Technol.2005, 190, 255.], the silicon carbide coating prepared by the embedding method has a large stress on the surface, so it is also prone to cracking of instant noodles [Fu Qian-Gang, Li He-Jun, Shi Xiao-Hong, Li Ke-Zhi, Sun Guo-Dong. Scripta Mater.2005, 52, 923.], while the coating prepared by the in-situ forming method needs to be treated at 1500 °C at a high temperature, and cannot be prepared at one time [Huang Jian -Feng, Li He-Jun, Zeng Xie-Rong, Li Ke-Zhi.Surf.coat.Technol.2006, 200, 5379.], also using the slurry coating reaction method to prepare the coating still requires multiple brushes It cannot be prepared in one time and needs post-heat treatment [Huang Min, Li Ke-Zhi, Li He-Jun, Fu Qian-Gang, Sun Guo-DongCarbon.2007, 45, 1105.]

Method used

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  • Method for preparing carbon/carbon composite material nanometer silicon carbide-mullite composite external coating
  • Method for preparing carbon/carbon composite material nanometer silicon carbide-mullite composite external coating
  • Method for preparing carbon/carbon composite material nanometer silicon carbide-mullite composite external coating

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Embodiment 1

[0012] Example 1: 1) Preparation of acicular mullite powder First, 4ml of SiO 2 %≥28% tetraethyl orthosilicate was dissolved in 20ml of absolute ethanol, then 10ml of distilled water was added, the pH of the solution was adjusted to 2 with hydrochloric acid, and magnetically stirred for 0.5h at room temperature to fully prehydrolyze the tetraethyl orthosilicate, calculated as Solution A; Secondly, take 24g of Al(NO 3 ) 3 9H 2 Add O into 10ml of distilled water and stir until Al(NO 3 ) 3 9H 2After O is fully dissolved, pour it into solution A, place the mixed solution on a magnetic stirrer and stir evenly, then adjust the pH value to 4.5 with ammonia water, and calculate it as solution B; then, dry solution B at 60°C to dry Then put the dry gel into the microwave hydrothermal reaction kettle, add distilled water to the 2 / 3 of the volume of the reaction kettle, and control the temperature at 160°C in the microwave reactor. Finally, the dried samples were calcined in a muff...

Embodiment 2

[0013] Example 2: 1) Preparation of acicular mullite powder First, 5ml of SiO 2 %≥28% ethyl orthosilicate was dissolved in 20ml of absolute ethanol, then 15ml of distilled water was added, the pH value of the solution was adjusted to 3 with hydrochloric acid, magnetically stirred at room temperature for 1.5h to fully pre-hydrolyze the orthosilicate, calculated as Solution A; Secondly, take 25.5g of Al(NO 3 ) 3 9H 2 O was added to 15ml of distilled water and stirred at room temperature until Al(NO 3 ) 3 9H 2 After O is fully dissolved, pour it into solution A, place the mixed solution on a magnetic stirrer and stir evenly, then adjust the pH value to 5 with ammonia water, and calculate it as solution B; then, dry solution B at 60°C to dry Then put the dry gel into the microwave hydrothermal reaction kettle, add distilled water to the 2 / 3 of the volume of the reaction kettle, and control the temperature at 180°C in the microwave reactor. Finally, the dried samples were cal...

Embodiment 3

[0014] Embodiment 3: 1) Preparation of acicular mullite powder At first, the SiO of 6ml 2 %≥28% ethyl orthosilicate is dissolved in 20ml of absolute ethanol, then add 20ml of distilled water, adjust the pH value of the solution to 4 with hydrochloric acid, stir magnetically for 3 hours at room temperature to fully pre-hydrolyze the orthosilicate, and count it as a solution A; Secondly, take 27g of Al(NO 3 ) 3 9H 2 O was added to 20ml of distilled water, and stirred at room temperature until Al(NO 3 ) 3 9H 2 After O is fully dissolved, pour it into solution A, place the mixed solution on a magnetic stirrer and stir evenly, then adjust the pH value to 5.5 with ammonia water, and calculate it as solution B; then, dry solution B at 60°C to dry Then put the dry gel into the microwave hydrothermal reaction kettle, add distilled water to the 2 / 3 of the volume of the reaction kettle, and control the temperature at 200°C in the microwave reactor. Finally, the dried samples were c...

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Abstract

The invention provides a method for preparing carbon / carbon composite material nanometer silicon carbide-mullite composite external coating. The method comprises the following steps: adding mullite powder and nanometer silicon carbide powder into isopropanol for ultrasonic oscillation, adding iodine into the mixture for another ultrasonic oscillation, and placing the mixture in a hydrothermal reaction kettle; clamping the carbon / carbon composite material test sample with SiC internal coating on a cathode clip in the hydrothermal kettle for hydrothermal electrophoresis reaction, taking out anddrying the test sample to obtain the carbon / carbon composite material nanometer silicon carbide-mullite composite external coating. The mullite adopted as the C / C-SiC external coating has higher thermal stability and oxidation resistance, and has melting point more than 1,800 DEG C. The coefficient of thermal expansion of the mullite is close to that of the SiC, so the mullite cannot generate thermal stress at high temperature. The mullite can generate SiO2 and Al2O3 with low penetration and excellent high-temperature stability with oxygen at high temperature, additionally; nanometer silicon carbide particles can effectively overcome microcrack and other defects of the SiC internal coating, so that the high-temperature oxidation resistance of the coating can be greatly improved.

Description

technical field [0001] The invention relates to a method for preparing a composite outer coating of a carbon / carbon composite material, in particular to a carbon / carbon composite material prepared by hydrothermal electrophoretic deposition with a uniform surface and no micro-cracks, and a uniform thickness without penetrating holes and cracks A method for nano-silicon carbide-mullite composite outer coating. Background technique [0002] In recent years, carbon / carbon (C / C) composites have gradually become a research hotspot. Due to the characteristics of low thermal expansion coefficient, low density, ablation resistance, corrosion resistance, stable friction coefficient, good thermal and electrical conductivity, high strength and high modulus of carbon / carbon composite materials, especially the mechanical properties do not decrease but increase with the increase of temperature. characteristics, so it is used in aviation, aerospace and civil industry. However, many of its...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B41/85
Inventor 黄剑锋王博杨强曹丽云曾燮榕吴建鹏刘淼
Owner SHAANXI UNIV OF SCI & TECH
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