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A kind of preparation method of carbon/carbon composite material mullite whisker toughened mullite composite coating

A technology of mullite whiskers and carbon composite materials, which is applied in the field of preparing carbon/carbon composite composite outer coatings, can solve the problems that the preparation cannot be completed at one time, the surface of the outer coating is easy to crack, and the thickness of the coating is insufficient. The effect of controllable structure, smooth surface and short reaction cycle

Active Publication Date: 2016-02-10
INST OF FLEXIBLE ELECTRONICS TECH OF THU ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of supercritical fluid technology to prepare C / C composite coatings requires high temperature and high pressure for the preparation process, which requires high equipment requirements, and the formed outer coating should be heat treated in an inert atmosphere, and the preparation cycle It is relatively long [BemeburgPL, KrukonisVJ.Processingofcarbon / carboncompositesusingsupercriticalfluidtechnology[P].UnitedStatesPatentUS5035921,1991], the coating prepared by the in-situ forming method needs to be treated at a high temperature of 1500°C, and cannot be prepared at one time [HuangJian-Feng, LiHe-Jun, ZengXie-Rong, LiKe-Zhi.Surf.coat.Technol.2006,200,5379.], the surface of the outer coating prepared by sol-gel method is easy to crack and the coating thickness is insufficient [HuangJian-Feng, ZengXie-Rong, LiHe-Jun, XiongXin-Bo, SunGuo-ling.Surf.coat.Technol.2005,190,255.], and although adopting detonation spraying and ultrasonic spraying method to prepare part alloy coating, still, this technology still has many imperfections Where, the high-temperature anti-oxidation performance of the prepared coating still needs to be further improved
However, the method of preparing mullite whisker toughened mullite composite outer coating by ultrasonic-double pulse hydrothermoelectrophoresis deposition method has not been reported yet.

Method used

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  • A kind of preparation method of carbon/carbon composite material mullite whisker toughened mullite composite coating
  • A kind of preparation method of carbon/carbon composite material mullite whisker toughened mullite composite coating

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Experimental program
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Effect test

Embodiment 1

[0025] 1) Choose mullite powder (commercially available mullite powder is dry-milled for 12-24 hours, and the average particle size is controlled at about 1 μm), commercially available mullite whiskers (length-to-diameter ratio is 100-200), Commercially available carbon iodide (purity ≥ 99.7%) and sec-butanol (purity ≥ 99.8%) are raw materials;

[0026] 2) First, disperse the mixed powder composed of mullite powder and mullite whiskers in 100mL of sec-butanol, and prepare suspension A1 with a mixed powder concentration of 30g / L, and the mullite in the mixed powder The mass fraction of the powder is 50%, the mass fraction of the mullite whiskers is 50%, the suspension A1 is ultrasonically oscillated for 60min, the ultrasonic power is 500W, and then placed on a magnetic stirrer to stir for 36h, while stirring, heating, heating The temperature was controlled at 40°C to obtain suspension A2;

[0027] 3) Add carbon iodide to the suspension A2 to obtain a mixture, the concentration...

Embodiment 2

[0032] 1) Choose mullite powder (commercially available mullite powder is dry-milled for 12-24 hours, and the average particle size is controlled at about 1 μm), commercially available mullite whiskers (length-to-diameter ratio is 100-200), Commercially available carbon iodide (purity ≥ 99.7%) and sec-butanol (purity ≥ 99.8%) are raw materials;

[0033] 2) First, disperse the mixed powder composed of mullite powder and mullite whiskers in 120mL of sec-butanol, and prepare suspension A1 with a mixed powder concentration of 35g / L, and the mullite in the mixed powder The mass fraction of powder is 55%, the mass fraction of mullite whiskers is 45%, the suspension A1 is ultrasonically oscillated for 70min, the ultrasonic power is 400W, and then placed on a magnetic stirrer to stir for 40h, while stirring, heating, heating The temperature was controlled at 50°C to obtain suspension A2;

[0034] 3) Add carbon iodide to the suspension A2 to obtain a mixture, the concentration of carb...

Embodiment 3

[0038] 1) Choose mullite powder (commercially available mullite powder is dry-milled for 12-24 hours, and the average particle size is controlled at about 1 μm), commercially available mullite whiskers (length-to-diameter ratio is 100-200), Commercially available carbon iodide (purity ≥ 99.7%) and sec-butanol (purity ≥ 99.8%) are raw materials;

[0039] 2) First, disperse the mixed powder composed of mullite powder and mullite whiskers in 120mL of sec-butanol, and prepare a suspension A1 with a mixed powder concentration of 40g / L. The mullite in the mixed powder The mass fraction of the powder is 60%, the mass fraction of the mullite whiskers is 40%, the suspension A1 is ultrasonically oscillated for 80min, the ultrasonic power is 300W, and then placed on a magnetic stirrer to stir for 40h, while stirring, heating, heating The temperature was controlled at 60°C to obtain suspension A2;

[0040] 3) Add carbon iodide to the suspension A2 to obtain a mixture, the concentration o...

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Abstract

The invention provides a preparation method of a carbon / carbon composite material mullite whisker toughened mullite composite coating. The preparation method comprises the following steps: dispersing mullite powder and mullite whiskers into sec-butyl alcohol, performing ultrasonic oscillation on the mixture, and stirring the mixture while heating the mixture to obtain a suspension A2; adding carbon iodide into the suspension A2, and stirring the mixture while heating the mixture to obtain a suspension B; and pouring the suspension B into a hydrothermal kettle in which a graphite electrode is taken as an anode and a conductive substrate as a cathode, performing ultrasonic dual-pulse hydrothermal electrophoretic deposition, and drying a test sample. The carbon / carbon composite material mullite whisker toughened mullite composite outer coating prepared by using the method is uniform in thickness, is free from penetration cracks and micropores, and has high bonding strength with a substrate. The preparation method is implemented at one time in the hydrothermal kettle without subsequent thermal treatment, and has the advantages of simple preparation process, short reaction period, convenience in operation, adoption of readily-available raw materials, low preparation cost and wide development prospect.

Description

technical field [0001] The invention relates to a method for preparing a carbon / carbon composite material composite outer coating, in particular to a method of ultrasonic-double-pulse hydrothermoelectrophoresis deposition of a carbon / carbon composite material mullite whisker toughened mullite composite outer coating Preparation. Background technique [0002] C / C composite material is a carbon-based composite material with carbon fiber as the reinforcing phase. Since it is only composed of a single carbon element, it not only has the advantages of excellent ablation resistance, low density, and low thermal expansion coefficient of carbon and graphite materials, but also It also has excellent mechanical properties at high temperatures, such as high strength, high modulus, good fracture toughness and wear resistance. In particular, its strength does not decrease but increases with the increase of temperature, making it one of the most promising high-tech new materials, and is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B41/85
Inventor 黄剑锋周磊张永亮李翠艳欧阳海波郝巍
Owner INST OF FLEXIBLE ELECTRONICS TECH OF THU ZHEJIANG