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Preparation method of carbon/carbon composite material MoB2 anti-oxidation outer coating

A carbon composite material and anti-oxidation technology, which is applied in the field of preparation of carbon/carbon composite material MoB2 anti-oxidation outer coating, can solve the problems of easy cracking on the surface of the outer coating, inability to complete the preparation at one time, and insufficient coating thickness, etc., to achieve The effect of short preparation cycle, uniform thickness and low cost

Active Publication Date: 2014-12-24
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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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 must be heat treated in an inert atmosphere. The preparation cycle Relatively long [Bemeburg P L, Krukonis V J.Processing of carbon / carbon composites using supercritical fluid technology[P].United States Patent US5035921,1991], the coating prepared by the in-situ forming method needs to be treated at a high temperature of 1500°C, and Can not be prepared at one time [Huang Jian-Feng, Li He-Jun, Zeng Xie-Rong, Li Ke-Zhi.Surf.coat.Technol.2006,200,5379.], the outer coating prepared by sol-gel method The surface 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.], while using The coating prepared by the slurry coating reaction method still has the disadvantages of multiple coatings, which cannot be completed at one time, and requires post-heat treatment [Fu Qian-Gang, Li He-Jun, Wang Yong-Jie, Li Ke-Zhi, Tao Jun. Surface & Coating Technology.2010,204,1832.], although some alloy coatings have been prepared by using explosive spraying and ultrasonic spraying methods, the process still has many imperfections, and the prepared high-temperature oxidation resistance still needs further improvement. [Terentieva V S, Bogachkova O P, Goriatcheva E V.Method for protecting products made of a refractory material against oxidation, and resulting products[p].US 5677060,1997.]

Method used

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  • Preparation method of carbon/carbon composite material MoB2 anti-oxidation outer coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) First take MoB 2 Powder, dispersed in 150mL of methanol with a purity ≥ 99.8%, prepared into a suspension with a concentration of 40g / L, then put the suspension into a 500W ultrasonic generator to vibrate for 30min, took it out, put it into a magnetic rotor, and placed it in a magnetic stirring Stirred on the mixer for 4h to obtain suspension A, wherein, MoB 2 The powder is wet ball milled for 36 hours, dried at 80°C for 4 hours, and the average particle size is 100-300nm;

[0024] 2) Add iodine bromide with a purity of ≥99.7% to the suspension A, prepare a solution with a concentration of iodine bromide of 4.0g / L, put it into a 500W ultrasonic generator and shake for 30min, take it out and place it on a magnetic stirrer Stir for 4h to obtain solution B;

[0025] 3) Pour solution B into the hydrothermal reaction kettle, and the filling degree is controlled at 70%; then clamp the carbon / carbon composite material sample with SiC inner coating on the cathode clamp in ...

Embodiment 2

[0028] 1) First take MoB 2 Powder, dispersed in 150mL of methanol with a purity ≥ 99.8%, prepared into a suspension with a concentration of 40g / L, then put the suspension into an 800W ultrasonic generator to vibrate for 40min, took it out, put it into a magnetic rotor, and placed it in a magnetic stirring Stirred on the mixer for 4h to obtain suspension A, wherein, MoB 2 The powder is wet ball milled for 36 hours, dried at 80°C for 4 hours, and the average particle size is 100-300nm;

[0029] 2) Add iodine bromide with a purity ≥ 99.7% to the suspension A, prepare a solution with a concentration of iodine bromide of 4.0g / L, put it into a 500W ultrasonic generator and shake for 40min, take it out and put it on a magnetic stirrer Stir for 4h to obtain solution B;

[0030] 3) Pour solution B into the hydrothermal reaction kettle, and the filling degree is controlled at 70%; then clamp the carbon / carbon composite material sample with SiC inner coating on the cathode clamp in the...

Embodiment 3

[0033] 1) First take MoB 2 Powder, dispersed in 150mL of methanol with a purity ≥ 99.8%, prepared into a suspension with a concentration of 45g / L, then put the suspension into a 500W ultrasonic generator to vibrate for 60min, took it out, put it into a magnetic rotor, and placed it in a magnetic stirring Stirred on the mixer for 4h to obtain suspension A, wherein, MoB 2 The powder is wet ball milled for 36 hours, dried at 80°C for 4 hours, and the average particle size is 100-300nm;

[0034] 2) Add iodine bromide with a purity ≥ 99.7% to the suspension A, prepare a solution with an iodine bromide concentration of 5.0g / L, put it into an 800W ultrasonic generator and shake it for 60min, take it out and place it on a magnetic stirrer Stir for 4h to obtain solution B;

[0035] 3) Pour solution B into the hydrothermal reaction kettle, and the filling degree is controlled at 70%; then clamp the carbon / carbon composite material sample with SiC inner coating on the cathode clamp in ...

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Abstract

The invention provides a preparation method of a carbon / carbon composite material MoB2 anti-oxidation outer coating. The preparation method comprises the following steps of dispersing MoB2 powder in methanol, performing ultrasonic oscillation and stirring to obtain a suspension A; adding iodine bromide into the suspension A, performing ultrasonic oscillation, and stirring to obtain a solution B; pouring the solution B into a hydrothermal reaction kettle and controlling the filling degree to be 70-80%; then clamping a carbon / carbon composite material test sample with a SiC inner coating on a cathode clamp in the hydrothermal kettle, and placing the hydrothermal kettle into an oven; respectively connecting a positive electrode and a negative electrode of the hydrothermal kettle onto two corresponding electrodes of a pulsed power supply, and naturally cooling to room temperature after the end of hydrothermal electrophoresis electric arc discharge; opening the hydrothermal kettle, taking out the test sample and then drying to obtain the carbon / carbon composite material MoB2 anti-oxidation outer coating. The carbon / carbon composite material MoB2 anti-oxidation outer coating prepared by the preparation method provided by the invention has the advantages of uniform thickness and no cracks on the surface; the adopted process method has the advantages of simplicity in preparation, convenience in operation, easiness in obtainment of raw materials, short preparation period and low cost.

Description

【Technical field】 [0001] The invention relates to a method for preparing a carbon / carbon composite material composite outer coating, in particular to a carbon / carbon composite material MoB 2 Preparation method of oxidation resistant outer coating. 【Background technique】 [0002] C / C composite material is also called carbon fiber carbon-based composite material. Because 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 has the advantages of high temperature resistance. Has excellent mechanical properties. In particular, its strength does not decrease but increases with the increase of temperature, making it one of the promising high-tech new materials, and is widely used as ablation materials and thermal structural materials in the field of aviation and aerospace technology. However, C / C composites are rapidly oxidized i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B41/85
Inventor 黄剑锋张永亮曹丽云郝巍张博烨
Owner SHAANXI UNIV OF SCI & TECH
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