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Preparation method of carbon/carbon composite material HfB2 anti-oxidation outer coating

A carbon composite material and anti-oxidation technology, which is applied in the field of preparation of carbon/carbon composite HfB2 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 thickness of the coating, etc., to achieve Combining the effects of high strength, controllable structure and convenient operation

Active Publication Date: 2014-12-24
SHAANXI UNIV OF SCI & TECH
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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 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 Although some alloy coatings have been prepared by explosive spraying and ultrasonic spraying, there are still many imperfections in this process, and the high-temperature oxidation resistance of the prepared coatings needs to be further improved [Terentieva V S, Bogachkova O P, Goriatcheva E V. Method for protecting products made of a refractory material against oxidation, and resulting products[p].US5677060,1997.]

Method used

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  • Preparation method of carbon/carbon composite material HfB2 anti-oxidation outer coating

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) First take HfB 2 The powder is then dispersed in 150mL of isopentenol with a purity ≥ 99.8%, and prepared into a suspension with a concentration of 20g / L. Then, the suspension is placed in a 500W ultrasonic generator and shaken for 40min. After taking it out, put it into a magnetic rotor. Placed on a magnetic stirrer and stirred for 5h to obtain suspension A, wherein, HfB 2 The powder is wet ball milled and dried at 80°C for 4 hours, with an average particle size of 100-300nm;

[0026] 2) Add elemental iodine with a purity ≥ 99.7% to the suspension A, prepare a solution with an elemental iodine concentration of 3.0g / L, put it into a 500W ultrasonic generator and shake for 40min, take it out and stir it on a magnetic stirrer 5h to obtain solution B;

[0027] 3) Pour solution B into a device that uses graphite electrodes as anodes and conductive substrates as cathodes. The cathodes are fixed on the rotating body and rotated under the drive of the motor. The cathode a...

Embodiment 2

[0030] 1) First take HfB 2 The powder is then dispersed in 150mL of isopentenol with a purity ≥ 99.8%, and prepared into a suspension with a concentration of 20g / L. Then, the suspension is placed in a 600W ultrasonic generator and shaken for 40 minutes. After taking it out, put it into a magnetic rotor. Placed on a magnetic stirrer and stirred for 5h to obtain suspension A, wherein, HfB 2 The powder is wet ball milled and dried at 80°C for 4 hours, with an average particle size of 100-300nm;

[0031] 2) Add elemental iodine with a purity ≥ 99.7% to the suspension A, prepare a solution with an elemental iodine concentration of 3.0g / L, put it into a 600W ultrasonic generator and shake for 40min, take it out and stir it on a magnetic stirrer 5h to obtain solution B;

[0032] 3) Pour solution B into a device that uses graphite electrodes as anodes and conductive substrates as cathodes. The cathodes are fixed on the rotating body and rotated under the drive of the motor. The cath...

Embodiment 3

[0035] 1) First take HfB 2 The powder is then dispersed in 200mL of prenyl alcohol with a purity ≥ 99.8%, and prepared into a suspension with a concentration of 25g / L. Then, the suspension is placed in an 800W ultrasonic generator and shaken for 60 minutes. After taking it out, put it into a magnetic rotor. Placed on a magnetic stirrer and stirred for 5h to obtain suspension A, wherein, HfB 2 The powder is wet ball milled and dried at 80°C for 5 hours, with an average particle size of 100-300nm;

[0036] 2) Add elemental iodine with a purity ≥ 99.7% to the suspension A, prepare a solution with an elemental iodine concentration of 3.0g / L, put it into an 800W ultrasonic generator and vibrate for 60min, take it out and stir it on a magnetic stirrer 5h to obtain solution B;

[0037] 3) Pour solution B into a device that uses graphite electrodes as anodes and conductive substrates as cathodes. The cathodes are fixed on the rotating body and rotated under the drive of the motor. T...

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Abstract

The invention provides a preparation method of a carbon / carbon composite material HfB2 anti-oxidation outer coating. The preparation method comprises the following steps of dispersing HfB2 powder in 3-methyl-2-buten-1-ol, performing ultrasonic oscillation and stirring to obtain a suspension A; adding an iodine elementary substance into the suspension A, performing ultrasonic oscillation and stirring to obtain a solution B; pouring the solution B into a device which takes a graphite electrode as an anode, takes a conductive matrix as a cathode, fixes the cathode on a rotating body and can rotate under the drive of a motor, wherein the cathode and anode of the device are connected with two corresponding electrodes of a constant-current power supply; then clamping a C / C composite material test sample with a SiC inner coating on the cathode in the device, placing the device into a constant-temperature oven, and closing the power supply of the device and the oven after the end of the reaction; opening the device, taking out the test sample and then drying to obtain the carbon / carbon composite material HfB2 anti-oxidation outer coating. The carbon / carbon composite material HfB2 anti-oxidation outer coating has no cracks on the surface and great bonding strength of the coating; the process is simple, raw materials are easy to obtain, and the preparation cost is relatively low.

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 HfB 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王丹
Owner SHAANXI UNIV OF SCI & TECH
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