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Method for preparing carbon/carbon composite MoSi2-ZrSiO4-SiC gradient complex outer coating

A carbon composite material and outer coating technology, which is applied in the field of preparing carbon/carbon composite material composite outer coating, can solve the problems of easy cracking on the surface of the outer coating, cannot be completed in one preparation, and insufficient coating thickness, and achieves excellent resistance to The effect of high temperature oxidation performance, easy control of deposition process and low cost

Active Publication Date: 2013-04-17
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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. The improvement of [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.], and the preparation of coatings by hydrothermoelectrophoretic deposition[ Huang Jianfeng, Wang Bo, Li Hejun, Liu Miao, Cao Liyun, Yao Chunyan. A MoSi 2 / SiC oxidation protective coating for carbon / carbon composites[J].Corrosion Science,2011,2(53):834-839.]

Method used

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  • Method for preparing carbon/carbon composite MoSi2-ZrSiO4-SiC gradient complex outer coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) Take commercially available molybdenum disilicide powder with a particle size of 3-6 μm and micron-scale analytically pure ZrSiO through dry ball milling 4 Powder and nano-silicon carbide powder with a particle size of 40nm, according to ZrSiO 4 :SiC:MoSi 2 = 1:10:1 mass ratio mixed and dispersed in ethanol with a purity ≥ 99.8% to prepare suspension A with a concentration of 40g / L;

[0031] By ZrSiO 4 :SiC:MoSi 2 = 5:5:5 mass ratio mixed and dispersed in ethanol with a purity ≥ 99.8% to prepare a suspension B with a concentration of 50g / L;

[0032] By ZrSiO 4 :SiC:MoSi 2 = 12:5:10 mass ratio mixed and dispersed in ethanol with a purity ≥ 99.8% to prepare a suspension C with a concentration of 60g / L;

[0033] 2) Put the suspensions A, B, and C into a 500W ultrasonic generator and vibrate for 100 minutes, take them out, and place them on a magnetic stirrer for 12 hours;

[0034] 3) Add elemental tellurium with a purity of ≥99.7% to the suspensions A, B, and C r...

Embodiment 2

[0039] 1) Take commercially available molybdenum disilicide powder with a particle size of 3-6 μm and micron-scale analytically pure ZrSiO through dry ball milling 4 Powder and nano-silicon carbide powder with a particle size of 40nm, according to ZrSiO 4 :SiC:MoSi 2 =5:13:8 mass ratio mixed and dispersed in ethanol with a purity ≥99.8% to prepare a suspension A with a concentration of 40g / L;

[0040] By ZrSiO 4 :SiC:MoSi 2 = 10:10:12 mass ratio mixed and dispersed in ethanol with a purity ≥ 99.8% to prepare a suspension B with a concentration of 50g / L;

[0041] By ZrSiO 4 :SiC:MoSi 2 = 15:10:12 mass ratio mixed and then dispersed in ethanol with a purity ≥ 99.8% to prepare a suspension C with a concentration of 60g / L;

[0042] 2) Put the suspensions A, B, and C into an 800W ultrasonic generator to vibrate for 80 minutes, take them out, and place them on a magnetic stirrer for 18 hours;

[0043] 3) Add elemental tellurium with a purity of ≥99.7% to the suspensions A, B,...

Embodiment 3

[0048] 1) Take commercially available molybdenum disilicide powder with a particle size of 3-6 μm and micron-scale analytically pure ZrSiO through dry ball milling 4 Powder and nano-silicon carbide powder with a particle size of 40nm, according to ZrSiO 4 :SiC:MoSi 2 = 10:20:10 mass ratio mixed and then dispersed in ethanol with a purity ≥ 99.8% to prepare suspension A with a concentration of 40g / L;

[0049] By ZrSiO 4 :SiC:MoSi 2 =8:12:10 mass ratio mixed and dispersed in ethanol with a purity ≥ 99.8% to prepare a suspension B with a concentration of 50g / L;

[0050] By ZrSiO 4 :SiC:MoSi 2 = 10:1:15 mass ratio mixed and then dispersed in ethanol with a purity ≥ 99.8% to prepare a suspension C with a concentration of 60g / L;

[0051] 2) Put the suspensions A, B, and C into a 1000W ultrasonic generator to vibrate for 60 minutes, take them out, and place them on a magnetic stirrer for 24 hours;

[0052] 3) Add elemental tellurium with a purity of ≥99.7% to the suspensions A, ...

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Abstract

The invention discloses a method for preparing a carbon / carbon composite MoSi2-ZrSiO4-SiC gradient complex outer coating. The MoSi2-ZrSiO4-SiC gradient complex outer coating is prepared with a cathode rotating microwave hydrothermal pulsed arc discharge deposition method; microwave presents self-heating and high efficiency in a reaction system, and generated partial high temperature and high pressure can effectively reduce the reaction activation energy of MoSi2, ZrSiO4 and SiC suspended particles, so that reaction of the suspended particles is more complete and sufficient in a pulsed arc discharge depotition process, and the coating with a dense structure is obtained. In addition, as a cathode rotates at a high speed, the defect that a coating with a dense and uniform structure can only be obtained through coating repeatedly with the traditional hydrothermal method is avoided, and the dense MoSi2-ZrSiO4-SiC gradient complex outer coating with microscopic cracks and different thicknesses can be obtained under controllable conditions. According to the MoSi2-ZrSiO4-SiC gradient complex outer coating prepared with the method, nano silicon carbide is diffused in the coating in a gradient manner, so that the defect is filled, the coating is densified, and the interfacial binding force is good.

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 for preparing a carbon / carbon composite material MoSi 2 -ZrSiO 4 - A method of SiC gradient composite overcoating. 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...

Claims

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Application Information

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IPC IPC(8): C04B41/85
Inventor 黄剑锋郝巍曹丽云费杰殷立雄王开通
Owner SHAANXI UNIV OF SCI & TECH
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