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Method for preparing carbon/carbon composite material SiC-MoSi2-C-AlPO4 composite gradient external coating

A technology of sic-mosi2-c-alpo4 and carbon composite materials, which is applied in the field of preparing carbon/carbon composite composite gradient outer coatings, can solve the problems of easy cracking of the outer coating surface, insufficient coating thickness, and high requirements. Achieve the effects of simple and efficient preparation, complete and sufficient reaction, and accelerated deposition rate

Active Publication Date: 2013-03-27
XINING GONGJIN NEW MATERIAL TECHNOLOGY CO LTD
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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 US 5035921,1991], the coating prepared by the in-situ forming method needs to be treated at a high temperature of 1500°C, And it cannot 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 of the layer 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 The preparation of the coating by the molten 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 explosive spraying and ultrasonic spraying, 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].US5677060,1997.], while the ultrasonic cathode rotating microwave hydrothermoelectrophoresis arc discharge Preparation of SiC-MoSi by Deposition Method 2 -C-AlPO 4 The method of composite gradient outer coating has not been reported yet

Method used

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  • Method for preparing carbon/carbon composite material SiC-MoSi2-C-AlPO4 composite gradient external coating
  • Method for preparing carbon/carbon composite material SiC-MoSi2-C-AlPO4 composite gradient external coating

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) Commercially available aluminum phosphate powder was calcined at 1300°C for 30 minutes, and then wet ball milled to produce C-AlPO with an average particle size of 3-6 μm 4 Powder, the commercially available molybdenum disilicide powder is dry-milled to make MoSi with an average particle size of 3-6 μm 2 powder, then C-AlPO 4 Powder, MoSi 2 Powder and nano-silicon carbide powder with an average particle size of 40nm, according to C-AlPO 4 :SiC:MoSi 2 = 1:20:1 mass ratio mixed evenly to form a mixed powder;

[0030] 2) Disperse the mixed powder in ethanol with a purity ≥ 99.8%, and prepare suspension A with a concentration of 30g / L, suspension B with a concentration of 20g / L and suspension C with a concentration of 25g / L;

[0031] 3) Put the suspensions A, B, and C into a 500W ultrasonic generator to vibrate for 40 minutes, take them out, and place them on a magnetic stirrer for 18 hours;

[0032] 4) Add elemental tellurium with a purity ≥ 99.7% to suspensions A,...

Embodiment 2

[0037] 1) Commercially available aluminum phosphate powder was calcined at 1300°C for 30 minutes, and then wet ball milled to produce C-AlPO with an average particle size of 3-6 μm 4 Powder, the commercially available molybdenum disilicide powder is dry-milled to make MoSi with an average particle size of 3-6 μm 2 powder, then C-AlPO 4 Powder, MoSi 2 Powder and nano-silicon carbide powder with an average particle size of 40nm, according to C-AlPO 4 :SiC:MoSi 2 = 1:1:1 mass ratio mixed evenly to form a mixed powder;

[0038] 2) Disperse the mixed powder in ethanol with a purity ≥ 99.8%, and prepare suspension A with a concentration of 35g / L, suspension B with a concentration of 30g / L and suspension C with a concentration of 22g / L;

[0039] 3) Put the suspensions A, B, and C into an ultrasonic generator with a power of 800W to vibrate for 60 minutes, take them out, and place them on a magnetic stirrer for 24 hours;

[0040] 4) Add elemental tellurium with a purity ≥ 99.7% t...

Embodiment 3

[0045] 1) Commercially available aluminum phosphate powder was calcined at 1300°C for 30 minutes, and then wet ball milled to produce C-AlPO with an average particle size of 3-6 μm 4 Powder, the commercially available molybdenum disilicide powder is dry-milled to make MoSi with an average particle size of 3-6 μm 2 powder, then C-AlPO 4 Powder, MoSi 2 Powder and nano-silicon carbide powder with an average particle size of 40nm, according to C-AlPO 4 :SiC:MoSi 2 = 1:2:1 mass ratio mixed evenly to form a mixed powder;

[0046] 2) Disperse the mixed powder in ethanol with a purity ≥ 99.8%, and prepare suspension A with a concentration of 32g / L, suspension B with a concentration of 25g / L and suspension C with a concentration of 30g / L;

[0047] 3) Put the suspensions A, B, and C into an ultrasonic generator with a power of 1200W to vibrate for 90 minutes, take them out, and place them on a magnetic stirrer for 36 hours;

[0048] 4) Add elemental tellurium with a purity ≥ 99.7% ...

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Abstract

The invention relates to a method for preparing a carbon / carbon composite material SiC-MoSi2-C-AlPO4 composite gradient external coating, which is completed in a hydrothermal reactor at one time, does not need late heat treatment, maintains uniform thickness and does not generate through holes and cracks. At first, C-AlPO4 powder, silicone carbide nano powder and MoSi2 powder are weighed according to the mass ratio of (1-10):(1-20):(1-10) to be mixed, suspension liquids A, B and C of 20-40 grams / liter are then prepared, are subjected to ultrasonic concussion and magnetic stirring, and are then added with tellurium simple substance to prepare suspension liquids D, E and F with the tellurium simple substance concentrations of 0.5-2.0 grams / liter, an ultrasonic cathode rotary microwave hydrothermal electrophoresis arc discharge sedimentation method is adopted to sequentially deposit the suspension liquids D, E and F on a carbon / carbon composite material sample with a SiC internal coating, and finally, drying is carried out. The method has the advantages of short preparation period, simplicity in technological preparation, convenience in operation, easily-obtained raw materials and low preparation cost.

Description

technical field [0001] The invention relates to a method for preparing a composite gradient outer coating of a carbon / carbon composite material, in particular to a carbon / carbon composite material SiC-MoSi 2 -C-AlPO 4 A method for preparing a composite gradient 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 compo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B41/89
Inventor 曹丽云郝巍黄剑锋费杰马凤兰殷立雄王开通杜鸣菲
Owner XINING GONGJIN NEW MATERIAL TECHNOLOGY CO LTD
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