Preparation method of carbon/carbon material C-AlPO4-mullite-MoSi2 composite outer coating layer

A technology of c-alpo4- and mullite, which is applied in the field of preparing carbon/carbon composite composite outer coatings, can solve the problems of insufficient coating thickness, high requirements, imperfections, etc., and achieve low preparation costs and easy raw materials Easy to operate

Active Publication Date: 2012-09-19
XINING GONGJIN NEW MATERIAL TECHNOLOGY CO LTD
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  • Abstract
  • Description
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  • 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 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. The prepared high-temperature oxidation resistance Further improvement is needed [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.], while using microwave-ultrasonic cathode rotating water Preparation of C-AlPO by Thermoelectrophoretic Arc Discharge Deposition 4 - Mullite - MoSi 2 The method of composite outer coating has not been reported yet

Method used

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  • Preparation method of carbon/carbon material C-AlPO4-mullite-MoSi2 composite outer coating layer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) Commercially available aluminum phosphate powder was calcined at 1300°C and wet ball milled to prepare C-AlPO with an average particle size of 5 μm 4 , and then 0.5g of nano-mullite powder prepared by sol-gel-microwave hydrothermal method (200910218827.9), 1g of C-AlPO 4 The powder and 1g of molybdenum disilicide powder were added to the Erlenmeyer flask, wherein the molybdenum disilicide powder was commercially available molybdenum disilicide, and the average particle size was 10 μm by wet ball milling, and then 200ml of butanol with a purity of ≥99.8% was poured into Prepare the suspension A in the Erlenmeyer flask, then put the suspension A into a 1000W ultrasonic generator to vibrate for 30min, place it on a magnetic stirrer and stir for 15h;

[0026] 2) Add selenium with a purity ≥ 99.7% to the suspension A, so that the concentration of selenium is 1g / L, then put it into a 1000W ultrasonic generator and shake for 30min, take it out and stir it on a magnetic stir...

Embodiment 2

[0031] 1) Commercially available aluminum phosphate powder was calcined at 1300°C and wet ball milled to prepare C-AlPO with an average particle size of 5 μm 4 , and then 2g of nano-mullite powder prepared by the method of preparing nano-mullite powder by sol-gel-microwave hydrothermal method (200910218827.9), 0.5g of C-AlPO 4 The powder and 5g of molybdenum disilicide powder were added to the Erlenmeyer flask, wherein the molybdenum disilicide powder was commercially available molybdenum disilicide and the average particle size was 10 μm after wet ball milling, and then 400ml of butanol with a purity of ≥99.8% was poured into Prepare the suspension A in the Erlenmeyer flask, then put the suspension A into a 600W ultrasonic generator to vibrate for 80min, place it on a magnetic stirrer and stir for 20h;

[0032] 2) Add selenium with a purity ≥ 99.7% to the suspension A so that the concentration of selenium is 1g / L, then put it into a 500W ultrasonic generator and shake it for ...

Embodiment 3

[0036] 1) Commercially available aluminum phosphate powder was calcined at 1300°C and wet ball milled to prepare C-AlPO with an average particle size of 5 μm 4 , and then 5g of nano-mullite powder prepared by the method of preparing nano-mullite powder by sol-gel-microwave hydrothermal method (200910218827.9), 5g of C-AlPO 4 The powder and 8g of molybdenum disilicide powder were added to the Erlenmeyer flask, wherein the molybdenum disilicide powder was commercially available molybdenum disilicide, and the average particle size was 10 μm by wet ball milling, and then 500ml of butanol with a purity of ≥99.8% was poured into Prepare the suspension A in the Erlenmeyer flask, then place the suspension A in an 800W ultrasonic generator to vibrate for 50 minutes, and place it on a magnetic stirrer to stir for 18 hours;

[0037] 2) Add selenium with a purity ≥ 99.7% to the suspension A, so that the concentration of selenium is 1g / L, then put it into a 600W ultrasonic generator and sh...

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Abstract

The invention relates to a preparation method of a carbon / carbon material C-AlPO4-mullite-MoSi2 composite outer coating layer. The preparation method comprises the steps of: adding mullite powder, C-AlPO4 powder and MoSi2 powder into butanol to obtain suspension A, and adding elementary selenium into the suspension A to obtain solution B; and pouring the solution B into a device which uses a graphite electrode as an anode and a conductive substrate as a cathode for microwave ultrasonic cathode rotation hydrothermal electrophoretic arc-discharge deposition reaction, after the reaction is ended, naturally cooling to room temperature and drying to obtain the final product, i.e. a SiC-C / C test sample protected by the C-AlPO4-mullite-MoSi2 composite outer coating layer. The C-AlPO4-mullite-MoSi2 composite outer coating layer prepared by adopting the method has the advantages of uniform thickness and no surface crack. The preparation method of the C-AlPO4-mullite-MoSi2 composite outer coating layer has the advantages that the preparation period is short, the advantages of hydrothermal, electrophoretic, ultrasonic, microwave and arc-discharge processes are combined, the preparation steps are simple, the operation is convenient to conduct, the raw materials are easy to obtain and the preparation cost is lower.

Description

technical field [0001] The invention relates to a method for preparing a carbon / carbon composite material composite outer coating, in particular to a microwave-ultrasonic cathodic rotation hydrothermoelectrophoresis arc discharge deposition method to prepare a uniform surface without micro-cracks, and uniform thickness without penetrating holes and Crack-generated carbon / carbon material C-AlPO 4 - Mullite - MoSi 2 Preparation method of composite 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 o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B41/89
Inventor 曹丽云王开通黄剑锋刘亮亮辛宇卓艺乔
Owner XINING GONGJIN NEW MATERIAL TECHNOLOGY CO LTD
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