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Preparation method of C-AlPO4-mullite/glass layer gradient composite antioxidation coating

An anti-oxidation coating, c-alpo4- technology, which is applied in the field of preparing carbon/carbon composite material composite outer coating, can solve the problems of not being able to prepare at one time, the surface of the outer coating is easy to crack, and the thickness of the coating is insufficient. The effect of convenient operation, high bonding strength and low preparation cost

Active Publication Date: 2013-08-28
吴文婕
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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.], while cathode rotary hydroelectrophoresis arc discharge deposition combined with coating method to prepare C-AlPO 4 -The method of mullite / glass layer gradient composite anti-oxidation coating has not been reported yet

Method used

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  • Preparation method of C-AlPO4-mullite/glass layer gradient composite antioxidation coating
  • Preparation method of C-AlPO4-mullite/glass layer gradient composite antioxidation coating

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Experimental program
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Embodiment 1

[0028] 1) Take commercially available analytically pure SiO 2 Powder, analytical pure B 2 o 3 Powder, analytical pure Al 2 o 3 Powder, analytically pure MgO powder, by SiO 2 :B 2 o 3 :Al 2 o 3 : MgO=5:3:2:1 mass ratio Mix the powder evenly, use wet ball milling and dry at a constant temperature of 60°C to get the mixed powder A;

[0029] 2) Put the mixed powder A into the crucible, then put the crucible into the silicon-molybdenum rod electric furnace, control the heating rate to 10°C / min, raise the furnace temperature from room temperature to 1300°C and keep it for 5h, then take out the crucible, Quickly put into cold water for rapid cooling, and grind the gained glass block into glass powder B;

[0030] 3) The 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 , take 0.5g of nano-mullite powder and 1g of C-AlPO 4 Add the powder into the Erlenmeyer flask, then pour 40...

Embodiment 2

[0036] 1) Take commercially available analytically pure SiO 2 Powder, analytical pure B 2 o 3 Powder, analytical pure Al 2 o 3 Powder, analytically pure MgO powder, by SiO 2 :B 2 o 3 :Al 2 o 3 : MgO=7:6:3:3 mass ratio Mix the powder evenly, use wet ball milling and dry at a constant temperature of 60°C to get the mixed powder A;

[0037] 2) Put the mixed powder A into the crucible, then put the crucible into the silicon-molybdenum rod electric furnace, control the heating rate to 20°C / min, raise the furnace temperature from room temperature to 1400°C for 4 hours, then take out the crucible, Quickly put into cold water for rapid cooling, and grind the gained glass block into glass powder B;

[0038] 3) The 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 , take 1g of nano-mullite powder and 3g of C-AlPO 4 Add the powder into the Erlenmeyer flask, then pour 200ml of is...

Embodiment 3

[0044] 1) Take commercially available analytically pure SiO 2 Powder, analytical pure B 2 o 3 Powder, analytical pure Al 2 o 3 Powder, analytically pure MgO powder, by SiO 2 :B 2 o 3 :Al 2 o 3 : MgO=9:5:5:2 mass ratio Mix the powder evenly, use wet ball milling and dry at a constant temperature of 60°C to get the mixed powder A;

[0045] 2) Put the mixed powder A into the crucible, then put the crucible into the silicon-molybdenum rod electric furnace, control the heating rate to 40°C / min, raise the furnace temperature from room temperature to 1500°C for 3 hours, then take out the crucible, Quickly put into cold water for rapid cooling, and grind the gained glass block into glass powder B;

[0046] 3) The 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 , take 2g of nano-mullite powder and 4g of C-AlPO 4 Add the powder into the conical flask, then pour 800ml of isopr...

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Abstract

The invention relates to a preparation method of a C-AlPO4-mullite / glass layer gradient composite antioxidation coating, which comprises the following steps: mixing SiO2, B2O3, Al2O3 and MgO to obtain powder A; calcining the powder A, and grinding to obtain glass powder B; adding the mullite powder and the C-AlPO4 powder into isopropanol to obtain a suspension C; adding a simple substance iodine into the suspension C to obtain a solution D; pouring the solution D into a device which uses a graphite electrode as the anode and a conductive base as the cathode, clamping a C / C composite material sample with an SiC internal coating onto the cathode in the device, and carrying out electrophoretic arc discharge deposition to obtain a sample E; adding the glass powder B into ethanol to obtain a slurry, repeatedly brushing the slurry on the surface of the sample E, and drying to obtain a sample F; and putting the sample F in a crucible, putting the crucible in a vertical vacuum furnace, heating to react while introducing argon as a protective atmosphere, and opening the furnace and the crucible to obtain the C-AlPO4-mullite / glass layer gradient composite antioxidation coating. The composite coating prepared by the method provided by the invention can protect a C / C composite material at 1500 DEG C in static air for 700 hours, and the oxidative weight loss is less than 0.8%.

Description

Technical field: [0001] The invention relates to a method for preparing a composite outer coating of carbon / carbon composite materials, in particular to a cathode rotary hydrothermal electrophoresis arc discharge deposition combined with a coating method to prepare a uniform surface without micro-cracks, and a uniform thickness without penetrating holes and C-AlPO 4 -The preparation method of mullite / glass layer gradient composite anti-oxidation 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(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 吴文婕