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Preparation method for ultra-high-temperature ceramic modified C/C composite material

A technology for ultra-high-temperature ceramics and composite materials, which is applied in the field of preparation of ultra-high-temperature ceramics modified C/C composite materials, and can solve problems such as the decline in mechanical properties of composite materials, long production cycles of process methods, and long preparation cycles of composite materials. Favorable anti-ablation performance, shortened preparation cycle, significant economic and social benefits

Active Publication Date: 2015-11-04
无锡博智复合材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation cycle of the composite material is long, and the complete densification of the material requires at least about 10 impregnation-pyrolysis cycles, and a certain amount of pores will inevitably remain in the final composite material.
In addition, the gaseous by-products produced in the cracking process have certain damage to the fiber, and with the shrinkage of the matrix, there is residual stress inside the material.
Document 2 "Li Z, Li H, Zhang S, et al.Effect of reaction melt infiltration temperature on the ablation properties of 2D C / C-SiC-ZrC composites[J].Corrosion Science,2012,58:12-19. "The C / C-SiC-ZrC composite material was prepared by using the isothermal chemical vapor deposition process combined with the reaction infiltration method, and the reaction infiltration temperature has a significant impact on the ablation performance of the composite material, but the production cycle of this process is long. Reactive infiltration has a certain damage to the fiber, which reduces the mechanical properties of the composite material

Method used

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  • Preparation method for ultra-high-temperature ceramic modified C/C composite material
  • Preparation method for ultra-high-temperature ceramic modified C/C composite material
  • Preparation method for ultra-high-temperature ceramic modified C/C composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step 1: Set the density to 0.45g / cm 3 The 2D carbon felt is processed into a disc with a size of Φ80mm×10mm, and it is ultrasonically cleaned twice in anhydrous ethanol solution for 15 minutes each time, and dried at 80°C;

[0028] Weigh 500g of organic zirconium precursor and 12L of xylene liquid, dissolve the organic zirconium precursor in xylene, and prepare the precursor solution;

[0029] Step 2: Using chemical liquid phase vaporization deposition technology, place the processed 2D carbon felt in the liquid phase deposition furnace, and pour the prepared precursor solution into the furnace, and then increase the temperature at a rate of 20°C / min Raise the temperature from room temperature to 1200°C, keep it warm for 16 hours, and then gradually decrease the temperature from 1200°C to 600°C at a cooling rate of 20°C / min, turn off the power, cool it naturally, and finally take out the 2D carbon felt;

[0030] Step 3: Place the 2D carbon felt deposited in step 2 in an isothe...

Embodiment 2

[0033] Step 1: Set the density to 0.5g / cm 3 The 2D carbon felt is processed into a disc with a size of Φ80mm×15mm, ultrasonically cleaned twice in anhydrous ethanol solution, 15min each time, and dried at 80℃; weigh 1kg organic hafnium precursor and 10L xylene liquid , And dissolve the organic zirconium precursor in xylene to prepare the precursor solution;

[0034] Step 2: Using chemical liquid phase vaporization deposition technology, place the processed 2D carbon felt in the liquid phase deposition furnace, and pour the prepared precursor solution into the furnace, and then increase the temperature at a rate of 20°C / min Raise the temperature from room temperature to 1000°C, keep it warm for 24 hours, and then gradually decrease the temperature from 1000°C to 600°C at a cooling rate of 20°C / min, turn off the power, cool naturally, and finally take out the 2D carbon felt;

[0035] Step 3: Place the 2D carbon felt treated in step 2 in an isothermal furnace for heat treatment: incre...

Embodiment 3

[0038] Step 1: Set the density to 0.6g / cm 3 The 2D carbon felt is processed into a disc with a size of Φ80mm×20mm, ultrasonically cleaned twice in anhydrous ethanol solution, 15min each time, and dried at 80℃; weigh 2kg organic tantalum precursor and 10L xylene liquid , And dissolve the organic tantalum precursor in xylene to prepare the precursor solution;

[0039] Step 2: Using chemical liquid phase vaporization deposition technology, place the processed 2D carbon felt in a liquid phase deposition furnace, and pour the prepared precursor solution into the furnace, and then increase the temperature at a rate of 20°C / min Raise the temperature from room temperature to 1100°C, keep it for 36 hours, and then gradually decrease the temperature from 1100°C to 600°C at a cooling rate of 20°C / min. Turn off the power supply, cool it naturally, and finally take out the sample;

[0040] Step 3: Place the sample in step 2 in an isothermal furnace for heat treatment: increase the temperature f...

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Abstract

The invention relates to a preparation method for an ultra-high-temperature ceramic modified C / C composite material. The preparation method comprises: carrying out a reaction on an ultra-high-temperature ceramic precursor solution at a high temperature by adopting a chemical liquid phase vaporized deposition process technology to generate a ceramic and pyrolytic carbon; depositing the ceramic and pyrolytic carbon; in a carbon fiber preform; and finally carrying out thermal treatment to obtain the ultra-high-temperature ceramic modified C / C composite material. The innovation of the preparation method provided by the invention is that the ultra-high-temperature ceramic modified C / C composite material is prepared by adopting the chemical liquid phase vaporized deposition process, so that the problems that a conventional process method is long in production period, has a certain damage to fiber and the like are overcome, and the ultra-high-temperature ceramic modified C / C composite material which is uniformly distributed is prepared within a short time. In the method, the component proportion, the chemical liquid phase vaporized deposition process parameters and the thermal treatment process have a great influence on the experimental result. By adjusting the experimental parameters, the ultra-high-temperature ceramic which is uniformly distributed can be obtained in the C / C composite material, so that the anti-oxidizing and ablation-resisting performances of the C / C composite material are favorably enhanced.

Description

Technical field [0001] The invention belongs to the technical field of matrix modified C / C composite materials, and specifically relates to a preparation method of ultra-high temperature ceramic modified C / C composite materials. Background technique [0002] Carbon / carbon (C / C) composite materials have many excellent properties and have been successfully used in military fields: such as aircraft wing fronts, rocket engine nozzles, throat liners, missile nose cones, aviation brakes, etc. However, with the development of aerospace technology, C / C composite materials are required to face a more severe environment. However, C / C composite materials can no longer meet their thermal protection requirements due to their easy oxidation and insufficient ablation resistance. Therefore, the introduction of ultra-high temperature ceramic components into C / C composites is considered to be an effective way to improve their oxidation resistance and ablation resistance. [0003] The traditional p...

Claims

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Application Information

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IPC IPC(8): C04B35/83C04B35/622
Inventor 卢锦花何秦川李贺军付前刚李伟宋强
Owner 无锡博智复合材料有限公司
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