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Preparation and Application of Hafnium Carbide Precursor Impregnation Solution

A technology of precursor and impregnation solution, which is applied in the field of preparation of hafnium carbide modified C/C composite materials, can solve the problems of low bonding strength, broaden the scope of application and improve the effect of high temperature ablation resistance

Inactive Publication Date: 2018-01-16
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Hafnium carbide modified C / C composites prepared by CVD process, although the HfC coating has better uniformity and structure is easy to control, but because the combination between the substrate and the coating belongs to physical adsorption, the bonding strength between the two is low

Method used

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  • Preparation and Application of Hafnium Carbide Precursor Impregnation Solution
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  • Preparation and Application of Hafnium Carbide Precursor Impregnation Solution

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Under the protection of nitrogen atmosphere, add 32 g (0.1 mol) hafnium tetrachloride to a 250 ml three-necked flask with mechanical stirring, add 100 ml xylene as a solvent, cool the reaction system below 0 ℃, and then slowly drop 24 ml (0.4mol) of absolute ethanol, reacted for 3 hours under low temperature protection, transferred the reaction solution to a 250 ml beaker, added 60 ml of distilled water, stirred at room temperature for 1 hour, and extracted the organic phase in the reaction solution with dichloromethane. Add 20 g of anhydrous magnesium sulfate to the enriched organic phase, let it stand for 6 hours, filter, and distill off xylene at 90 °C to obtain 22.1 g of light yellow liquid.

Embodiment 2

[0024] Under the protection of nitrogen atmosphere, add 32 g (0.1 mol) hafnium tetrachloride to a 250 ml three-necked flask with mechanical stirring, add 100 ml xylene as a reaction solvent, cool the reaction system below 0 °C, and then slowly drop Add 31 ml (0.4 mol) of propanol, react for 3 hours under low temperature protection, transfer the reaction solution to a 400 ml beaker, add 60 ml of distilled water, stir at room temperature for 1 hour, use dichloromethane to extract the organic phase in the reaction solution, Add 20 g of anhydrous magnesium sulfate to the enriched organic phase, let it stand for 6 hours, filter, and distill off xylene at 90 °C to obtain 24.8 g of light yellow liquid.

Embodiment 3

[0026] Under the protection of nitrogen atmosphere, add 32 g (0.1 mol) hafnium tetrachloride to a 250 ml three-necked flask with mechanical stirring, add 100 ml xylene as a reaction solvent, cool the reaction system below 0 °C, and then slowly drop Add 43 ml (0.4 mol) cyclohexanol, react for 3 hours under low temperature protection, transfer the reaction solution to a 400 ml beaker, add 60 ml of distilled water, stir at room temperature for 1 hour, use dichloromethane to extract the organic phase in the reaction solution , add 20 g of anhydrous magnesium sulfate to the enriched organic phase, let stand for 6 hours, filter, and distill off xylene at 90 °C to obtain 30.2 g of light yellow liquid.

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Abstract

The invention relates to a preparation method and an application of a hafnium carbide precursor impregnation liquid. The preparation method is characterized in that hafnium tetrachloride and ROH undergo a nucleophilic substitution reaction under the protection of nitrogen, and R is an ethyl group, a propyl group, a cyclohexyl group or a benzyl group; and the preparation method comprises the following steps: adding hafnium tetrachloride to toluene or xylene, cooling a reaction system to 0DEG C or below, adding the ROH to the reaction system, reacting, and rising the temperature of the reaction system to room temperature; carrying out pumping filtration on a precipitate in the reaction system to obtain a solution A, removing impurities in the solution A to obtain a solution B, and extracting an organic phase in the solution B to obtain a solution C; and adding a drying agent to the solution C, carrying out pumping filtration, and carrying out reduced pressure distillation to obtain the hafnium carbide precursor impregnation liquid. Uniform introduction of a HfC ceramic phase prepared in the invention to a carbon / carbon composite material matrix effectively solves the problem of application of the carbon / carbon composite material at a high temperature, and introduction of the hafnium carbide ceramic phase greatly improves the high temperature ablation resistance of the C / C composite material and widens the application range of the C / C composite material.

Description

technical field [0001] The invention relates to a preparation method of a hafnium carbide precursor impregnation solution. The invention also relates to the preparation process of the hafnium carbide modified C / C composite material by using the precursor impregnation and cracking method. technical background [0002] Hafnium carbide (HfC) has excellent physical and chemical properties, such as high hardness, high melting point (3890 ° C), solid phase stability, thermodynamic stability and good thermal shock resistance, and also has high strength and wear resistance at a certain temperature sex hot [0003] Conductivity and electrical conductivity, so it is one of the ultra-high temperature materials that people are currently interested in. [0004] Carbon-carbon composites have low density, high thermal conductivity, excellent thermal shock resistance and good ablation resistance, and are ideal materials for preparing high-temperature thermal structural components. They ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/56C04B35/622C04B41/82
Inventor 苏哲安黄启忠薛亮黄东陈蕾
Owner CENT SOUTH UNIV
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