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Preparation method and application of hafnium carbide precursor impregnation liquid

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 problem of low bonding strength, achieve the effect of broadening the application range and improving high temperature ablation resistance

Inactive Publication Date: 2016-05-25
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 method and application of hafnium carbide precursor impregnation liquid
  • Preparation method and application of hafnium carbide precursor impregnation liquid
  • Preparation method and application of hafnium carbide precursor impregnation liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Under the protection of nitrogen atmosphere, add 32g (0.1mol) of hafnium tetrachloride in a 250ml three-necked flask with mechanical stirring, add 100ml of xylene as the solvent, cool the reaction system to below 0℃, and then slowly add 24ml (0.4 mol) Dehydrated ethanol, react for 3 hours under low temperature protection, transfer the reaction solution to a 250ml beaker, add 60ml of distilled water, stir at room temperature for 1 hour, extract the organic phase in the reaction solution with dichloromethane to enrich the organic phase 20g of anhydrous magnesium sulfate was added to the mixture, allowed to stand for 6 hours, filtered, and xylene was distilled out at 90°C to obtain 22.1g of light yellow liquid.

Embodiment 2

[0024] Under the protection of nitrogen atmosphere, 32g (0.1mol) hafnium tetrachloride was added to a 250ml three-necked flask with mechanical stirring, 100ml xylene was added as the reaction solvent, the reaction system was cooled to below 0°C, and then 31ml ( 0.4mol) Propanol, react for 3 hours under low temperature protection, transfer the reaction solution to a 400ml beaker, add 60ml of distilled water, stir at room temperature for 1 hour, extract the organic phase in the reaction solution with dichloromethane to enrich the organic phase Add 20 g of anhydrous magnesium sulfate to the mixture, 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, 32g (0.1mol) hafnium tetrachloride was added to a 250ml three-necked flask with mechanical stirring, 100ml xylene was added as the reaction solvent, the reaction system was cooled to below 0℃, and then 43ml ( 0.4mol) Cyclohexanol, react for 3 hours under low temperature protection, transfer the reaction solution to a 400ml beaker, add 60ml of distilled water, stir at room temperature for 1 hour, extract the organic phase in the reaction solution with dichloromethane, Add 20 g of anhydrous magnesium sulfate to the phase, let it 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 immersion liquid. The invention also relates to a preparation process for preparing the hafnium carbide modified C / C composite material by using the precursor impregnation cracking method. technical background [0002] Hafnium Carbide (HfC) has excellent physical and chemical properties, such as high hardness, high melting point (3890℃), solid phase stability, thermodynamic stability and good thermal shock resistance. It also has high strength and wear resistance at a certain temperature Sex, heat [0003] Conductivity and conductivity, so it is one of the ultra-high temperature materials of interest at present. [0004] Carbon-carbon composite material has low density, high thermal conductivity, excellent thermal shock resistance and good ablation resistance. It is an ideal material for preparing high-temperature thermal structural parts. It has been widely used in aviation in recen...

Claims

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Application Information

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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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