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

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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 con...

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

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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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