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Preparation method of tantalum carbide ceramic precursor

A ceramic precursor, tantalum carbide technology, applied in the field of tantalum carbide ceramics, can solve the problems of carbon fiber damage, affecting the mechanical properties and high temperature resistance of composite materials, and achieve the effect of reducing raw material costs, low cost and simple process

Active Publication Date: 2019-11-22
NAT UNIV OF DEFENSE TECH
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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing a precursor of tantalum carbide ceramics. The present invention mainly solves the problem that when TaC is prepared by the conversion method of the existing precursor, the high-temperature carbothermal reduction reaction will cause a large amount of fine damage to the surface of the carbon fiber; the raw materials used for preparing the precursor Only physical level mixing is carried out between them, and no chemical reaction occurs, which affects the technical problems of various mechanical properties and high temperature resistance properties of the obtained composite materials.

Method used

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  • Preparation method of tantalum carbide ceramic precursor
  • Preparation method of tantalum carbide ceramic precursor
  • Preparation method of tantalum carbide ceramic precursor

Examples

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Effect test

Embodiment 1

[0031] In a high-purity argon environment, 17.925g (0.05mol) of tantalum source compound (TaCl 5 ) into the three-necked flask. Add 200mL triethylamine and 5.0g (0.05mol) N,N′-dimethylethylenediamide lithium (LiN(CH 3 )CH 2 CH 2 N(CH 3 ) Li), and fully stirred, reacted at room temperature for 2h. Add dropwise 3.45g (0.15mol) lithium amide (NH 2 Li), continue to stir, react 2h. After cooling, the precipitated LiCl was removed by filtration. The filtrate was heated to 320° C. in a high-purity nitrogen / argon environment, kept for 1 hour, and cooled to obtain a black, brittle tantalum carbide precursor with a synthesis yield of 52.6%.

[0032] Result analysis: measure the thermogravimetric curve, infrared spectrogram, X-ray diffraction spectrogram of embodiment 1 gained product respectively by existing method, gained result is listed in Figure 1~3 middle.

[0033] figure 1 It is the infrared spectrogram (FT IR) of the tantalum carbide precursor obtained in Example 1. A...

Embodiment 2

[0037] In a high-purity argon environment, 14.5g (0.025mol) of tantalum source compound (TaBr 5 ) into the three-necked flask. 200mL triethylamine and 3.845g (0.025mol) N,N'-dimethyl 1,4-cyclohexanediamide lithium (C 8 h 16 N 2 Li 2 ), and fully stirred, reacted at room temperature for 3h. Add dropwise 1.725g (0.075mol) lithium amide (NH 2 Li), continued to stir, and reacted for 1h. After cooling, the LiBr precipitate was removed by filtration. The filtrate was heated to 300° C. in a high-purity nitrogen / argon environment, kept for 1 hour, and cooled to obtain a black, brittle tantalum carbide precursor with a synthesis yield of 50.2%. The ceramic yield of the obtained precursor at 1000 °C is about 69.4%.

Embodiment 3

[0039] The difference from Example 1 is: stirring for 1 hour, adding lithium amide dropwise, continuing to stir, reacting for 4 hours, raising the temperature of the reaction system to 350°C, and keeping it warm for 0.5 hours;

[0040] The tantalum source compound, lithium polyamide compound and lithium amide are mixed according to the molar ratio of Ta-X bond to lithium polyamide compound being 1:1, and the molar ratio of Ta-X bond to lithium amidide being 1:3. The tantalum source compound is TaI 5 . The synthesis yield was 46.3%. The ceramic yield of the obtained precursor at 1000 °C is about 67.8%.

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Abstract

The invention provides a preparation method of a tantalum carbide ceramic precursor. The method includes the steps of performing pre-reactions to a tantalum source compound TaX5 (X is Cl, Br or I) successively with an amido lithium compound and aminated lithium, each having two N-Li bonds, at room temperature; and heating the system to perform a reaction to obtain the tantalum carbide ceramic precursor. The preparation method is low in cost and has simple processes. The tantalum carbide ceramic precursor is suitable for preparing a tantalum carbide ceramic material.

Description

technical field [0001] The invention relates to the technical field of tantalum carbide ceramics, in particular to a method for preparing a tantalum carbide ceramic precursor. Background technique [0002] The rapid development of aerospace technology has put forward an urgent demand for ultra-high temperature materials. Ultra-high temperature material refers to a special material that can maintain stable physical and chemical properties in a high-temperature (above 2000°C) environment and a high-temperature reaction atmosphere. As a member of ultra-high temperature materials, tantalum carbide (TaC) ceramics has a very high melting point (3880 ° C), which is higher than most metal carbides, and has high mechanical strength, high hardness, excellent thermodynamics and chemical stability. With excellent high temperature resistance, oxidation resistance and ablation resistance, it is an ultra-high temperature ceramic material with broad application prospects in the field of ul...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/56C04B35/622
CPCC04B35/5607C04B35/622
Inventor 简科王军王浩邵长伟王小宙苟燕子谢征芳
Owner NAT UNIV OF DEFENSE TECH
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