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A kind of zirconium carbide ceramic organic precursor and preparation method thereof

A technology of organic precursor and zirconium carbide, which is applied in the field of zirconium carbide ceramic organic precursor and its preparation, can solve the problems of expensive raw materials, complicated process route, long preparation period, etc., and achieves simple and easy to obtain production costs and raw materials that are simple and easy to obtain. , the effect of short preparation cycle

Inactive Publication Date: 2016-07-27
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, the current methods for preparing zirconium carbide ceramic organic precursors have the following defects: complex process route; long preparation cycle; expensive raw materials; high cost; poor solubility of the prepared precursor in organic solvents, etc.

Method used

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  • A kind of zirconium carbide ceramic organic precursor and preparation method thereof
  • A kind of zirconium carbide ceramic organic precursor and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0020] An organic precursor of zirconium carbide ceramics and a preparation method thereof. The steps of the preparation method are:

[0021] Step 1. Use the Schlenk device as the equipment for preparing the organic precursor of zirconium carbide ceramics. First, the Schlenk device is evacuated to a vacuum degree of 0.08~0.083MPa, and Ar gas is introduced, and then repeated vacuuming until the vacuum degree is 0.08~0.083MPa and Infuse Ar gas 2 to 3 times; then continuously infuse Ar gas into the Schlenk apparatus as a protective atmosphere.

[0022] Step 2, under the condition of continuously feeding Ar gas, the stirring rate is 600 ~ 900r / min and room temperature, the ZrCl 4 Add the powder and 6-7 parts of toluene to the container, then place the container on a magnetic stirrer and stir until the ZrCl 4 Disperse the powder in toluene; add 4 parts of amine dropwise to the container, stir for 0.8~1.2h, and finally add 1~1.1 parts of carbon source into the container, stir for ...

Embodiment 2

[0025] An organic precursor of zirconium carbide ceramics and a preparation method thereof. The steps of the preparation method are:

[0026] Step 1. Use the Schlenk device as the equipment for preparing the organic precursor of zirconium carbide ceramics. First, the Schlenk device is evacuated to a vacuum degree of 0.083~0.086MPa, and Ar gas is introduced, and then repeated vacuuming until the vacuum degree is 0.083~0.086MPa and Infuse Ar gas 3 to 4 times; then continuously infuse Ar gas into the Schlenk apparatus as a protective atmosphere.

[0027] Step 2, under the condition of continuously feeding Ar gas, the stirring rate is 900 ~ 1200r / min and room temperature, the ZrCl 4 Add the powder and 7-8 parts of toluene to the container, then place the container on a magnetic stirrer and stir until the ZrCl 4 Disperse the powder in toluene; add 4 parts of amine dropwise to the container, stir for 1.2~1.6h, finally add 1.1~1.2 parts of carbon source into the container, stir for...

Embodiment 3

[0030] An organic precursor of zirconium carbide ceramics and a preparation method thereof. The steps of the preparation method are:

[0031] Step 1. Use the Schlenk device as the equipment for preparing the organic precursor of zirconium carbide ceramics. First, the Schlenk device is evacuated to a vacuum degree of 0.086~0.089MPa, and Ar gas is introduced, and then repeated vacuuming until the vacuum degree is 0.086~0.089MPa and Infuse Ar gas 3 to 4 times; then continuously infuse Ar gas into the Schlenk apparatus as a protective atmosphere.

[0032] Step 2, under the condition of continuously feeding Ar gas, the stirring speed is 1200 ~ 1500r / min and room temperature, the ZrCl 4 Add the powder and 8-9 parts of toluene to the container, then place the container on a magnetic stirrer and stir until the ZrCl 4 Disperse the powder in toluene; add 4 parts of amine dropwise to the container, stir for 1.6~2h, and finally add 1.2~1.3 parts of carbon source into the container, stir...

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Abstract

The invention relates to a zirconium carbide ceramic organic precursor and a preparation method thereof. According to the technical scheme, the preparation method comprises the following steps: vacuumizing an Schlenk device until the vacuum degree is 0.08-0.098MPa, introducing Ar gas, and then repeating above operations for 2-4 times; continuously introducing Ar gas as protective atmosphere into the Schlenk device; under the conditions of Ar gas atmosphere, a stirring rate of 600-2400r / min and room temperature, adding 1 part of the amount of substance of ZrCl4 powder and 6-12 parts of the amount of substance of toluene into a container, and placing the container on a magnetic stirrer for stirring until ZrCl4 powder is dispersed in toluene; dropwise adding 4 parts of amount of substance of amine into the container, stirring for 0.8-3.2 hours and finally adding 1-1.6 parts of the amount of substance of a carbon source into the container and stirring for 0.8-3.2 hours to obtain the zirconium carbide ceramic organic precursor. The preparation method has the characteristics of simple and easily available raw materials, simple process, short preparation period and low cost and the zirconium carbide ceramic organic precursor prepared by the preparation method has good solubility in an organic solvent.

Description

technical field [0001] The invention belongs to the field of zirconium carbide ceramic materials. In particular, it relates to a zirconium carbide ceramic organic precursor and a preparation method thereof. Background technique [0002] Zirconium carbide (ZrC) ceramics is a typical transition metal carbide, with high melting point, high strength, chemical corrosion resistance, good high temperature stability and other excellent characteristics. It is used in thin film materials, high temperature structural materials, superhard tool materials, Many fields such as microelectronic materials and nuclear energy storage materials have broad application prospects, and are also ideal high-temperature protection materials, which are used in C / C composite materials for anti-oxidation, anti-ablation and other fields. [0003] The traditional methods of preparing zirconium carbide ceramics mainly include: direct synthesis method, carbothermal reduction method, self-propagating high tem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/56C04B35/622
Inventor 李轩科张贤董志军袁观明李艳军张江
Owner WUHAN UNIV OF SCI & TECH