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Nano hafnium carbide ceramic organic precursor and preparation method thereof

A technology of organic precursor and hafnium carbide, which is applied in the field of nano-hafnium carbide ceramic organic precursor and its preparation, can solve the problems of complex reaction process route, poor solubility of precursor, long preparation cycle, etc., and achieve cheap and easy raw materials , short preparation cycle and low production cost

Active Publication Date: 2018-05-29
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 existing methods for preparing hafnium carbide ceramic organic precursors have the following defects: the reaction process route is complicated, the preparation cycle is long; the raw materials are expensive and the cost is high; the precursor cracking product contains HfO 2 ; The prepared precursor has poor solubility in organic solvents, etc.

Method used

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  • Nano hafnium carbide ceramic organic precursor and preparation method thereof
  • Nano hafnium carbide ceramic organic precursor and preparation method thereof

Examples

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Embodiment 1

[0024] A preparation method of nano hafnium carbide ceramic organic precursor, the steps of the preparation method are:

[0025] Step 1. Use a three-necked flask as the main reaction equipment for preparing the organic precursor of hafnium carbide ceramics. One of the ports is used to feed the protective gas argon, the other port is equipped with a constant pressure funnel for adding raw materials, and the third port is connected to reflux After the device is connected to the tail gas treatment device; first vacuumize the three-necked flask to 0.06MPa ~ 0.11MPa, and then pass in argon gas, then repeat vacuuming to 0.06MPa ~ 0.11MPa and pass in argon gas for 2 to 3 times; The argon gas is continuously fed inside as a protective atmosphere;

[0026] Step 2. Under a protective atmosphere, add 1 part of hafnium source to 2.5 to 2.6 parts of acetylacetone, and stir the resulting mixture at room temperature at a rate of 300r / min to 500r / min for 3.5h to 4h, then add 10 to 11 parts o...

Embodiment 2

[0029] A nano hafnium carbide ceramic organic precursor and a preparation method thereof, the steps of the preparation method are:

[0030] Step 1. Use the Schlenk device as the equipment for preparing the organic precursor of hafnium carbide ceramics. First, the Schlenk device is evacuated to 0.07MPa-0.10MPa, and argon is introduced, and then the vacuum is repeatedly evacuated to 0.07MPa-0.10MPa and argon is introduced. 2 to 3 times; then continue to feed argon into the Schlenk apparatus as a protective atmosphere.

[0031]Step 2. Under the argon atmosphere, add 1 part of hafnium source to 2-2.1 parts of acetylacetone, and stir the resulting mixture at room temperature at a rate of 600r / min-900r / min 3h to 3.5h, then add 9 to 10 parts of alcohol, react at 85°C to 90°C for 2.2h to 2.3h, add 3 to 3.1 parts of carbon source, and react at reflux temperature for 2.4h to After 2.5h, an orange transparent solution was obtained. The solvent is removed by a rotary evaporator, and the...

Embodiment 3

[0034] An organic precursor of zirconium carbide ceramics and a preparation method thereof. The steps of the preparation method are:

[0035] Step 1. Use the Schlenk device as the equipment for preparing the organic precursor of hafnium carbide ceramics. First, the Schlenk device is evacuated to 0.083MPa-0.086MPa, and argon gas is introduced, and then the vacuum is repeatedly evacuated to 0.083MPa-0.086MPa and argon gas is introduced. 3 to 4 times; then continue to feed argon into the Schlenk apparatus as a protective atmosphere.

[0036] Step 2. Under the argon atmosphere, add 1 part of hafnium source to 2.1-2.2 parts of acetylacetone, and stir the resulting mixture at room temperature at a rate of 900r / min-1200r / min 2.5h to 3h, then add 7 to 8 parts of alcohol, react at 75°C to 80°C for 2.4h to 2.5h, add 2.5 to 2.6 parts of carbon source. The reaction was carried out at reflux temperature for 2.9h-3h, and an orange transparent solution was obtained. After the solvent is r...

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Abstract

The invention relates to a preparation method of a nano hafnium carbide ceramic organic precursor. The method successively includes the steps of: 1. designing and adopting a device with protective atmosphere as the equipment for preparation of the hafnium carbide ceramic organic precursor; 2. in the protective atmosphere, adding 1 part of a hafnium source into 2-4 parts of acetylacetone, stirringthe obtained mixture at a rate of 300r / min-2500r / min for 0.5h-4h under room temperature, then adding 5-15 parts of alcohol, carrying out reaction at 40DEG C-100DEG C for 1h-4h, adding 1-4 parts of a carbon source, carrying out reaction at a reflux temperature for 2h-4h to obtain an orange transparent solution; and removing the solvent, then performing drying in a vacuum drying box at 80DEG C-150DEG C for 3h-5h to obtain a brown solid, i.e. a hafnium carbide precursor. The method provided by the invention has the characteristics of cheap and easily available raw materials, simple process, shortpreparation cycle, low cost, and good solubility of the prepared nano hafnium carbide ceramic organic precursor in an organic solvent.

Description

technical field [0001] The invention belongs to the field of hafnium carbide ceramic materials. In particular, it relates to a nanometer hafnium carbide ceramic organic precursor and a preparation method thereof. Background technique [0002] Hafnium carbide ceramics have excellent properties such as high melting point, high strength, chemical corrosion resistance, and good high temperature stability. They are used in many fields such as thin film materials, high temperature structural materials, superhard tool materials, microelectronic materials and nuclear energy storage materials It has broad application prospects and is also an ideal high-temperature protection material. After the C / C composite material is modified by hafnium carbide ceramics, its anti-oxidation and anti-ablation properties are significantly improved. [0003] The traditional preparation methods of hafnium carbide ceramics mainly include direct synthesis, carbothermal reduction, self-propagating high-t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/56C07C45/77C07C49/14
CPCC04B35/5622C04B2235/48C07C45/77C07C49/14
Inventor 李轩科张程董志军袁观明丛野张江
Owner WUHAN UNIV OF SCI & TECH
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