Method for preparing high-purity superfine zirconium boride powder by high-frequency plasma

A high-frequency plasma and plasma technology is applied in the field of preparing high-purity ultrafine zirconium boride powder, which can solve the problems of low activity, low cost of raw materials, and high process cost, and achieve good particle dispersibility, strong adaptability of raw materials, and high preparation technology. simple effect

Inactive Publication Date: 2012-05-23
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the above several preparation methods, the direct synthesis method has high powder purity, but the raw materials are expensive, the particle size is coarse, and the activity is low, which is not conducive to sintering and post-processing; the carbon or boron carbide reduction method in industrial production has low raw material cost and major disadvantages The reason is high energy consumption, long production cycle, and high process cost; the electrolysis method is also more suitable for industrial production, but it is easy to introduce impurities, the product purity is not high, and it is necessary to prevent zirconium boride from sintering in the production process; the process of self-propagating high-temperature synthesis method is simple , the reaction speed is fast, the time is very short, the energy consumption is very small, the activity of the synthetic powder is high, which is beneficial to sintering and post-processing, but the disadvantage is that the reaction speed is too fast, it is not easy to control, and the reaction is sometimes incomplete. There will be more impurities, and its reaction process, product structure and performance are not easy to accurately control

Method used

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  • Method for preparing high-purity superfine zirconium boride powder by high-frequency plasma
  • Method for preparing high-purity superfine zirconium boride powder by high-frequency plasma
  • Method for preparing high-purity superfine zirconium boride powder by high-frequency plasma

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Using boron trichloride and zirconium tetrachloride as raw materials, superfine zirconium boride powder is prepared by high-frequency plasma hydrogenation synthesis. The chemical reaction is shown in the following formula.

[0036] 2BCl 3 +ZrCl 4 +5H 2 →ZrB 2 +10HCl

[0037] With hydrogen as the carrier gas, gaseous boron trichloride and gaseous zirconium tetrachloride are added into the plasma reactor, wherein the ratio of boron trichloride and zirconium tetrachloride is added in a ratio of 2:1 according to the ratio of the amount of substances . During the experiment, the vacuum degree in the system was maintained at 200Pa. The tail gas is discharged after being absorbed by sodium hydroxide solution. The synthesized product is washed and dried to obtain superfine zirconium boride with a particle size of 30-60nm.

Embodiment 2

[0039] Using boric acid and zirconia as raw materials, superfine zirconium boride powder is prepared by high-frequency plasma hydrogenation synthesis. The chemical reaction is shown in the following formula.

[0040] 2H 3 BO 3 +ZrO 2 +5H 2 →ZrB 2 +8H 2 o

[0041] Using hydrogen as a carrier gas, boric acid and zirconia are added into the plasma reactor, wherein the proportion of boric acid and zirconia is added in a ratio of 2:1 according to the ratio of the amount of substances. During the experiment, a cooling gas was introduced at the tail flame of the plasma arc to maintain a vacuum of 1kPa in the system. The synthesized product is washed and dried to obtain superfine zirconium boride with a particle size of 10-40nm.

Embodiment 3

[0043] Using diboron trioxide and zirconium dioxide as raw materials, superfine zirconium boride powder is prepared by high-frequency plasma hydrogenation synthesis. The chemical reaction is shown in the following formula.

[0044] B 2 o 3 +ZrO 2 +5H 2 →ZrB 2 +5H 2 o

[0045] Firstly, boron trioxide and zirconium dioxide are ball-milled and mixed at a ratio of 1:1, and a mixed gas of hydrogen and argon is used as a carrier gas, and solid raw materials are added to the plasma arc region. The reactor wall is provided with an insulation device. The synthesized product is washed and dried to obtain superfine zirconium boride with a particle size of 50-100nm.

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Abstract

The invention relates to a method for preparing a high-purity superfine zirconium boride powder by high-frequency plasma. A superhigh temperature heat source provided by a high-frequency plasma arc provides enough high temperature and energy for synthetic reaction; the electrodeless heating characteristic of the high-frequency plasma guarantees the high-purity quality of the product; particles freely deposit and grow in an airflow to obtain superfine particles with good dispersibility; and a reactor is designed to achieve a purpose of regulating product particle size. The zirconium boride powder prepared by the method provided by the invention has the advantages of high purity, good dispersibility and nano-scale size and is suitable for preparing high-temperature ceramic and compound material. The high-frequency plasma technology has a short flow and is suitable for large-scale production.

Description

technical field [0001] The invention relates to a method for preparing high-purity ultrafine zirconium boride powder. More specifically, the invention relates to a method for preparing high-purity ultrafine zirconium boride powder by using a high-frequency plasma process. Background technique [0002] With the development of modern technologies such as aviation, atomic energy, and new smelting technologies, more and more stringent requirements are put forward for high-temperature structural materials, requiring materials to have good high-temperature performance to adapt to harsh operating environments, such as thermal shock resistance, high-temperature strength, Corrosion resistance, oxidation resistance, etc. As a special high-temperature ceramic material, zirconium boride has high melting point, high strength, high hardness, good electrical and thermal conductivity, good flame retardancy, heat resistance, oxidation resistance, corrosion resistance and neutron capture, et...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/04C04B35/626C04B35/58
Inventor 袁方利白柳杨张海宝胡鹏李晋林黄淑兰
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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