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Preparation of high-purity titanium biboride ceramic micropowder by using self-spreading high-temp. reduction synthesis process

A self-propagating high-temperature, titanium diboride technology, applied in the field of refractory compounds and their solid-phase synthesis, can solve the problems of long time, coarse product particle size, large powder particle size, etc., achieve low energy consumption and time consumption, and simple process , the effect of fine grain

Inactive Publication Date: 2002-03-27
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of this method: complex production equipment, high reaction temperature, long time, huge energy consumption, coarse grains of titanium diboride obtained, low boron content, poor product purity
Chinese patent CN105533A reports a carbon thermal reduction synthesis method of titanium diboride ceramic powder based on activated carbon as a reducing agent, ammonium pentaborate as a boron source and titanium dioxide as a titanium source. The time is long and the particle size of the product is coarse (about 10μm)
The powder synthesized by this process has high purity, but the particle size of the powder is large and some of them form hard aggregates; in addition, because the raw materials used are simple elements, the manufacturing cost is high and it cannot be industrialized.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0015] Example 1: 27 grams of TiO 2 Powder (≤80μm), 26g B 2 o 3 Mg powder (≤120μm), 47 grams of Mg powder (≤200μm) are fully mixed. The mixed sample is pressed into a block blank, put into a self-propagating high-temperature synthesis reactor, and under the protection of argon gas at normal temperature and pressure, the surface of the sample is ignited with a tungsten wire or an electric arc. The combustion wave spreads rapidly. At this time, the combustion temperature of the sample is 1800-2000°C, and the combustion reaction is completed within 1-2 minutes. After the sample was completely cooled, it was placed in a ball mill for ball milling for 2 hours. The obtained powder was put into a reaction kettle, 10 liters of hydrochloric acid with a concentration of 1 mol / l was added and stirred continuously, acid washed at 50° C. for 4 hours, filtered and dried. The composition of the obtained micropowder is: Ti68.2wt%, B30.1wt%, O0.5wt%, N0.1wt%, Mg0.1wt%, and the average part...

example 2

[0016] Example 2: 29 grams of TiO 2 Powder (≤80μm), 26g B 2 o 3 Mg powder (≤120μm), 45 grams of Mg powder (≤200μm) are fully mixed. The mixed sample is pressed into a block blank, put into a self-propagating high-temperature synthesis reactor, and under the protection of argon gas at normal temperature and pressure, the surface of the sample is ignited with a tungsten wire or an electric arc. The combustion wave spreads rapidly. At this time, the combustion temperature of the sample is 2000-2200°C, and the combustion reaction is completed within 1-2 minutes. After the sample was completely cooled, it was placed in a ball mill for ball milling for 2 hours. The obtained powder was put into a reaction kettle, 20 liters of sulfuric acid with a concentration of 0.5 mol / l was added and stirred continuously, acid washed at 50° C. for 6 hours, filtered and dried. The composition of the obtained micropowder is: Ti68.8wt%, B30.35wt%, O0.7wt%, N0.1wt%, Mg0.05wt%, and the average part...

example 3

[0017] Example 3: 29 grams of TiO 2 Powder (≤80μm), 28g B 2 o 3 Mg powder (≤1200μm), 43 grams of Mg powder (≤200μm) are fully mixed. The mixed sample is pressed into a block blank, put into a self-propagating high-temperature synthesis reactor, and under the protection of argon gas at normal temperature and pressure, the surface of the sample is ignited with a tungsten wire or an electric arc. The combustion wave spreads rapidly. At this time, the combustion temperature of the sample is 1700-1900°C, and the combustion reaction is completed within 1-2 minutes. After the sample was completely cooled, it was placed in a ball mill for ball milling for 2 hours. The obtained powder was put into a reaction kettle, 10 liters of hydrochloric acid with a concentration of 1 mol / l was added and stirred continuously, acid washed at 50° C. for 4 hours, filtered and dried. The composition of the obtained micropowder is: Ti67.87wt%, B31.3wt%, O0.6wt%, N0.1wt%, Mg0.13wt%, and the average p...

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PUM

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Abstract

The preparation method of high-purity TiB2 ceramic micropowder uses active metal reducing agent and cleap oxide raw material, and adopts the following steps: uniformly mixing TiO2, B2O3 and metal Mg powder, die-pressing and forming, placing the above-mentioned obtained material in a self-spreading high-temp. synthesis equipment with argon protection at normal temp. and normal pressure, lighting to make combustion, breaking combustion product, pickling so as to obtain the invented high-purity TiB2 ceramic micropowder. As compared with traditional carbon thermal reduced TiB2 ceramic powder saidinvention possesses the advantages of high purity, fine crystal grain, simple process and low energy consumption and time consumption, and as compared with SHS simple substance synthetic TiB2 ceramicpowder it is low in production cost.

Description

technical field [0001] The invention relates to a refractory compound and a solid phase synthesis method thereof. Background technique [0002] Titanium diboride ceramic powder is an important new type of engineering ceramic raw material. Its important physical and chemical properties include: high melting point (>3000°C), high hardness (>30GPa), high chemical stability, and high thermal conductivity. (120W / mK), high modulus (>570GPa), excellent electrical conductivity. Mainly used in: hard tool materials, composite material additives, new heating elements (>1800°C), high-temperature inert electrodes (>1200°C), high-temperature wear-resistant electrodes, high-temperature corrosion-resistant electrodes, high-strength lead frames for large-scale integrated circuits materials etc. But high purity TiB 2 The high price of raw materials limits the large-scale development and application of such materials. The traditional synthesis process of titani...

Claims

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Application Information

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IPC IPC(8): C04B35/515C04B35/58C04B35/65
Inventor 傅正义王为民王皓
Owner WUHAN UNIV OF TECH
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