Preparation method of nano titanium diboride powder

A nano-titanium diboride, titanium diboride technology, applied in nanotechnology, nanotechnology, boron/boride, etc., can solve the problems of poor powder dispersion, uneven particle size distribution, and many structural defects , to achieve the effects of accelerating the ball milling process, enhancing surface activity, and uniform particle size distribution

Active Publication Date: 2020-02-21
安徽中航纳米技术发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition there is TiCl 4 and NaBH 4 As the reaction raw material, a reduction reaction (500-700°C) occurs in an inert gas (Ar) to obtain TiB with a uniform particle size (20nm) 2 powder, but the hydrogen chloride gas produced has environmental pollution and the prepared powder has poor dispersibility
The traditional mechanochemical method mainly uses ball milling to make the raw material particles finer, improve the surface energy of the powder, and reduce the reaction temperature. It has the advantages of simple process and high production efficiency, but the synthetic powder has uneven particle size distribution and many structural defects. is an area that needs further improvement

Method used

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  • Preparation method of nano titanium diboride powder
  • Preparation method of nano titanium diboride powder

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preparation example Construction

[0019] The present invention proposes a preparation method of nano titanium diboride powder, the steps are as follows:

[0020] Step 1, preparing titanium diboride coarse powder

[0021] According to the weight ratio of 1:3~5:2~3, take titanium nitrate, magnesium powder, and boron tribromide and place them in a sealed high-pressure reactor, and react at 200~300°C for 1~5 hours, and the reaction product is washed with acid Remove impurities, filter, and dry to obtain titanium diboride coarse powder, which contains some titanium nitride impurities (titanium nitride cannot be removed by pickling).

[0022] Step 2, ball milling to prepare nano-titanium diboride powder

[0023] Put the ball mill tank containing titanium diboride coarse powder and grinding aid ethylene glycol (the weight ratio of the two is 1:1) into the plasma ball mill, set the rotation speed of 300-600 rpm and the milling time ( 4, 8, 12 hours) after ball milling.

[0024] After the ball milling is finished, t...

Embodiment 1

[0032] The preparation of nano titanium diboride powder, the steps are as follows:

[0033] Step 1, preparing titanium diboride coarse powder

[0034] According to the weight ratio of 1:3:2, take titanium nitrate, magnesium powder, and boron tribromide in a sealed high-pressure reactor, and react at 260°C for 3 hours. The reaction product is washed with acid to remove impurities, filtered, and dried to obtain two Coarse titanium boride powder contains some titanium nitride impurities.

[0035] Step 2, ball milling to prepare nano-titanium diboride powder

[0036] Put the ball mill tank containing titanium diboride coarse powder and grinding aid ethylene glycol (the weight ratio of the two is 1:1) into the plasma ball mill, set the speed at 400 rpm and the ball milling time for 4 hours Perform ball milling.

[0037] After the ball milling is finished, the reaction product is taken out and classified to obtain titanium diboride nanopowders with different particle size distrib...

Embodiment 2

[0039] The preparation of nano titanium diboride powder, the steps are as follows:

[0040] Step 1, preparing titanium diboride coarse powder

[0041] According to the weight ratio of 1:5:3, take titanium nitrate, magnesium powder, and boron tribromide in a sealed high-pressure reactor, and react at 220°C for 4 hours. The reaction product is washed with acid to remove impurities, filtered, and dried to obtain two Coarse titanium boride powder contains some titanium nitride impurities.

[0042] Step 2, ball milling to prepare nano-titanium diboride powder

[0043] Put the ball mill tank containing titanium diboride coarse powder and grinding aid ethylene glycol (the weight ratio of the two is 1:1) into the plasma ball mill, set the speed at 600 rpm and the ball milling time for 8 hours Perform ball milling.

[0044] After the ball milling is finished, the reaction product is taken out and classified to obtain titanium diboride nanopowders with different particle size distrib...

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Abstract

The invention discloses a preparation method of nano titanium diboride powder, and relates to the technical field of preparation of high-melting-point boride powder. Titanium nitrate, magnesium powderand boron tribromide are taken and placed in a sealed high-pressure reaction kettle and undergo a reaction, a reaction product is washed, filtered and dried, titanium diboride coarse powder is obtained, and the coarse powder contains part of titanium nitride impurities; a ball-milling tank filled with the titanium diboride coarse powder and a grinding aid is put into a plasma ball mill, the rotating speed and the ball-milling time are set, and then ball-milling treatment is carried out; and after the ball milling is finished, a reaction product is taken out and is subjected to grading treatment to obtain the nano titanium diboride powder with different particle size distributions. No harmful substance is generated in the ball milling process, and environmental protection is facilitated. Meanwhile, plasmas with certain strength are introduced in the ball milling process, so that the surface activity of powder particles is enhanced, further reaction of impurity phases in the raw materials is induced, the structural defects of the powder are further controlled, the product is purified, and meanwhile, the ball milling process is accelerated.

Description

technical field [0001] The invention relates to the technical field of preparation of high melting point boride powder, in particular to a preparation method of nanometer titanium diboride powder. Background technique [0002] Transition metal borides with high melting point, high strength, good wear resistance and chemical stability, high electrical and thermal conductivity have become a hot research direction in recent years. Titanium diboride (TiB 2 ) is an important boride material, which is a diboride of a Group IVB metal and has the same hexagonal planar network structure. Titanium diboride (TiB 2 ) In addition to the good physical and chemical properties of transition metal borides, it also has excellent electrical properties, oxidation resistance and high temperature creep resistance, which makes titanium diboride (TiB 2 ) has a wide range of applications in the fields of structural materials, functional materials, and ultra-high temperature materials. [0003] A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/04B82Y30/00
CPCC01B35/04B82Y30/00C01P2006/80
Inventor 王开新韩成良周正曹显志郭秀凤
Owner 安徽中航纳米技术发展有限公司
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