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Preparation method of titanium nitride nano-powder

A technology of titanium nitride nanometer and nanometer powder, which is applied in the field of preparation of titanium nitride nanometer powder, which can solve the problems of difficult control of the reaction process, high reaction temperature and high energy consumption, and achieve low production cost and low energy consumption of the reaction. Low, high-purity effect

Active Publication Date: 2018-09-28
青岛桥海陶瓷新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The gas phase method is a new technology developed in recent decades: using titanium tetrachloride, ammonia, hydrogen, and nitrogen as raw materials, chemical reactions are carried out in the reactor to prepare titanium nitride powder. This method reacts quickly, but the reaction The process is not easy to control, and the reaction temperature is high and energy consumption is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A preparation method of titanium nitride nanopowder, comprising the following steps:

[0025] 1) Using toluene as a reaction aid, add liquid ammonia to the reaction aid, after the liquid ammonia and toluene are stably separated, add titanium tetrachloride toluene solution to the toluene and carry out the compound reaction at -60°C under vacuum conditions, The vacuum pressure is 0.8 atmospheric pressure, and the titanium nitride precursor is obtained by washing after the reaction; the mass ratio of titanium tetrachloride:ammonia:toluene is 50:300:150.

[0026] 2) The titanium nitride precursor obtained in step 1) is carried out under a nitrogen protective atmosphere at a temperature of 800°C, high-temperature roasting, and the roasting time is controlled at 30 minutes to obtain titanium nitride nanopowders. After testing, the titanium nitride nanopowders The particle size of the body is 100nm.

Embodiment 2

[0028] A preparation method of titanium nitride nanopowder, comprising the following steps:

[0029] 1) Toluene is used as a reaction aid, and liquid ammonia is added to the reaction aid. After the liquid ammonia and toluene are stably separated, titanium tetrachloride solution is added to the toluene to perform a compound reaction at -50°C under vacuum conditions. The pressure is 1 atmosphere, and washing is performed after the reaction to obtain a titanium nitride precursor; the mass ratio of titanium tetrachloride:ammonia:toluene is 100:500:400.

[0030] 2) Carry out the titanium nitride precursor obtained in step 1) under a nitrogen protective atmosphere at a temperature of 1000°C, high-temperature roasting, and the roasting time is controlled at 60 minutes to obtain titanium nitride nanopowders. After testing, the titanium nitride nanopowders The particle size of the body is 300nm.

Embodiment 3

[0032] A preparation method of titanium nitride nanopowder, comprising the following steps:

[0033] 1) Toluene is used as a reaction aid, and liquid ammonia is added to the reaction aid. After the liquid ammonia and toluene are stably separated, titanium tetrachloride solution is added to the toluene to carry out a compound reaction at -40°C under vacuum conditions. The pressure is 1 atmosphere, and washing is performed after the reaction to obtain a titanium nitride precursor; the mass ratio of titanium tetrachloride:ammonia:toluene is 200:700:600.

[0034] 2) Carry out the titanium nitride precursor obtained in step 1) under a nitrogen protective atmosphere at a temperature of 1200°C, high-temperature roasting, and the roasting time is controlled at 120min to obtain titanium nitride nanopowders. After testing, the titanium nitride nanopowders The particle size of the body is 500nm.

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Abstract

The present invention provides a preparation method of a titanium nitride nano-powder. The preparation method comprises the following steps: 1) selecting one or more of non-polar aromatic hydrocarbonsand halogenated hydrocarbons as reaction promoter, adding liquid ammonia to the reaction promoter, adding titanium tetrachloride solution to the reaction promoter for a combination reaction at a lowtemperature after stable stratification of the liquid ammonia and the reaction promoter, and washing after the reaction is finished, thereby obtaining titanium nitride precursor; 2) carrying out high-temperature calcination of the titanium nitride precursor obtained in the step 1) to obtain titanium nitride nano-powder, wherein the titanium tetrachloride solution is prepared by dissolving titaniumtetrachloride in an organic solvent, and the organic solvent is one or more of non-polar aromatic hydrocarbons and halogenated hydrocarbons. The titanium nitride powder obtained by the preparation method is high in purity, uniform in particles, narrow in particle size distribution and small in particle size.

Description

technical field [0001] The invention belongs to the technical field of titanium nitride preparation, and in particular relates to a preparation method of titanium nitride nanometer powder. Background technique [0002] Titanium nitride powder is the basic raw material for the preparation of titanium nitride ceramics, and is the key to the performance of titanium nitride ceramics. The nano-sized titanium nitride powder is black, and the micron-sized titanium nitride powder is yellow. Titanium nitride ceramic is a high-performance ceramic, which has excellent physical and chemical properties, such as high strength, high hardness, high temperature resistance, wear resistance, acid and alkali corrosion resistance, and good electrical conductivity, thermal conductivity, etc. Advantages are widely used. [0003] Nano-titanium nitride powder refers to titanium nitride powder whose grain size is within 100 nanometers. Using it as a raw material instead of micron-sized titanium nitr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C04B35/626
CPCC04B35/58014C04B35/626C04B2235/5445
Inventor 韩召刘在翔陈琦陈守刚王俊有金波马丁·科恩斯图尔特
Owner 青岛桥海陶瓷新材料科技有限公司
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