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A method for preparing nano titanium nitride powder by atmospheric pressure chemical vapor deposition

A technology of atmospheric pressure chemical vapor phase and nano-titanium nitride, which is applied in chemical instruments and methods, nanotechnology for materials and surface science, nanotechnology, etc., can solve problems such as high toxicity and unhealthy experimenters, and achieve repeatability High performance, low price, cost reduction effect

Active Publication Date: 2021-09-17
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Second, although chemical vapor deposition is also used for synthesis, the reactant melamine used can decompose at high temperature to produce highly toxic cyanide gas, which is harmful to the health of experimenters

Method used

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  • A method for preparing nano titanium nitride powder by atmospheric pressure chemical vapor deposition
  • A method for preparing nano titanium nitride powder by atmospheric pressure chemical vapor deposition
  • A method for preparing nano titanium nitride powder by atmospheric pressure chemical vapor deposition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] First, 1mmol of titanium powder and 15mmol of ammonium chloride are fully mixed and ground, the ground powder is put into a tube furnace, and the tube furnace is vacuumed for 20 minutes;

[0043] Then, feed argon and hydrogen, the argon flow rate is 50 sccm, the hydrogen flow rate is 20 sccm, the tube furnace is heated to 1200 °C at a heating rate of 2 °C / min, and the nanocrystal growth is completed by keeping the temperature for 20 min, then the heating is stopped and cooled to At room temperature, a black powder is obtained, which is the target product.

[0044] figure 1 It is the X-ray diffraction spectrum of the TiN nano-powder grown according to Example 1, and no impurity peak appears, indicating that the product is pure TiN.

[0045] figure 2 It is a SEM topography photo of the TiN nano powder grown according to Example 1. It can be seen that the size of the TiN particles is 100-200 nm, and agglomeration occurs among the particles.

Embodiment 2

[0047] First, 1mmol of titanium powder and 8mmol of ammonium chloride are fully mixed and ground, the ground powder is put into a tube furnace, and the tube furnace is vacuumed for 20 minutes;

[0048] Then, feed argon and hydrogen, the argon flow rate is 400 sccm, the hydrogen flow rate is 80 sccm, the tube furnace is heated to 900 °C at a heating rate of 3 °C / min, and the nanocrystal growth is completed by keeping the temperature for 60 min, then the heating is stopped and cooled to At room temperature, a black powder is obtained, which is the target product.

[0049] image 3 It is the X-ray diffraction spectrum of the TiN nano-powder grown according to Example 2. It can be seen that the main component of the product is TiN, and the crystallinity is good.

[0050] Figure 4 It is a SEM topography photo of the TiN nano powder grown according to Example 2, it can be seen that the TiN particle size is 50-100 nm.

Embodiment 3

[0052] First, fully mix and grind 1mmol titanium powder and 10mmol ammonium chloride, put the ground powder into a tube furnace, and vacuumize the tube furnace for 20 minutes;

[0053] Then, feed argon and hydrogen, the flow rate of argon gas is 200 sccm, the flow rate of hydrogen gas is 40 sccm, the tube furnace is heated to 800 °C at a heating rate of 5 °C / min, and the nanocrystal growth is completed by keeping the temperature for 30 min, then the heating is stopped and cooled to At room temperature, a black powder is obtained, which is the target product.

[0054] Figure 5 It is the X-ray diffraction spectrum of the TiN nano powder grown according to Example 3. It can be seen that the main component of the product is TiN, and the crystallinity is good.

[0055] Figure 6 It is a SEM image of the TiN nano powder grown according to Example 3. It can be seen that the size of TiN particles is 50-100 nm, and there is agglomeration phenomenon among the particles.

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Abstract

The invention discloses a method for preparing nano-titanium nitride powder by atmospheric pressure chemical vapor deposition method. The titanium source and the nitrogen source are fully mixed and ground; then the ground powder is put into a tube furnace, and then the Heating the tube furnace to a specified temperature under a reducing atmosphere and keeping it warm, and cooling to room temperature after the reaction was completed to obtain a gray-black powder, which is the target product TiN. The present invention adopts the chemical vapor deposition method to synthesize high-purity nano-titanium nitride powder, which avoids the reaction process of high temperature and high time-consuming, and the preparation method requires few raw materials and few synthesis steps, and the whole process involved is convenient and simple to operate and low in cost. low and easy to mass-produce.

Description

technical field [0001] The invention belongs to the technical field of nanometer material preparation, and in particular relates to a method for preparing nanometer titanium nitride powder by an atmospheric pressure chemical vapor deposition method. Background technique [0002] Nitrogen is the most abundant element in the air, but because of its very stable chemical properties, it is difficult to react chemically, but under some specific conditions, it can form nitrides with some transition elements, such as titanium nitride, nitrogen Vanadium, zirconium nitride, etc. Among these nitrides, more research and attention has been paid to titanium nitride. Titanium nitride has many excellent physical and chemical properties, such as high melting point (2950 ° C), high hardness, its Mohs hardness is 8-9, high temperature chemical stability and excellent thermal conductivity and electrical conductivity. In addition, titanium nitride is also It has excellent magnetic and optical p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/076B82Y30/00
Inventor 葛万银常哲焦思怡徐美美张塨凡施金豆高文兴
Owner SHAANXI UNIV OF SCI & TECH
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