Method for preparing titanium carbonitride from titanium carbonitride powder and hydrolyzable titanium source

A titanium carbonitride, hydrolyzable technology, applied in the field of ceramic powder preparation, can solve the problems of material defects, easy denitrification, difficult to achieve mass production, etc., and achieve the effect of low preparation cost

Active Publication Date: 2021-06-25
XIAMEN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses physical methods to realize the mixing of carbon and titanium. Due to the difference in the ratio and polarity of the raw materials, it is difficult to mix the raw materials evenly, and it is easy to cause incomplete reaction.
[0004] Chinese patent application CN 101462701 A discloses a method for preparing titanium nitride ceramic powder, which uses a low-temperature combustion method to uniformly mix titanium source and carbon source to prepare precursor powder, but this method needs to use strong acid as an oxidant, which requires certain equipment , it is difficult to achieve mass production
The synthesis temperature of this method is 450°C, while the sintering temperature of titanium carbonitride-based cermets is 1300-1450°C, and the powder synthesis temperature is much lower than its use temperature. In practical applications, denitrification is very easy to cause material defects, and the use value is not high.
The reaction vessel of this method is a high-temperature and high-pressure stainless steel reactor, which is difficult to achieve mass production

Method used

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  • Method for preparing titanium carbonitride from titanium carbonitride powder and hydrolyzable titanium source
  • Method for preparing titanium carbonitride from titanium carbonitride powder and hydrolyzable titanium source
  • Method for preparing titanium carbonitride from titanium carbonitride powder and hydrolyzable titanium source

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Titanium carbonitride was prepared according to the following steps:

[0044] (1) Mix 300ml of cyclohexane with 150ml of ethanol, adjust the pH to 2~3, add 12g of cetyltrimethylammonium bromide, adjust the pH to 2~3, and slowly drop in the 24ml of titanium tetrachloride to obtain liquid A. Mix 150ml ethanol with 50ml deionized water. Add 18g of cetyltrimethylammonium bromide and 6.68g of carbon black, and stir for 30 minutes to obtain liquid B. Mix liquids A and B and continue to stir for 30 minutes.

[0045] (2) Mix 150ml of ammonia water and 150ml of deionized water, pour it into an infusion bottle, use a 34G needle under high-speed magnetic stirring conditions, drop the diluted ammonia water into the mixed solution obtained in (1), and wait until the pH is 7 Stop dripping ammonia. The suspension was suction filtered to extract the precipitate.

[0046] (3) After the precipitate is dried, it is heated to 600° C. in a vacuum tube furnace and kept for 2 hours to ob...

Embodiment 2

[0051] Titanium carbonitride was prepared according to the following steps:

[0052] (1) Mix 600ml of cyclohexane with 300ml of ethanol, adjust the pH to 2~3, add 20g of cetyltrimethylammonium bromide, adjust the pH to 2~3, and slowly drop in the 48ml of titanium tetrachloride was obtained as liquid A. Mix 300ml ethanol with 200ml deionized water. Add 25g of cetyltrimethylammonium bromide and 12.33g of carbon black, and stir for 30min to obtain liquid B. Mix liquids A and B and continue to stir for 30 minutes.

[0053] (2) Mix 250ml of ammonia water and 250ml of deionized water, pour it into an infusion bottle, and use a 34G needle under high-speed magnetic stirring conditions, drop the diluted ammonia water into the mixed solution obtained in (1) until the pH is 7 Stop dripping ammonia. The suspension was suction filtered to extract the precipitate.

[0054] (3) After the precipitate is dried, it is heated to 600° C. in a vacuum tube furnace and kept for 2 hours.

[005...

Embodiment 3

[0058] Titanium carbonitride was prepared according to the following steps:

[0059] (1) Mix 300ml of cyclohexane with 150ml of ethanol, adjust the pH to 2~3, add 12g of cetyltrimethylammonium bromide, adjust the pH to 2~3, and slowly drop in the 24ml of titanium tetrachloride to obtain liquid A. Mix 150ml ethanol with 50ml deionized water. Add 18g of cetyltrimethylammonium bromide and 6.68g of carbon black to obtain liquid B. Mix liquids A and B and continue to stir for 30 minutes.

[0060] (2) Mix 150ml of ammonia water and 150ml of deionized water, pour it into an infusion bottle, use a 34G needle under high-speed magnetic stirring conditions, drop the diluted ammonia water into the mixed solution obtained in (1), and wait until the pH is 7 Stop dripping ammonia. The suspension was suction filtered to extract the precipitate.

[0061] (3) After the precipitate is dried, it is heated to 600° C. in a vacuum tube furnace and kept for 2 hours.

[0062] (4) Grind the precu...

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Abstract

The invention relates to a method for preparing titanium carbonitride from titanium carbonitride powder and a hydrolyzable titanium source. The hydrolyzable titanium source is used as the titanium source, carbon black is used as the carbon source, and Triton X‑100 or hexadecane is used. Trimethylammonium bromide is used as surfactant, cyclohexane is used as hydrolysis buffer, and ammonia water is used as precipitant. The preparation process is as follows: configure emulsion→drop ammonia water→suction filtration of suspension, wash, dry→precursor Powder pretreatment → carbothermal nitriding reduction → titanium carbonitride. The method does not use ball mill mixing, can realize mass production, the particle size of the product is 200-300nm, the purity is greater than 99%, the preparation cost is low, and a new synthetic route is provided for titanium carbonitride.

Description

technical field [0001] The invention relates to the technical field of ceramic powder preparation, in particular to a method for preparing titanium carbonitride from titanium carbonitride powder and a hydrolyzable titanium source. Background technique [0002] WC-Co cemented carbide has high strength and good toughness, and is widely used in modern manufacturing, but its hardness and wear resistance are slightly insufficient, which is limited in some applications. Titanium carbonitride-based cermet material has become an ideal material to replace WC-Co cemented carbide due to its high hardness, high red hardness and wear resistance. However, in order to prepare titanium carbonitride cermet materials with excellent comprehensive properties, it is necessary to prepare titanium carbonitride ceramic powders with high purity, fine particle size and stable sintering performance. [0003] The preparation methods of titanium carbonitride powder include carbothermal nitriding reduct...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/58C04B35/622C04B35/626
Inventor 张厚安刘嘉威古思勇陈莹麻季冬廉冀琼
Owner XIAMEN UNIV OF TECH
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