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Method of synthesizing titanium carbonitride powder using low temperature molten salt carbon heat reduction

A technology of titanium carbonitride and low-temperature molten salt, which is applied in chemical instruments and methods, inorganic chemistry, titanium compounds, etc., can solve the problems of decreased activation energy and complex process, and achieve large particle size, high purity, and crystal grain The effect of regular shapes

Inactive Publication Date: 2006-09-13
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

H.H.Nersisyan et al. studied the synthesis of WC powder by using magnesia thermal and carbothermal reduction methods under molten salt conditions, and calculated the reaction activation energy as 35kcal / mol (H.H.Nersisyan, H.I.Won, C.W.Won, Combustion synthesis of WC powder in the presence of alkali salts, Materials letters, 2005, 59: 3950-3954), due to the existence of gas phase and liquid phase, the activation energy of the reaction decreases, and the crystal form of WC powder is well developed, but this method produces a large amount of by-product MgO and Na 2 WO 4 , need repeated pickling, the process is more complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Mix C in carbon black (average particle size 30nm) and anatase titanium dioxide (average particle size 1.08μm) at a molar ratio of 1:1~3, and add the above-mentioned mixture in a weight percentage of 5~ 30% lithium carbonate (average particle size 100μm), mixed evenly, press-molded under 10-200Mpa pressure, then kept at 800-1600℃ for 60-180 minutes under the condition of carbon embedding, and took out after natural cooling . The phase composition is analyzed by X-ray diffraction, and the microscopic analysis is carried out by scanning electron microscope and electron probe. The effect is significantly different with or without the presence of molten salt.

[0016] The test results show that under the condition of buried carbon, the phase of the molten salt sample is almost all titanium carbonitride (XRD analysis), and there is a very small amount of rutile. The particle size is uniform and regular, and the size is about 7 μm ( SEM), the composition is approximately Ti...

Embodiment 2

[0018] Mix C in starch (average particle size 100 μm) and rutile titanium dioxide (average particle size 2.34 μm) in a molar ratio of 1:1 to 3, and add sulfuric acid with a weight percentage of 6 to 40% of the above mixture Sodium hydrogen (average particle size: 200μm) and 1-6% water are mixed evenly and then pelletized on a disc granulator, then kept at 900-1700°C for 90-180 minutes under a nitrogen atmosphere, and then cooled naturally take out. The phase composition is analyzed by X-ray diffraction, and the microscopic analysis is carried out by scanning electron microscope and electron probe. The effect is significantly different with or without the presence of molten salt.

[0019] The test results show that: under a nitrogen atmosphere, at a lower temperature (1000°C), the phase of the molten salt sample is almost all titanium nitride (XRD analysis), and the particle size is uniform and regular, with a size of 5 ~8μm (SEM), the composition is TiN (EPMA); products with...

Embodiment 3

[0021] Mix C in graphite (average particle size 80 μm) and anatase titanium dioxide (average particle size 1.08 μm) in a molar ratio of 1:1 to 3, and add 4 to 20 weight percent of the above mixture % ammonium bisulfate (average particle size 150μm) and 1-6% polyvinyl alcohol, mixed evenly and then machine-pressed at a pressure of 40-250Mpa, and then kept at 800-1800°C for 50 minutes in an argon atmosphere. ~600 minutes, take out after natural cooling. The phase composition is analyzed by X-ray diffraction, and the microscopic analysis is carried out by scanning electron microscope and electron probe. The effect is significantly different with or without the presence of molten salt.

[0022] The test results show that: under this condition, the phase of the molten salt is almost entirely titanium carbide (XRD analysis), with a very small amount of rutile, the particle size is uniform and regular, the size is about 5 μm (SEM), and the composition is TiC (EPMA); and the sample ...

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Abstract

A process for synthesizing the powder of titanium carbonitride includes such steps as proportionally mixing C-contained mixture, TiO2 fused salt and binder, die pressing to become balls, heating at 600-1800 deg.C for 30-120 min under protection of A2 or N2, and natural cooling.

Description

1. Technical field [0001] The invention belongs to the preparation technology of non-oxide ceramics. In particular, it relates to a method for synthesizing titanium carbonitride powder by a carbothermal reduction method in the presence of molten salt at low temperature. 2. Background technology [0002] Ti(C 1-X , N X ) is a continuous solid solution formed by TiN and TiC, and its properties change with the composition X. TiN has better toughness, while TiC has higher hardness. Generally speaking, as X increases, the hardness of the material decreases and the toughness increases. Titanium carbonitride is a non-oxide ceramic material with excellent performance and wide application, and it is also a high-grade refractory material. It combines the advantages of TiN and TiC, has high melting point, high hardness, wear resistance, oxidation resistance, corrosion resistance and other characteristics, and has good thermal conductivity, electrical conductivity and chemical stabi...

Claims

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Application Information

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IPC IPC(8): C01G23/00C01B21/082C01B31/30C04B35/515
Inventor 李远兵陈希来李亚伟李楠赵雷金胜利雷中兴洪学勤
Owner WUHAN UNIV OF SCI & TECH
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