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Method for preparing titanium nitride ceramic powder

A titanium nitride ceramic and titanium nitride technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of uneven mixing, high reaction temperature, long reaction time, etc., achieve uniform mixing, reduce Reaction temperature, effect of preventing agglomeration

Inactive Publication Date: 2009-06-24
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to increase the uniformity of raw material mixing, and at the same time, two kinds of submicron particles with smaller particle size can be directly contacted and reacted to improve the reaction activity, and synthesize high-purity and fine-grained ceramic powder under lower reaction temperature conditions; The thermal reduction method uses titanium dioxide and carbon black as raw materials to prepare titanium nitride powder, and the problems of uneven mixing, high reaction temperature and long reaction time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 0.1 mol of titanium tetrachloride, 0.1 mol of glucose, 0.2 mol of nitric acid, and 0.1 mol of urea. The above-mentioned substances were dissolved in 100ml of distilled water to prepare a solution, and the solution was heated on a temperature-controllable electric furnace at 300°C. After a series of processes such as volatilization, concentration, and bubbling, the solution underwent a combustion reaction to obtain a precursor. The precursor was pulverized and treated in air at 400° C. for 1 hour. The obtained material was reacted for 1 hour under the conditions of 1400° C. and a nitrogen flow rate of 3 l / min, and the reaction product was subjected to subsequent treatment to obtain titanium nitride powder.

Embodiment 2

[0021] Weigh 0.09 mol of titanium tetrachloride, 0.06 mol of citric acid, 1.5 mol of nitric acid, and 0.5 mol of urea. Dissolve the above-mentioned substances in 100ml of distilled water to prepare a solution, and heat the solution on a temperature-controllable electric furnace at 200°C. After the solution undergoes a series of processes such as volatilization, concentration, and bubbling, a combustion reaction occurs to obtain a precursor . The precursor was pulverized and treated in air at 200° C. for 2 hours. The obtained material was reacted for 10 hours under the conditions of 1200° C. and a nitrogen flow rate of 1 l / min, and the reaction product was subjected to subsequent treatment to obtain titanium nitride powder.

Embodiment 3

[0023] Weigh 0.09 mol of titanium tetrachloride, 0.06 mol of sucrose, 5 mol of nitric acid, and 0.5 mol of urea. Dissolve the above-mentioned substances in 100ml of distilled water to prepare a solution, and heat the solution on a temperature-controllable electric furnace at 400°C. After a series of processes such as volatilization, concentration, and bubbling, the solution undergoes a combustion reaction to obtain a precursor . The precursor was pulverized and treated in air at 600° C. for 1 hour. The resulting material was reacted at 1600° C. and a nitrogen flow rate of 5 l / min for 8 hours, and the reaction product was subjected to subsequent treatment to obtain titanium nitride powder.

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Abstract

The invention relates to a method for preparing titanium nitride ceramic powder, which belongs to the field of the preparation of ceramic powder. A titanium source comprises soluble titanium salt, namely titanium tetrachloride or titanium tetrabromide, and a carbon source comprises glucose, sucrose, citric acid and soluble starch. Nitric acid is used as an oxidizing agent, and urea is used as a fuel; and ammonium nitrate is used as a preparing agent. The mol ratio Ti ;C of the titanium source to the carbon source is 1 to (4-16), and the mol ratio of the nitric acid with the ammonium nitrate to the urea with the ammonium nitrate is (1-12) ;2. Various raw materials are dissolved in water and then are heated at a temperature of between 100 and 600 DEG C, and a solution undergoes a combustion reaction to generate precursors; the precursors are pulverized and then are pretreated for 0 to 10 hours at a temperature of between 200 and 800 DEG C, and then a carbon thermal reduction is carried out for 1 to 10 hours in the atmosphere of flowing nitrogen at a temperature of between 800 and 1,800 DEG C. Follow-up treatment is carried out on products to obtain titanium nitride powder. The titanium source and the carbon source in the precursors of the invention have fine granularity and are uniformly mixed; therefore, the method has good reaction activity and also has the advantages of lowering the temperature of the carbon thermal reduction reaction and improving the reaction rate. The method can prepare nanometer-level non-oxidized ceramic powder with good decentrality.

Description

technical field [0001] The invention belongs to the technical field of ceramic powder preparation, and in particular provides a method for preparing nano titanium nitride ceramic powder. Background technique [0002] Titanium nitride (TiN) ceramics have a series of advantages such as high strength, high hardness, high temperature resistance, acid and alkali corrosion resistance, wear resistance, good electrical conductivity and thermal conductivity, and are widely used in the preparation of cermets, cutting tools, and melting metals. Lining materials for electrodes for crucibles, molten salt electrolysis metals, electrical contacts and coating materials for metal surfaces, etc. [0003] High-quality powder raw materials are a prerequisite for obtaining high-performance products. To prepare ceramic materials with excellent performance, it is often necessary to first prepare powder raw materials with high purity, fine particle size, and good sintering performance. The prepara...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/076C04B35/58
Inventor 曲选辉秦明礼王建欧阳明亮张玲艳贾宝瑞
Owner UNIV OF SCI & TECH BEIJING
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