Method for preparing micro-nano titanium carbonitride powder with controllable carbon-nitrogen ratio by adopting solid state nitrogen source

A technology of titanium carbonitride and carbon-nitrogen ratio, which is applied in the field of ceramic material preparation, can solve the problems of difficult and accurate control of C/N, high reaction temperature, and low production efficiency, and achieve precise and controllable carbon-nitrogen ratio and low preparation temperature , low cost effect

Inactive Publication Date: 2014-03-26
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The disadvantages of the prior art are that the reaction temperature is high and the time is long, so the production efficiency is low, the energy consumption is large, the production cost is high, and the C / N ratio is difficult to accurately control, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: Preparation of TiC 0.9 N 0.1 Ceramic powder

[0032] The raw materials are commercial titanium powder with a particle size of 200 mesh, carbon black and ammonium chloride, and the molar ratio is 1:0.9:0.1. The ingredients are 30 grams in total, 30 grams of NaCl are added, and after mixing, they are put into a stainless steel ball mill tank of a ball mill, and the steel tank is used After the rubber ring is sealed, vacuumize to 0.5Pa, fill with argon, and the pressure is 0.9atm. Then evacuate to 0.5Pa, and then fill with argon, the pressure is 0.9atm. Control the ball-to-material ratio to 10:1, and control the speed of the ball mill to 300 rpm. After ball milling for 6 hours, use a tablet machine to make a φ20mm green body under an axial pressure of 4MPa, and put the green body at 900°C in molten NaCl for 30 minutes. Put the salt block with Ti(C,N) ceramic powder cooled down after the reaction into water 10 times the weight of the salt block, and soak f...

Embodiment 2

[0033] Embodiment 2: Preparation of TiC 0.8 N 0.2 Ceramic powder

[0034] The raw materials are commercial titanium powder with a particle size of 200 mesh, carbon black and ammonium chloride. The molar ratio is 1:0.8:0.2. The ingredients are 30 grams in total. After the rubber ring is sealed, vacuumize to 1.0Pa, fill with argon, and the pressure is 1atm. Then evacuate to 1.0Pa, and then fill with argon, the pressure is 1atm. Control the ball-to-material ratio to 20:1, and control the speed of the ball mill to 200 rpm. After ball milling for 5 hours, use a tablet machine to make a φ20mm green body under an axial pressure of 5MPa, and put the green body at 1000°C in molten NaCl for 30 minutes. Put the salt block with Ti(C,N) ceramic powder cooled down after the reaction into water 10 times the weight of the salt block, and soak for 10 hours. After NaCl is completely dissolved in water. Filter out the Ti(C, N) ceramic powder, rinse and dry the Ti(C, N) ceramic powder repea...

Embodiment 3

[0035] Embodiment 3: Preparation of TiC 0.7 N 0.3 Ceramic powder

[0036]The raw materials are commercial titanium powder with a particle size of 200 mesh, carbon black and ammonium chloride, and the molar ratio is 1:0.7:0.3. The ingredients are 30 grams in total, 30 grams of NaCl are added, and after mixing, they are put into a stainless steel ball mill tank of a ball mill, and the steel tank is used After the rubber ring is sealed, vacuumize to 1.0Pa, fill with argon, and the pressure is 1.1atm. Then evacuate to 1.0Pa, and then fill with argon, the pressure is 1.1atm. Control the ball-to-material ratio to 20:1, and control the speed of the ball mill to 150 rpm. After ball milling for 8 hours, use a tablet press to make a green body with a diameter of 20 mm under an axial pressure of 4 MPa, and put the green body at 800 ° C. in molten NaCl for 30 minutes. Put the salt block with Ti(C,N) ceramic powder cooled down after the reaction into water 10 times the weight of the sa...

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Abstract

The invention discloses a method for preparing micro-nano titanium carbonitride powder with controllable carbon-nitrogen ratio by adopting a solid state nitrogen source. The method comprises the steps of 1, preparing ammonium chloride, titanium powder and carbon black; 2, uniformly mixing the ammonium chloride, the titanium powder and the carbon black; 3, adding sodium chloride into the mixture; 4, grinding and uniformly mixing the mixed powder obtained in the step 3 to prepare a blank; 5, placing the blank into the fusing sodium chloride, performing temperature preservation and cooling to obtain sodium chloride salt blocks carrying the titanium carbonitride powder; and 6, performing desalting treatment on the sodium chloride salt blocks carrying the titanium carbonitride powder to prepare the titanium carbonitride powder with the size being 300-500nm. According to the invention, Ti(C, N) ceramic powder is prepared by taking the titanium powder and the carbon black as the raw materials and the ammonium chloride as solid state nitrogen source, the preparation process is simple, the cost is low, the preparation temperature is low, the energy consumption is small, and the carbon nitrogen ration is controllable.

Description

technical field [0001] The invention relates to the improvement of the preparation method of titanium carbonitride powder, in particular to a method for preparing micro-nano titanium carbonitride powder with a controllable carbon-nitrogen ratio by using a solid nitrogen source, and belongs to the technical field of ceramic material preparation. Background technique [0002] Ti(C, N) has a series of advantages such as high strength, high hardness, high temperature resistance, acid and alkali resistance, wear resistance, good electrical conductivity and thermal conductivity, and is widely used in the preparation of cermets, cutting tools, molds, and smelting metals. Lining materials for crucibles, electrodes for molten salt electrolysis of metals, and coating materials for electrical contacts and metal surfaces. Especially the superfine powder has great development value and application prospect as the reinforcing phase of composite materials. [0003] The main method of prep...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/58C04B35/626
Inventor 杨瑞嵩李明田刘春海崔学军金永中林修洲
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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