Method for preparing nanocrystalline zirconium carbide powder

A technology of zirconium carbide and nanocrystals, which is applied in the field of ceramic materials, can solve the problems of uneven particle size, complex reaction process, and high energy consumption, etc., and achieve easy large-scale production, simple preparation process, and uniform grain size Effect

Inactive Publication Date: 2012-11-07
SHANGHAI UNIV
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  • Abstract
  • Description
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Problems solved by technology

The electric arc furnace carbothermal reduction method has high requirements for reaction equipment, high energy consumption, low production capacity, and the average particle size of the generated powder particles is relatively large; the self-propagating high-temperature synthesis method uses metal zirconium as a raw material, and the cost is high. The reaction process and product performance It is difficult to control, and it is not easy to obtain nanocrystalline products; the high-energy ball milling method consumes a lot of energy, the particle size of the generated powder is uneven, and it is easy to introduce impurities; Complex, harsh conditions, long production cycle, and residual harmful derivatives in the product

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  • Method for preparing nanocrystalline zirconium carbide powder

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Embodiment 1

[0017] A method for preparing nanocrystalline zirconium carbide powder, the method comprising the following processes and steps:

[0018] (1) Zirconium oxychloride, sucrose, and ammonia water are used as raw materials, and polyethylene glycol 6000 is used as a dispersant. First mix absolute ethanol and water at a volume ratio of 5:1, and add polyethylene glycol 6000 with a total amount of alcohol and water of 1 wt%, and then add 0.05mol zirconium oxychloride to the mixed solution of absolute ethanol and water , stirred for 1 hour, slowly added 17ml of ammonia water into the mixture through a separatory funnel, then added 0.02mol of sucrose into the mixture, stirred at room temperature for 3 hours, after fully reacting, dried at 60°C, ground and pressed into a green body.

[0019] (2) Place the green body in a high-temperature tube furnace to embed activated carbon, and synthesize it through a high-temperature reaction at 1550°C under the protection of a high-purity argon atmos...

Embodiment 2

[0022] A method for preparing nanocrystalline zirconium carbide powder, the method comprising the following processes and steps:

[0023] (1) Zirconium oxychloride, sucrose, and ammonia water are used as raw materials, and polyethylene glycol 6000 is used as a dispersant. First mix absolute ethanol and water at a volume ratio of 3:1, and add polyethylene glycol 6000 with a total amount of alcohol and water of 1.5wt%, and then add 0.05mol zirconium oxychloride to the mixed solution of absolute ethanol and water , stir for 1 hour, slowly drop 23ml of ammonia water into the mixture through a separatory funnel, then add 0.05mol sucrose into the mixture, stir at room temperature for 3 hours, after fully reacting, dry at 60°C, grind and press into a green body .

[0024] (2) Place the green body in a high-temperature tube furnace to embed activated carbon, and synthesize it through a high-temperature reaction at 1650°C under the protection of a high-purity argon atmosphere, keep it...

Embodiment 3

[0026] A method for preparing nanocrystalline zirconium carbide powder, the method comprising the following processes and steps:

[0027] (1) Zirconium oxychloride, sucrose, and ammonia water are used as raw materials, and polyethylene glycol 6000 is used as a dispersant. First mix absolute ethanol and water at a volume ratio of 8:1, and add polyethylene glycol 6000 with a total amount of alcohol and water of 0.5wt%, and then add 0.05mol zirconium oxychloride to the mixed solution of absolute ethanol and water , stir for 1 hour, slowly drop 20ml of ammonia water into the mixture through a separatory funnel, then add 0.04mol sucrose into the mixture, stir at room temperature for 3 hours, after fully reacting, dry at 60°C, grind and press into a green body .

[0028] (2) Place the green body in a high-temperature tube furnace to embed activated carbon, and synthesize it through a high-temperature reaction at 1600°C under the protection of a high-purity argon atmosphere, keep it...

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Abstract

The invention relates to a method for preparing nanocrystalline zirconium carbide powder, which comprises the steps that zirconium oxychloride, ammonia water and cane sugar are used as raw materials; the zirconium oxychloride and the cane sugar are dissolved in the mixed solution of absolute ethyl alcohol and water according to a certain proportion; polyethylene glycol 6000 serving as a dispersing agent is added into the mixed solution, and then the ammonia water is dropwise added into the mixed solution for reaction to obtain zirconium hydroxide precipitation; the dried powder is pressed into green bodies; and the green bodies are baked in high-purity argon atmosphere at high temperature of 1500-1650 DEG C and then fully ground to obtain the nanocrystalline zirconium carbide powder. The method for preparing the nanocrystalline zirconium carbide powder has the advantages that the cost of the raw materials is low, the process is simple, the purity of the product is high, and the size of crystalline grains is uniform. The method for preparing the nanocrystalline zirconium carbide powder is favorable to large-scale production.

Description

technical field [0001] The invention relates to a method for preparing nanocrystalline zirconium carbide powder, which belongs to the technical field of ceramic materials. Background technique [0002] Zirconium carbide materials have the characteristics of high melting point, high strength, high hardness, radiation resistance, corrosion resistance, high chemical stability, good thermal conductivity and electrical conductivity, etc. , nuclear control materials and other fields have been important applications. [0003] At present, the methods for preparing zirconium carbide powder mainly include: electric arc furnace carbothermal reduction method, self-propagating high-temperature synthesis method, high-energy ball milling method, sol-gel method, reverse micelle method, etc. The electric arc furnace carbothermal reduction method has high requirements for reaction equipment, high energy consumption, low production capacity, and the average particle size of the generated powd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/30C04B35/56C01B32/914
Inventor 甄强孙凌云张中伟李榕王亚丽
Owner SHANGHAI UNIV
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