Method for producing ultrafine zirconium powder

A production method and technology of zirconium powder, which is applied in the field of production of ultrafine zirconium powder, can solve problems such as being unable to meet the application requirements of ultrafine zirconium powder, avoid spontaneous combustion and explosion phenomena, stabilize the process, and meet technical indicators and application requirements Effect

Active Publication Date: 2014-10-22
CITIC JINZHOU METAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, at present, zirconium powder with fine particle size mainly includes zirconium powder for thermal batteries, which is used as heating material for thermal batteries of weapons such as rockets and missiles. <6μm accounts for 30% to 40%, and its particle size is coarser than ultrafine zirconium powder, which cannot meet the application requirements of ultrafine zirconium powder

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] （1） Put 10kg zirconium sponge (the total zirconium content is greater than 99.4%) and 2kg electrolytic zirconium powder (the total zirconium content is greater than 99%) into the crucible of the hydrogenation reactor (the charging amount accounts for 2 / 3 of the total volume of the crucible), Pump high vacuum, when the vacuum degree is less than or equal to 10Pa, close the valve of the vacuum system, pass in high-purity hydrogen, energize the resistance wire, control the current to 10A, heat the mixture of sponge zirconium and electrolytic zirconium to 300°C, and stop the power supply. Hold the heat for 2.5 hours to hydrogenate the raw material zirconium, and keep the hydrogenation reactor at normal pressure during the whole hydrogenation process to obtain zirconium hydride;

[0021] (2) Put 4.0kg of zirconium hydride into a ball mill tank with 4.2kg of agate balls. The model of the ball mill tank is Φ247mm×355mm, and the inner substrate is a zirconium lining. Fill the b...

Embodiment 2

[0026] (1) Put 8kg zirconium sponge (total zirconium content greater than 99.4%) and 2kg electrolytic zirconium powder (total zirconium content greater than 99%) into the crucible of the hydrogenation reactor (feeding amount accounts for 2 / of the total volume of the crucible 3), draw a high vacuum, when the vacuum degree is less than or equal to 10Pa, close the valve of the vacuum system, pass in high-purity hydrogen, energize the resistance wire, control the current to 20A, heat the mixture of sponge zirconium and electrolytic zirconium to 400°C, Stop energizing, keep warm for 2 hours to hydrogenate the raw material zirconium, keep the hydrogenation reactor at normal pressure during the whole hydrogenation process, and obtain zirconium hydride;

[0027] (2) Put 5.5kg of zirconium hydride into a ball milling jar containing 5.0kg of agate balls. The model of the ball milling jar is Φ247 mm × 355mm, and the inner substrate is a zirconium lining. Fill the ball milling jar with de...

Embodiment 3

[0032] (1) Put 12kg zirconium sponge (total zirconium content is greater than 99.4%) and 4kg electrolytic zirconium powder (total zirconium content is greater than 99%) into the crucible of the hydrogenation reactor (feeding amount accounts for 2 / of the total volume of the crucible 3) Draw a high vacuum. When the vacuum degree is less than or equal to 10Pa, close the valve of the vacuum system, pass in high-purity hydrogen, energize the resistance wire, and control the current to 15A. Heat the mixture of sponge zirconium and electrolytic zirconium to 360°C to ignite. Stop energizing, keep warm for 2.2 hours to hydrogenate the raw material zirconium, keep the hydrogenation reactor at normal pressure during the whole hydrogenation process, and obtain zirconium hydride;

[0033] (2) Put 5.0kg of zirconium hydride into a ball mill jar with 4.5kg of agate balls. The model of the ball mill is Φ247mm×355mm, and the inner substrate is zirconium lining. Fill the ball mill jar with deio...

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Abstract

The invention discloses a method for producing ultrafine zirconium powder. The method comprises the following steps: mixing firearm zirconium sponge and electrolyzed zirconium serving as raw material zirconium, adding the mixture into a material receiving crucible of a hydrogenation reactor, igniting the raw material zirconium and hydrogenating to obtain zirconium hydride; putting the zirconium hydride into a ball-milling tank loaded with a ball-milling medium, and performing ball milling till the granularity of the zirconium hydride is smaller than or equal to 400 meshes; putting the smashed zirconium hydride into a vacuum drying oven for drying, loading the smashed and dried zirconium hydride into a dehydrogenating furnace for dehydrogenating, putting the dehydrogenated zirconium hydride into the ball-milling tank loaded with the ball-milling medium for performing ball-milling, sieving, washing and drying to obtain ultrafine zirconium powder. The method has the advantages that the raw materials are readily available, the technological process is stable, the phenomena of self-ignition and explosion are avoided, and the technical index and safety production requirements of the ultrafine zirconium powder can be met.

Description

technical field [0001] The invention relates to a production method of ultrafine zirconium powder. Background technique [0002] Zirconium powder has excellent gas absorption performance and is widely used in ammunition, fireworks and electric vacuum fields. The ultra-fine zirconium powder can greatly improve the burning speed and detonation sensitivity, and the ignition diffusion spreads quickly, which is stable and reliable. The ultra-fine zirconium powder with active zirconium content > 90% and particle size ≤ 10 μm, accounting for 70%, can be used as an ignition agent for nuclear power source pyrotechnics. [0003] Because zirconium powder has a large specific surface and specific surface energy, it reacts rapidly with oxygen. When the average particle size of zirconium powder is ≤10μm and it is suspended, it will spontaneously ignite and explode. Therefore, at present, zirconium powder with fine particle size mainly includes zirconium powder for thermal batteries,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/00
Inventor 齐牧崔传海李广明刘飞李杰孙秀焕王敏张绪东
Owner CITIC JINZHOU METAL
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