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Method for preparing low-oxygen high-pure metal hafnium powder

A technology of pure metal and hafnium powder, which is applied in the manufacture of low-oxygen high-purity hafnium metal powder and high-purity hafnium powder. and the effect of the likelihood of undergrowth

Active Publication Date: 2015-05-27
有研资源环境技术研究院(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, hafnium is a good getter, which will inevitably absorb gas in the preparation process, especially it is easy to combine with oxygen, which will cause certain difficulties in the preparation of low-oxygen metal hafnium powder

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh metal hafnium powder with a purity of 90wt% and a particle size of less than 1mm and blocky deoxidizer metal calcium chips with a purity greater than 95wt%, the molar ratio of the metal calcium chips and metal hafnium powder is 2:1, and weigh a certain amount of Purity greater than 96wt%, particle size less than 2mm molten salt CaCl 2 , and molten salt CaCl 2 The molar ratio of deoxidizer and deoxidizer is 1:1, according to the sequence of 1 / 4 mass of molten salt, raw material, deoxidizer, 3 / 4 mass of molten salt into the molybdenum crucible. Put the crucible into the reaction tank, cover the lid, vacuumize to 0.01Pa, and wash with argon. Heated to 850°C for 0.5 hours, kept at 850°C for 0.5 hours, protected by argon, and cooled to room temperature in an argon atmosphere after deoxygenation. The reaction product was washed 15 times with 0.2M hydrochloric acid at room temperature, and then washed once with deionized water at room temperature. The obtained product ...

Embodiment 2

[0034] Weigh metal hafnium powder with a purity of 95wt% and a particle size of less than 1mm and a deoxidizer LiH with a purity of more than 96wt% and a particle size of less than 1mm. The molar ratio of the deoxidizer LiH to the metal hafnium powder is 1:1. 96.0wt%, molten salt NaCl with a particle size of less than 2mm, and the molar ratio of molten salt NaCl and deoxidizer is 3:1, in the order of 1 / 4 mass of molten salt, raw materials, deoxidizer, and 3 / 4 mass of molten salt into a niobium crucible. Put the crucible into the reaction tank, cover the lid, vacuumize to 0.04Pa, and wash with argon. Heated to 1300°C for 6 hours, kept at 1300°C for 2 hours, protected by argon, and cooled to room temperature in an argon atmosphere after deoxygenation. The reaction product was washed 10 times with 0.2M hydrochloric acid at 70°C, and then washed once with deionized water at 70°C. The obtained product was sieved and dried to obtain hafnium powder. The quality of hafnium powder was...

Embodiment 3

[0036] Weigh metal hafnium powder with a purity of 93wt% and a particle size of less than 1mm and block-shaped deoxidizer Mg with a purity of more than 98wt%, the molar ratio of metal Mg and metal hafnium powder is 2:1, and weigh a certain mass of hafnium with a purity greater than 96.0wt %, particle size less than 2mm molten salt MgCl 2 , and molten salt MgCl 2 The molar ratio of deoxidizer and deoxidizer is 3:1, according to the sequence of 1 / 4 mass of molten salt, raw material, deoxidizer, 3 / 4 mass of molten salt into the molybdenum crucible. Put the crucible into the reaction tank, cover it, vacuumize to 0.03Pa, and wash with argon. Heated to 900°C for 2 hours, kept at 900°C for 5 hours, protected by argon, and cooled to room temperature in an argon atmosphere after deoxygenation. The reaction product was washed 7 times with 0.2M nitric acid at 40°C, and then washed 10 times with deionized water at room temperature. The obtained product was sieved and dried to obtain the...

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Abstract

The invention relates to a method for preparing low-oxygen high-pure metal hafnium powder; the low-oxygen high-pure metal hafnium powder has the purity of greater than 99.5wt% and the oxygen content being smaller than 0.15 wt%. The preparation method comprises the following steps: a. filling metal hafnium powder, a deoxidizing agent and a molten salt into a crucible; b, putting the crucible into a reaction tank, sealing the equipment, vacuumizing and inflating argon gas to wash the crucible, heating and deoxidizing, then performing constant-temperature and thermal-insulating deoxidization, cooling and discharging at the end of the deoxidization; c, pickling the discharged product, then washing with de-ionized water, sieving and drying the obtained product, namely, the product of the low-oxygen high-pure metal hafnium powder. The molten salt system is capable of effectively removing impurities in the metal hafnium powder, in particular, remarkably reducing the oxygen content in the hafnium powder; and the prepared low-oxygen high-pure metal hafnium powder satisfies the material requirement of high-end products.

Description

technical field [0001] The invention relates to a method for manufacturing high-purity hafnium powder, in particular to a method for manufacturing low-oxygen high-purity metal hafnium powder. It can be used in the preparation of high-purity hafnium powder used in fields such as atomic energy industry, information industry, petrochemical industry, and aerospace, and belongs to the field of pyrometallurgy. Background technique [0002] Hafnium has excellent nuclear properties, and its thermal neutron capture cross section is as high as 115b (1b=10 -28 m 2 ), can absorb thermal neutrons in nuclear reactors, and is used as control materials for nuclear reactors, as well as protective coatings and flux attenuators in reactors. Metal hafnium has good corrosion resistance, and its corrosion resistance in hot water and steam mixture is higher than that of titanium and zirconium, so it can be used as a special structural material in chemical industry. In addition, hafnium also has...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F1/00
Inventor 王芳黄永章王力军薛红霞
Owner 有研资源环境技术研究院(北京)有限公司
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