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Superfine high-purity hafnium powder as well as preparation method and application thereof

A thin, high-purity hafnium technology is applied in the field of preparation of ultra-fine and high-purity hafnium powder.

Active Publication Date: 2012-07-04
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

[0003] The ultra-fine high-purity hafnium powder requires a purity of up to 99.99%, a total metal impurity content of less than 100ppm, an oxygen content of less than 0.2%, and a particle size of less than 1μm. There is no literature report on the preparation technology, and it is difficult to meet the above requirements with ordinary experimental methods.
Therefore, the preparation of ultrafine high-purity hafnium powder is a very difficult and challenging work

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Hafnium oxide with a purity of 99.9% and a particle size of less than 1mm and reducing agent powder CaH with a purity of more than 98.9% and a particle size of less than 2mm 2 , mixed evenly according to the molar ratio of 1:1, and loaded into a molybdenum crucible. Put the crucible into the reaction tank, cover it and then evacuate to 0.01Pa, wash with argon, heat to 800°C for 0.5 hours, and protect with argon. After constant temperature at 950°C for 5 hours, vacuumize at 800°C for 10 hours, then fill with argon to a slight positive pressure, and cool under the protection of argon. The reaction product was washed 15 times with 0.2M hydrochloric acid at room temperature, then washed once with deionized water at room temperature, and the resulting product was sieved to obtain hafnium powder. The quality of the final hafnium powder was: the purity of hafnium powder was 99.99%. The total content is less than 100ppm, the oxygen content is less than 0.2%, and the average pa...

Embodiment 2

[0032] Hafnium oxide with a purity greater than 99.9% (particle size less than 1mm) and a reducing agent LiH with a purity greater than 98.9% and a particle size less than 2mm are uniformly mixed at a molar ratio of 1:1 and loaded into a tantalum crucible. Put the crucible into the reaction tank, cover it, vacuumize to 0.03Pa, wash with argon, heat to 1400°C for 10 hours, and protect with argon. After constant temperature at 1400°C for 0.5 hours, vacuumize at 1400°C for 0.5 hours, then fill with argon to a slight positive pressure, and cool under the protection of argon. The reaction product was washed 15 times with 10M hydrochloric acid at 70°C, and then washed 15 times with deionized water at 100°C, and the product obtained was sieved to obtain hafnium powder. The content is 95ppm, the oxygen content is 0.2%, and the particle size is less than 0.8μm.

Embodiment 3

[0034] Mix hafnium oxide with a purity greater than 99.9% (particle size less than 1 mm) and Ca reducing agent powder with a purity greater than 99% and particle size less than 2 mm according to a molar ratio of 1:6, and put them into a hafnium crucible. Put the crucible into the reaction tank, cover it and then evacuate to 0.05Pa, wash with argon, heat to 1000°C for 10 hours, and protect with argon. After that, keep the temperature at 1000°C for 0.5 hours, then vacuumize for 10 hours, then fill it with argon to slightly positive pressure, and cool under the protection of argon. The reaction product was washed 10 times with 0.2M nitric acid at room temperature, then washed 15 times with 50°C deionized water, and the obtained product was sieved to obtain the final quality of metal hafnium: the purity of hafnium powder was 99.99%, and the metal impurities The total content is 80ppm, the oxygen content is less than 0.2%, and the average particle size is 0.9μm.

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Abstract

The invention relates to superfine high-purity hafnium powder as well as a preparation method and an application thereof. The grain size of the superfine high-purity hafnium powder is less than 1 micron; the purity reaches above 99.99%; the total content of metal impurities is less than 100ppm; and the oxygen content is less than 0.2%. The preparation method comprises the following steps: a) uniformly mixing hafnium oxide powder with reducing agent powder at a molar ratio of 1:1 to 1:6, and filling a mixture into a crucible; b) placing the crucible into a reaction tank, covering with a cover, then vacuumizing, filling argon for washing, heating and reducing, and performing constant-temperature insulation reduction; c) vacuumizing, filling argon again, and cooling under the argon protection; and d) washing: firstly, washing with an acid, then washing with deionized water, and screening and drying the obtained product, thereby obtaining the product of the superfine high-purity hafnium powder. The oxide generated by the method provided by the invention is capable of protecting hafnium powder, is anti-explosion and is safe and controllable.

Description

technical field [0001] The invention relates to a superfine high-purity hafnium powder and its preparation method and application, in particular to a superfine hafnium powder that can be widely used in the fields of atomic energy industry, information industry, bioengineering, military science, medical field, petrochemical industry, aerospace and aviation, etc. The preparation method of fine high-purity hafnium powder. Background technique [0002] Hafnium is a bright silver-white metal. Pure hafnium is plastic, easy to process, high temperature resistant, and corrosion resistant. It is an important material for the atomic energy industry. Hafnium has a large thermal neutron capture cross-section (115b), which can absorb thermal neutrons of nuclear reactors and control the reaction speed of the reactor, and is used for control rods and protection devices of atomic reactors. Hafnium powder can be used as a propeller for rockets; in the electrical industry, hafnium powder can...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/20C22B34/10
Inventor 王力军黄永章江洪林罗远辉张力陈松郎书玲车小奎
Owner 有研资源环境技术研究院(北京)有限公司
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