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Method for synergistically and deeply removing oxygen in metal hafnium by super-oxyphilic metal and calcium

A metal removal technology, applied in metal processing equipment, transportation and packaging, etc., can solve the problems of easy fluctuation of deoxidation effect and easy increase of calcium oxide activity, and achieve the effect of simple and easy method and good removal effect.

Active Publication Date: 2020-12-18
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

[0008] In order to solve the above problems, the object of the present invention is to provide a method for super-oxophilic metal-calcium synergistically deep removal of oxygen in metal hafnium, which further improves the calcium deoxidation technology of metal hafnium by adding super-oxophilic metal, solving the existing Calcium oxide activity is easy to increase in calcium deoxidation technology, and the deoxidation effect is easy to fluctuate

Method used

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  • Method for synergistically and deeply removing oxygen in metal hafnium by super-oxyphilic metal and calcium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Get metal hafnium bar 10g, initial oxygen content 3250ppm, press (CaCl 2 ): m(Hf)=15:1 Add 150g of anhydrous calcium chloride (dehydrated at 500°C for 24 hours before use), add 25g of high-purity calcium chips (at 900°C, the saturated solubility of calcium in anhydrous calcium chloride molten salt 2.5 times of that), add high-purity yttrium wire 3g (30% of hafnium raw material quality), add potassium chloride 45g (30% of anhydrous calcium chloride quality), metal hafnium bar, anhydrous calcium chloride, chloride Potassium and high-purity yttrium wires are filled in the hafnium crucible, and high-purity calcium chips are filled in the gap between the hafnium crucible and the stainless steel crucible, and then the stainless steel crucible is sealed with a high-temperature sealing gasket. figure 1 shown.

[0039] Put the sealed crucible into a vacuum tank heated by a resistance furnace, cover the furnace cover, vacuumize to 0.04Pa, and then wash it with argon. Under the ...

Embodiment 2

[0041] Get metal hafnium powder 20g, initial oxygen content 1030ppm, press (CaCl 2 ): m(Hf)=18:1 Add 360g of anhydrous calcium chloride (dehydrated at 500°C for 24 hours before use), add 47g of distilled calcium chips (at 900°C, the saturation solubility of calcium in anhydrous calcium chloride molten salt 2 times), add high-purity sponge lutetium 4g (20% of hafnium raw material quality), add potassium chloride 36g (10% of anhydrous calcium chloride quality), metal hafnium powder, anhydrous calcium chloride, potassium chloride 1. High-purity sponge lutetium is filled in the hafnium crucible, and the distilled calcium chips are filled in the gap between the hafnium crucible and the stainless steel crucible, and then the stainless steel crucible is sealed with a high-temperature sealing gasket, as shown in the attached figure 1 shown.

[0042] Put the sealed crucible into a vacuum tank heated by a resistance furnace, cover the furnace cover, vacuumize to 0.5 Pa, and then wash w...

Embodiment 3

[0044] Get metal hafnium tube 27g, initial oxygen content 990ppm, press (CaCl 2 ): m(Hf)=20:1 Add 540g of anhydrous calcium chloride (dehydrated at 500°C for 24 hours before use), add 51g of industrial calcium chips (at 1000°C, the saturation solubility of calcium in anhydrous calcium chloride molten salt 1.5 times), add high-purity erbium plate 5g (2% of hafnium raw material quality), add potassium chloride 216g (40% of anhydrous calcium chloride quality), metal hafnium tube, anhydrous calcium chloride, potassium chloride 1. High-purity erbium plates are filled in the hafnium crucible, industrial calcium chips are filled in the gap between the hafnium crucible and the stainless steel crucible, and then the stainless steel crucible is sealed with a high-temperature sealing gasket, as shown in the attached figure 1 shown.

[0045] Put the sealed crucible into a vacuum tank heated by a resistance furnace, cover the furnace cover, vacuumize to 0.6 Pa, and then wash with argon. ...

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Abstract

The invention discloses a method for synergistically and deeply removing oxygen in metal hafnium by super-oxyphilic metal and calcium. The method comprises the following steps: filling specific positions of a reactor with materials such as super-oxyphilic metal, anhydrous calcium chloride, a hafnium raw material and a calcium reducing agent; and carrying out distillation-deoxidation and disassembly-cleaning so as to stably reduce the oxygen content of hafnium to be smaller than 100 ppm. The super-oxyphilic metal has extremely high oxygen affinity, and oxygen in calcium chloride fused salt canbe subjected to solid solution or forms oxide, so that extremely low oxygen potential is created, and the thermodynamic problem of deep deoxidation is solved; and the calcium chloride fused salt has high fluidity and high solubility to the calcium reducing agent and calcium oxide, so that the kinetics problem of deoxidation is solved. Through organic combination of purification and deoxidation ofCa, deep, efficient and stable removal of oxygen in the metal hafnium is realized. The method disclosed by the invention is simple and easy to implement, good in oxygen removal effect and free of secondary pollution, and the product meets the use requirements in the fields of target material manufacturing, optical coating, electronic element manufacturing and the like.

Description

technical field [0001] The invention belongs to the technical field of metal smelting, and in particular relates to a method for synergistically deep removal of oxygen from metal hafnium by a super-oxophilic metal-calcium. Background technique [0002] Metal hafnium is a silver-white metal with excellent properties such as high temperature resistance, corrosion resistance, and easy processing. It is an important material in the fields of atomic energy industry, aerospace, military science, biomedicine, and petrochemical industry. The thermal neutron absorption cross section of metal hafnium is as high as 115b. After fission, each generation product is still hafnium. The neutron absorption cross section of the isotope changes little, and does not produce long half-life gamma rays after irradiation. Metal hafnium also has excellent high temperature resistance Corrosion, oxidation resistance, radiation resistance, good machinability and other characteristics, it is a safe and e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/14C22B5/04B22F1/00
CPCC22B34/14C22B5/04B22F1/145
Inventor 王力军马朝辉张顺利张建东闫国庆吴延科齐申
Owner 有研资源环境技术研究院(北京)有限公司
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