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Method for preparing high-purity hafnium by calcium in-situ distillation-deoxidation

A high-purity, in-situ technology, applied in the field of metal smelting, can solve the problems of high energy consumption and pollution of hafnium products, and achieve the effects of reducing energy consumption, high solubility, and reducing activity

Inactive Publication Date: 2019-04-16
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

Benefits of technology

This patented new technique described in the patents allows for efficient separation of harmful elements such as iron and zinc without causing environmental concerns due to their presence. By combining these two substances together, it simplifies the treatment processes involved and eliminates any unnecessary waste. Additionally, the resulting highly pure crystal containing both Fe and Zn remains intact throughout the treated crude acid solution. Overall, this approach provides technical benefits over current methods like calcining/drying techniques and hydrothermal decomposition technologies.

Problems solved by technology

This technical problem addressed in this patented text relating to the challenge faced when producing highly refined or chemically stable nioblunium dioxides called zirconium dioxyde ("ZDO"), particularly if they contain significant amounts of iron impurity like hydroxyanions found within their crystal structure. Existing techniques involve either extractable solvents or expensive processes involving ion exchange resin columns. These solutions require complicated equipment and consume too much time on account of dissolved metal impursites.

Method used

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  • Method for preparing high-purity hafnium by calcium in-situ distillation-deoxidation

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Take 1 metal hafnium block, the mass is 20g, the oxygen content is 850ppm, press (CaCl 2): m(Hf)=5:1 Weigh 100g of anhydrous calcium chloride (dehydrated at 300°C for 24 hours before use), and weigh 4g of high-purity calcium chips (at 900°C, calcium in anhydrous calcium chloride molten salt 0.5 times the saturation solubility), metal hafnium and anhydrous calcium chloride are filled in the hafnium crucible, 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. Specific as attached figure 1 shown.

[0036] 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 with argon. Under argon protection, heat up to 900°C at 5°C / min, and keep at 900°C for 40 hours. After the heat preservation is over, the furnace is cooled to room temperature. After coming ...

Embodiment 2

[0038] Take 1 metal hafnium block, with a mass of 20g and an oxygen content of 760ppm, press (CaCl 2 ): m(Hf)=20:1 Weigh 400g of anhydrous calcium chloride (dehydrated at 300°C for 36h before use), weigh 57g of industrial calcium chips (at 1050°C, calcium saturated in anhydrous calcium chloride molten salt 2 times the solubility), metal hafnium and anhydrous calcium chloride 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, specifically as follows attached figure 1 shown.

[0039] Put the sealed crucible into a vacuum tank heated by a resistance furnace, cover the furnace cover, vacuumize to 0.1Pa, and then wash with argon. Under argon protection, heat up to 1050°C at 5°C / min, and keep at 1050°C for 20 hours. After the heat preservation is over, the furnace is cooled to room temperature. After...

Embodiment 3

[0041] Get 1 metal hafnium wire, quality 15g, oxygen content 910ppm, press (CaCl 2 ): m(Hf)=40:1 Weigh 600g of anhydrous calcium chloride (dehydrated at 400°C for 19h before use), weigh 213g of industrial calcium chips (at 1100°C, calcium saturated in anhydrous calcium chloride molten salt 4 times of the solubility), metal hafnium and anhydrous calcium chloride 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, specifically as follows attached figure 1 shown.

[0042] Put the sealed crucible into a vacuum tank heated by a resistance furnace, cover the furnace cover, vacuumize to 0.2Pa, and then wash with argon. Under the protection of argon, heat up to 1100°C at 5°C / min, and keep at 1100°C for 14 hours. After the heat preservation is over, the furnace is cooled to room temperature. After coming...

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Abstract

The invention discloses a method for preparing high-purity hafnium by calcium in-situ distillation-deoxidation, and belongs to the technical field of metal smelting. The method comprises the followingsteps: raw material systems A and calcium reducing agents are separately placed in a closed reaction container for heating under an inertia atmosphere; calcium in the calcium reducing agents is dissolved in a high-purity calcium gas form to enter fused salt of the raw material systems A to realize deoxidation of hafnium raw materials to prepare high-purity hafnium with an oxygen content of not more than 0.10 wt%; the raw material systems A are mixtures of the hafnium raw materials and anhydrous calcium chloride; the raw material systems A contain or dose not contain one or two of alkali metalhalides and alkaline earth metal halides; the hafnium raw materials are metal hafnium, hafnium alloys or hafnium oxide; the calcium reducing agents are metal calcium or calcium alloys; and separatedareas for separate placement are isolated and in gas-phase communication. The method is simple and feasible and excellent in oxygen removing effect, and can meet the use requirements in such fields ashigh-purity metal hafnium film plating materials, dielectric materials, high-temperature alloys and atomic energy industry.

Description

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Claims

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Application Information

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Owner 有研资源环境技术研究院(北京)有限公司
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