Method for preparing refractory active metal or alloy

An active metal and refractory technology, applied in the field of metallurgy of rare earth metals, heavy rare earth metals and their alloys, can solve the problems of electrochemically polarized small metals, achieve short production processes, reduce energy consumption, and avoid secondary The effect of secondary electrolysis

Inactive Publication Date: 2006-09-27
WUHAN UNIV +1
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

However, the difference between the decomposition voltage of heavy rare earth oxides or oxychlorides and the decomposition voltage of calcium oxide is only 20-50mV, and the deposition of calcium will inevitably occur at the same time when electrolytically reducing solid hea

Method used

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  • Method for preparing refractory active metal or alloy
  • Method for preparing refractory active metal or alloy
  • Method for preparing refractory active metal or alloy

Examples

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Example Embodiment

[0043] Example 1

[0044] Tb with a purity of 99.99% 4 O 7 The powder is mixed with water, pressed into a block at 2-5MPa, and sintered in air at 1000°C for 1-4 hours. The porosity of the sample is 30-48%. figure 1 ). Weigh 5-10g of sintered body, place it in the molybdenum / tungsten / tantalum basket, and reduce to CaCl 2 The melt is used as the cathode, and the graphite crucible is used as the anode. In an argon atmosphere, the cell pressure is controlled to 3.4V at 900°C, and the electrolysis is carried out for 5-18 hours. The electrolysis product can be melted in a vacuum to remove the salt attached to the product. The impurity CaCl in the product can also be washed away by dimethyl sulfoxide 2 . After the electrolysis product is cleaned with dimethyl sulfoxide solvent, use SEM ( figure 2 ) Observe its morphology and EDAX analysis composition ( image 3 ), confirming that the spongy rare earth metal terbium was obtained by electrolysis.

Example Embodiment

[0045] Example 2

[0046] Dy with a purity of 99.9% 2 O 3 The powder is mixed with water, pressed into a block under 2MPa, and sintered in air at 700°C for 5 hours, and the porosity of the sample is 50-60%. Weigh 5-10g of sintered body and place it in a molybdenum / tungsten / tantalum basket as a cathode in CaCl 2 -In the NaCl mixed melt, graphite rods are used as anodes. In an argon atmosphere, the cell pressure is controlled to 4.5V at 650°C for electrolysis for 5-18 hours. The electrolysis product was confirmed to be Dy metal element ( Figure 4 ), the oxygen content is 1000~5000ppm.

Example Embodiment

[0047] Example 3

[0048] Tb with a purity of 99.99% 4 O 7 Powder with 10wt% NH 4 HCO 3 Fully mix, press into a block at 2-5MPa, pre-fire at 300°C for 1-3 hours in air, and then heat up to 1000°C for sintering for 2-4 hours to obtain a sample with a porosity of 65-75%. With CaCl at 600℃ 2 +LiCl mixed molten salt titanium crucible, bound Tb with molybdenum wire 4 O 7 The powder sintered block was used as the cathode and graphite was used as the anode. The electrolysis was carried out in an argon atmosphere at a controlled voltage of 4.2V for 8-16 hours. The electrolyzed product was taken out and washed with dimethyl sulfoxide. The analysis confirmed that pure metal terbium was obtained.

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Abstract

This invention relates to a method for preparation of refractory active metals or alloys, which comprises the following steps: selecting CaCl2 or mixed salt electrolyte mainly including CaCl2 as flux, coining or perfusing refractory active metals to be block-shaped, sintering them to get sintered cake, compounding sintered cake and liquid of conductive cathode group and making them as cathode, making graphite or inert electrode as anode; making electrolyzation voltage no lower than academic decomposition voltage of melted salt, and making electrochemical reduction carryed out on cathode, but not forming compact sedimentary deposit to prevent the touch of compounds and electrolyte, controlling electrolyzation temperature at 500-1000 degrees, controlling the electrolyzation time according to 1-4 times theoretical electrical energy demand, making sure inert atmosphere in electrolytic process; then getting refractory metals or alloys which is electrolyzation product. The invention has short flow of production, low energy consumption, little contamination, and is easy to product continuously.

Description

technical field [0001] The invention relates to a method for electrolytically refining refractory active metals and alloys from refractory active metal compounds, which is particularly suitable for the extraction of heavy rare earth metals and their alloys, and belongs to metallurgy of rare earth metal materials. Background technique [0002] Rare earth metals are important raw materials for magnetic materials, and various new magnetic functional alloys (such as permanent magnets, magnetostrictive, magneto-optical recording materials, etc.) composed of heavy rare earth metals and iron-based metals have been more and more widely used. At present, there are two methods for preparing heavy rare earth metals: metallothermic reduction and reduction-distillation. These methods require the use of pure active metal reducing agents and are carried out in an oxygen-free environment. Usually, the oxides need to be chlorinated or fluorinated in advance. The process is complicated, the p...

Claims

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Application Information

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IPC IPC(8): C25C3/26C25C3/34C25C3/36
Inventor 汪的华陈政邱国红金先波
Owner WUHAN UNIV
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