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Preparation method of Tb-Fe, Dy-Fe and Tb-Dy-Fe alloys employing electro-deoxidization

A technology of electrodeoxidation and ferroalloy, applied in the field of dysprosium-iron and terbium-dysprosium-iron alloy, electrodeoxidation to prepare terbium-iron, can solve the problems of complex alloy composition, high impurity content, difficult to meet, etc., and achieve high product quality, simple process and low cost Effect

Active Publication Date: 2010-12-08
江苏江南铁合金有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Due to the shortcomings of traditional preparation methods such as high energy consumption, complex alloy composition, high impurity content, environmental pollution, and complicated process, it is difficult to meet the requirements for high-quality, low-energy consumption products under the conditions of today's energy shortage.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 100 grams of Dy with a purity ≥99.999% 2 o 3 Add 20 grams of iron powder with a purity of ≥99.999% (you can also mix dysprosium and iron according to objective requirements), briquetting at 120Mpa, normal pressure, anaerobic protective atmosphere, and sintering at 1200°C for 6 hours to make a cathode. Place the cathode in a graphite electrolyzer; NaCl-CaCl 2 (Purity ≥ 99.999%) Mix 50 grams according to the molar ratio of 1:1, dehydrate to make electrolyte, put it in the electrolytic cell; heat it up to 650°C, after the electrolyte melts, insert the graphite electrode into the molten salt, 0.2cm away from the cathode block , electrolyze with a voltage of 3.4V until the current is lower than 1.0 ampere to end the reaction, take out the cathode and put it in a vacuum induction furnace to remelt the ingot. Through detection and analysis, the purity of the product dysprosium-iron alloy is over 99.99%.

Embodiment 2

[0026] 100 grams of Tb with a purity ≥99.999% 4 o 7 Add 15 grams of iron powder with a purity of ≥99.999% and 10 grams of Fe with a purity of ≥99.999% 2 o 3 Powder (proportioning dysprosium and iron can also be based on objective requirements), briquetting under 160Mpa, normal pressure, oxygen-free protective atmosphere, sintering at 1400°C for 4 hours to make a cathode, and placing the cathode in a graphite electrolytic cell; NaCl- CaCl 2 (Purity ≥ 99.999%) Mix 50 grams according to the molar ratio of 1:1, dehydrate to make electrolyte, put it in the electrolytic cell; heat it up to 650°C, after the electrolyte melts, insert the graphite electrode into the molten salt, 0.2cm away from the cathode block , electrolyze with a voltage of 3.4V until the current is lower than 1.0 ampere to end the reaction, take out the cathode and put it in a vacuum induction furnace to remelt the ingot. Through detection and analysis, the purity of the product terbium-iron alloy is over 99.99...

Embodiment 3

[0028] 100 grams of Tb with a purity ≥99.9999% 4 o 7 Powder and 100g purity ≥99.999% Dy 2 o 3 The powder is made by adding 40 grams of iron powder with a purity of ≥99.9999% (terbium, dysprosium and iron can also be mixed according to objective requirements), briquetting at 180Mpa, normal pressure, anaerobic protective atmosphere, and sintering at 1400 ° C for 4 hours Cathode, place the cathode in a graphite electrolyzer; NaCl-CaCl 2(Purity ≥ 99.9999%) Mix 100 grams according to the molar ratio of 1:1, dehydrate to make an electrolyte, put it in an electrolytic cell; heat it up to 650°C with electricity, after the electrolyte melts, insert the graphite electrode into the molten salt, 0.2cm away from the cathode block , electrolyze with a voltage of 3.4V until the current is lower than 1.0 ampere to end the reaction, take out the cathode and put it in a vacuum induction furnace to remelt the ingot. Through detection and analysis, the purity of the product terbium-dysprosium...

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Abstract

The invention relates to a preparation method of Tb-Fe, Dy-Fe and Tb-Dy-Fe alloys employing electro-deoxidization, comprising the following steps: adopting metal chloride or a mixture of metal chlorides as electrolyte of which the melting point is less than 800 DEG C, using carbon material or inert electrode as anode and the solid compound of Tb or Dy as cathode, placing the cathode and the electrolyte in a graphite electrolysis cell, heating by electrifying, inserting the anode in molten salt after melting the electrolyte to perform electro-deoxidization reaction under the conditions that the adopted voltage is more than the decomposition voltages of Tb4O7 and Dy2O3 and less than the decomposition voltage of the electrolyte, the interelectrode distance is not less than 0.1cm and the temperature is not more than 800 DEG C, completing the reaction when the electric current is less than 1.0A, then taking the cathode out to place in a vacuum induction furnace and perform remelting and ingoting. The new electrochemical method adopted in the invention for preparing Tb-Fe, Dy-Fe and Tb-Dy-Fe alloys has the advantage of simple process, low energy consumption, high quality of the preparedproduct, less impurity, low cost and environmental friend and the purity of the prepared Tb-Fe, Dy-Fe and Tb-Dy-Fe alloys is 99-99.9999%.

Description

technical field [0001] The invention relates to the technical field of preparing rare earth metals by electrodeoxidation, in particular to a method for preparing terbium-iron, dysprosium-iron and terbium-dysprosium-iron alloys by electrodeoxidation. Background technique [0002] High-purity dysprosium-iron and terbium-dysprosium-iron alloys are the best raw materials for producing magnetostrictive materials. People are more eager to obtain high-purity alloy materials, especially for the manufacture of high-performance magnetostrictive materials. At present, the common preparation methods include oxide or fluorine (chloride) compound direct reduction-fusion method and molten salt electrolysis method. [0003] Oxide or fluorine (chloride) compound direct reduction-fusion method: Dy 2 o 3 or Dy 2 o 3 Fluoride (chlorine) is produced by fluorine (chlorination), and pure metal dysprosium (Dy) is prepared by vacuum high-temperature calcium (magnesium) heat reduction, and then ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25C3/36
Inventor 翟玉春梅泽锋王伟梅平顾惠敏包岩谢宏伟林一飞
Owner 江苏江南铁合金有限公司