Method for preparing rare earth-gadolinium alloy by adopting co-deposition method

A gadolinium alloy and co-deposition technology, applied in the field of rare earth pyrometallurgy, can solve the problems of no research on the preparation of multi-element alloys, large distribution fluctuations, slag formation, etc., and achieve suitable for large-scale production, stable product composition, and simple process flow Effect

Active Publication Date: 2014-07-16
BAOTOU RES INST OF RARE EARTHS
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

But at the same time, there are also the following defects: the distribution of rare earth and iron in the alloy fluctuates greatly, it is difficult to control, and the distribution error is as high as 3%-5%, which affects the consistency of the product
Serious slag formation in the electrolysis process affects the further reduction of production costs
And it cannot be produced in large electrolytic furnaces such as 10000A, and the product consistency is extremely poor
Moreover, since the iron cathode is self-consumable and the cathode is frequently replaced during production, the labor intensity of the employees increases
At the same time, since the above-mentioned patents are all about the preparation of binary master alloys for NdFeB, no research has been done on the preparation of multi-element alloys

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The electrolyte ratio is praseodymium neodymium fluoride: gadolinium fluoride: lithium fluoride = 6.4: 0.6: 1 (weight ratio), and the raw material ratio is praseodymium neodymium oxide: gadolinium oxide = 11.8: 1 (weight ratio). Conduct electrolysis in a 300A electrolytic furnace, the electrolysis current intensity is 300A, and the cathode current density is 8A / cm 2 , the anode current density is 1.1A / cm 2 , the electrolysis time was 240min, the amount of mixed oxide added was 2.14kg, the electrolysis temperature was 1050°C, and the weight of the praseodymium neodymium gadolinium alloy obtained by electrolysis was 1.38kg. The alloy composition analysis results are as follows:

[0017] (mass fraction, %)

[0018] Pr Nd Gd C 22.7 68.3 8.9 0.037

Embodiment 2

[0020] The electrolyte ratio is praseodymium neodymium fluoride: gadolinium fluoride: lithium fluoride = 5.2: 1.6: 1 (weight ratio), and the raw material ratio is praseodymium neodymium oxide: gadolinium oxide = 3.9: 1 (weight ratio). Carry out electrolysis in a 300A electrolytic furnace, the electrolysis current intensity is 300A, and the cathode current density is 10A / cm 2 , the anode current density is 1.1A / cm 2 , electrolyzed for 240min, the amount of mixed oxide added was 2.14kg, and the electrolysis temperature was 1050°C. The alloy composition analysis results are as follows:

[0021] (mass fraction, %)

[0022] Pr Nd Gd C 19.8 60.2 19.9 0.035

Embodiment 3

[0024] The electrolyte ratio is neodymium fluoride: gadolinium fluoride: lithium fluoride = 6: 0.8: 1 (weight ratio), and the raw material ratio is neodymium oxide: gadolinium oxide = 12: 1 (weight ratio). Carry out electrolysis in a 300A electrolytic furnace, the electrolysis current intensity is 300A, and the cathode current density is 10A / cm 2 , the anode current density is 1A / cm 2 , electrolyzed for 240min, the amount of mixed oxide added was 1.5kg, the electrolysis temperature was 1040°C, and the weight of praseodymium neodymium gadolinium alloy was obtained by electrolysis was 0.98kg. The alloy composition analysis results are as follows:

[0025] (mass fraction, %)

[0026] Nd Gd C 90.8 9.1 0.034

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Abstract

The invention relates to a method for preparing a rare earth-gadolinium alloy by adopting a co-deposition method. The method is characterized by comprising the following steps: by taking a graphite block as an anode, a molybdenum rod as an inert cathode and a molybdenum crucible as a praseodymium-neodymium-gadolinium alloy acceptor, adding an electrolytic raw material into a fluoride molten salt electrolyte system containing rare earth fluoride, gadolinium fluoride and lithium fluoride the weight ratio of which is (6-3):(1.5-7):1, wherein the electrolytic raw material is a rare earth oxide and gadolinium fluoride mixture, and according to the weight percent, the rare earth oxide and gadolinium fluoride are respectively (99-35)% and (1-65)%; leading to direct current, wherein the current density of the anode is 0.5-2.0A/cm<2>, and the current density of the cathode is 5-25A/cm<2>; and electrolyzing at the electrolysis temperature of 1030DEG C-1200DEG C to obtain a rare earth-gadolinium alloy. The method has the advantages that the rare earth-gadolinium alloy is prepared by electrolyzing mixed oxides through the simple fluoride electrolyte system, so that the technological flow is simple, the cost is low, the ingredients of the product are stable, only CO2 and less CO are generated in the technological processes, so that the method is less in environmental pollution, is a green and environment-friendly technology and is suitable for large-scale production.

Description

technical field [0001] The present invention relates to a method for preparing rare earth gadolinium alloy by co-deposition method, in particular to a method for preparing rare earth gadolinium alloy by electrolytic co-deposition of oxide molten salt in fluoride system. Pyrometallurgy field. Background technique [0002] There are several methods for preparing rare earth metals and alloys with high melting point: (1) two kinds of metals mixed with each other; (2) thermal reduction method; (3) using a consumable solid cathode to precipitate rare earth metals on its surface by electrolysis and then Electrochemical method of alloying; (4) Electrochemical method of alloying through eutectoid electrolysis of mixed oxides using an inert cathode. In comparison, the fourth method is more superior than the first three methods, it does not need to prepare rare earth metals first, does not require high-cost reducing agents and complicated equipment, and does not require consumable cat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25C3/36
Inventor 张志宏陈国华于兵李坤曹永存刘玉宝赵二雄陈宇昕杨胜岭王荣温永清
Owner BAOTOU RES INST OF RARE EARTHS
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