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Method for preparing metal ytterbium by reduction distillation of ytterbium oxide raw material

A technology of ytterbium oxide and metal, which is applied in the field of vacuum metallurgical purification, can solve the problems of increased cost and unit consumption, low vacuum degree, etc., and achieve the effects of increased rare earth yield, uniform composition and stable operation

Active Publication Date: 2022-02-15
BAOTOU RES INST OF RARE EARTHS +1
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] High-purity metal ytterbium is widely used in various optoelectronic materials. Optoelectronic display materials require that the Cl content in metal ytterbium be less than 100PPM, and the Cl content in metal ytterbium obtained by direct reduction and distillation of pure ytterbium oxide raw materials with a Cl content as high as several hundred PPM It is usually 1.3-2 times of the Cl content in the raw material, far exceeding <100PPM; and because the Cl content in the raw material ytterbium oxide is high, the vacuum degree in the distillation process is low, resulting in a rare earth yield of metal ytterbium usually only 87-90%, and the cost Unit consumption will also increase

Method used

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Embodiment 2

[0032] Put the high-purity ytterbium oxide raw material with a Cl content of 310PPM into the molybdenum crucible in the vacuum furnace, seal it, raise the temperature to 600°C, keep it for 2 hours, raise the temperature to 800°C, keep it for 4 hours, finally raise the temperature to 1100°C, keep it for 8 hours, and cool to normal temperature; vacuum calcination effectively removes chloride impurities in the raw material, and at the same time increases the yield of rare earth.

[0033] Mix high-purity ytterbium oxide and lanthanum scraps in a certain proportion, briquette, put into a vacuum furnace, evacuate to 10Pa, heat up to 500°C for 30 minutes, hold for 120 minutes, heat up to 780°C, hold for 3 hours, heat up to 900°C for 30 minutes, Keep warm for 3 hours, raise the temperature to 1150°C in 30 minutes, keep warm for 10 hours, cut off the power for 120 minutes and drop to 600°C, turn off the mechanical pump, and cool to room temperature with argon gas.

[0034] Take metal s...

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Abstract

The invention discloses a method for preparing metal ytterbium by reduction distillation of ytterbium oxide raw material. The high-purity ytterbium oxide raw material with a chlorine content greater than 100PPM is put into a metal crucible, and the metal crucible is moved into a vacuum heating furnace. The temperature is below 10Pa, and the temperature is gradually raised to 1100-1200°C by staged heating and heat preservation methods for vacuum calcination; after the vacuum calcination is completed, the mechanical pump is turned off and cooled to room temperature; the vacuum heating furnace is removed from the metal crucible, and the vacuum calcined high-purity ytterbium oxide Briquette with lanthanum scraps and put them into a vacuum carbon tube furnace for reduction distillation; in a sealed environment, the vacuum degree is below 10Pa, the reduction distillation adopts the method of heating up, keeping warm, and cooling down in stages, and metal lanthanum reduces ytterbium oxide to metal ytterbium, The ytterbium metal is distilled and condensed in the receiver. The content of Cl in the metal ytterbium obtained by the invention is less than 100PPM, and the yield of rare earth is greatly increased.

Description

technical field [0001] The invention belongs to vacuum metallurgical purification technology, in particular to a method for preparing metal ytterbium by reduction distillation of ytterbium oxide raw material. Background technique [0002] Rare earth elements are widely used in functional materials due to their unique 4f electron shell structure, and the purity of rare earth elements is an important factor affecting their functions. Ytterbium is one of the rare earth elements, the mass fraction in the earth's crust is only 0.00026%, and the mass fraction of cerium is 0.0046%. The mass fraction of ytterbium in the earth's crust is only 5.65% of that of cerium, roughly equivalent to that of dysprosium, about 60% of its mass fraction. The rare earth ytterbium has excellent photoelectric properties, and the sustainable development of its resource utilization is of great significance in the process of building a powerful manufacturing country in my country. Strengthening the rese...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B5/04C22B5/16C22B59/00
CPCC22B5/04C22B5/16C22B59/00
Inventor 张先恒刘玉宝赵二雄苗旭晨陈国华刘冉
Owner BAOTOU RES INST OF RARE EARTHS