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Method for preparing metal ytterbium by reducing and distilling ytterbium oxide raw material with high chlorine content

A technology of ytterbium oxide and raw materials, applied in the field of vacuum metallurgical purification, can solve the problems of increased cost per unit consumption, low vacuum degree, etc., and achieve the effects of improving the yield of rare earth, uniform composition and obvious removal

Active Publication Date: 2020-07-24
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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Effect test

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 reducing and distilling an ytterbium oxide raw material with high chlorine content. The method comprises the following steps: puttingthe high-purity ytterbium oxide raw material with chlorine content greater than 100 PPM into a metal crucible, transferring the metal crucible into a vacuum heating furnace, gradually heating up the metal crucible to a temperature of 1100-1200 DEG C to perform vacuum roasting in a staged heating-up and heat-preserving way under a sealing environment with vacuum degree lower than 10 Pa; switching off a mechanical pump after completing vacuum roasting, and cooling the metal crucible to the normal temperature; moving the metal crucible out of the vacuum heating furnace, and putting vacuum-roastedhigh-purity ytterbium oxide and lanthanum chip pressure blocks into a vacuum carbon tube furnace to reduce and distill; reducing ytterbium oxide into metal ytterbium by metal lanthanum in a staged heating-up, heat-preserving and cooling way for reducing and distilling under the sealing environment with the vacuum degree lower than 10 Pa, and distilling and condensing the metal ytterbium in a receiver. Cl content in the metal ytterbium obtained by the method is less than 100 PPM, and the rare-earth yield 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 with high chlorine content. 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 coun...

Claims

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Application Information

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Patent Type & Authority Applications(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
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