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Microwave calcination preparation method of dysprosium oxide nano-powder

A technology of nano-powder and dysprosium oxide, which is applied in the field of rare earths, can solve problems such as difficult preparation of nano-powder, and achieve the effects of uniform size, uniform heat conduction, and high specific surface area

Pending Publication Date: 2020-08-14
GUANGXI ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the high-temperature solid-phase method is mostly used for the preparation of dysprosium oxide. The particle size of the prepared dysprosium oxide powder is relatively large, between 3-10 μm. Through strict requirements on the process conditions, the particle size can be reduced to 1-2 μm. The main reason is that During the high-temperature heating and burning process, the particles are agglomerated due to uneven heating. At the same time, when preparing the precursor, because the surface of the finer precursor is higher, there will be a strong tendency to agglomerate, and it is difficult to prepare nano-powder. body

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A microwave calcination preparation method of dysprosium oxide nanopowder, comprising the following steps,

[0026] (1) surface treatment: get the dysprosium chloride solution that concentration is 1.5mol / L, adjust pH to be alkaline, add the stearic acid of 5% of the volume of dysprosium chloride solution, mix and stir to obtain the first solution;

[0027] (2) Grass sinking reaction: under the condition of stirring at a temperature of 50°C, add oxalic acid solution dropwise to the first solution at a volume ratio of 1.0 times;

[0028] (3) Aging: standing and aging for 5 hours after the reaction;

[0029] (4) Purification: the precipitate obtained by washing and filtering with pure water is dried to obtain a solid dysprosium oxalate precursor;

[0030] (5) Microwave calcination: Put the solid dysprosium oxalate precursor into a microwave reactor, and heat and calcine it by microwave at 800°C for 1 hour to obtain dysprosium oxide nanopowder; the frequency of microwave ...

Embodiment 2

[0032] A microwave calcination preparation method of dysprosium oxide nanopowder, comprising the following steps,

[0033] (1) surface treatment: get concentration and be the dysprosium chloride solution of 2.0mol / L, adjust pH to be alkaline, add 20% sodium dodecylbenzenesulfonate of dysprosium chloride solution volume, mix and stir to obtain the first solution;

[0034] (2) Grass sinking reaction: under the condition of stirring at a temperature of 70°C, add oxalic acid solution dropwise in the first solution at a volume ratio of 1.6 times;

[0035] (3) Aging: standing and aging for 10 hours after the reaction;

[0036] (4) Purification: the precipitate obtained by washing and filtering with pure water is dried to obtain a solid dysprosium oxalate precursor;

[0037] (5) Microwave calcination: put the solid dysprosium oxalate precursor into a microwave reactor, and heat and calcine it by microwave at 1100°C for 3 hours to obtain dysprosium oxide nanopowder; the frequency of...

Embodiment 3

[0039] A microwave calcination preparation method of dysprosium oxide nanopowder, comprising the following steps,

[0040] (1) Surface treatment: take a dysprosium chloride solution with a concentration of 1.6mol / L, adjust the pH to be alkaline, add 8% polyethylene glycol by volume of the dysprosium chloride solution, mix and stir to obtain the first solution;

[0041] (2) Grass precipitation reaction: under the condition of stirring at a temperature of 60°C, add oxalic acid solution dropwise to the first solution at a volume ratio of 1.2 times;

[0042] (3) Aging: standing and aging for 6 hours after the reaction;

[0043] (4) Purification: the precipitate obtained by washing and filtering with pure water is dried to obtain a solid dysprosium oxalate precursor;

[0044] (5) Microwave calcination: Put the solid dysprosium oxalate precursor into a microwave reactor, and heat and calcine it by microwave at 900°C for 2 hours to obtain dysprosium oxide nanopowder; the frequency o...

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Abstract

The invention discloses a microwave calcination preparation method of dysprosium oxide nano-powder, which comprises the following steps: (1) surface treatment: taking a dysprosium chloride solution, regulating the pH value to greater than 7, adding a surface assistant accounting for 5-20% of the volume of the dysprosium chloride solution, and uniformly mixing and stirring to obtain a first solution, (2) grass precipitation reaction: dropwise adding an oxalic acid solution into the first solution according to a volume ratio of 1.0-1.6 times under a stirring condition, (3) aging: after the reaction is finished, carrying out standing aging, (4) purification: washing the precipitate obtained by filtration with pure water, and drying to obtain a solid dysprosium oxalate precursor, and (5) microwave calcination: putting the solid dysprosium oxalate precursor into a microwave reactor, and carrying out microwave heating calcination to obtain dysprosium oxide nano-powder. According to the preparation method, the surface additive is added in the preparation process, and meanwhile, a microwave heating calcining technology is adopted, so that the prepared dysprosium oxide nano-powder is fine and uniform in particle and large in specific surface area.

Description

technical field [0001] The invention belongs to the field of rare earths, and in particular relates to a microwave calcination preparation method of dysprosium oxide nanopowder. Background technique [0002] Dysprosium is used as a raw material for the production of dysprosium metal, as an additive for glass and NdFeB permanent magnets, and is also used in metal halide lamps, magneto-optical memory materials, yttrium-iron or yttrium-aluminum garnet, and in the atomic energy industry. Dysprosium oxide can also be used as an additive for NdFeB permanent magnets. Adding about 2 to 3% of dysprosium to this magnet can increase its coercive force. In the past, the demand for dysprosium was small, but with the development of NdFeB As the demand for magnets increases, it becomes a necessary added element, and the grade must be around 95-99.9%, and the demand is also increasing rapidly. Dysprosium oxide is also used as a raw material for making dysprosium metal, as an additive for g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/224B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01P2006/80C01P2004/64
Inventor 黄志民黄慨顾传君冼学权黄绍权黄华林
Owner GUANGXI ACAD OF SCI
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