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Preparation method for dysprosium oxide powder

A technology of dysprosium oxide and powder, which is applied in the field of rare earth powder material preparation, can solve the problems of high environmental protection pressure, high production cost, uneven powder dispersion, etc., and achieve the effect of narrow particle size distribution, low environmental protection pressure and simple control

Active Publication Date: 2018-12-11
FUJIAN CHANGJIANG GOLDEN DRAGON RARE EARTH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The alkoxide hydrolysis method firstly prepares the metal alkoxide compound, then undergoes a hydrolysis reaction, then treats it with an organic reagent, and then burns it. Because the organic reagent is used in the treatment process, the production cost is high, and the pollution is serious, which is not conducive to industrial implementation.
The microemulsion method is that two immiscible solvents form an emulsion under the action of a surfactant, and obtain nanoparticles after nucleation, coalescence, agglomeration, and heat treatment in the microbubbles. The method has high post-processing costs and low yields. , Environmental pressure and other issues
The precipitation method is currently the most widely used method in the preparation of nano-powders. Usually, the forward precipitation method is used, that is, the precipitant is added to the metal salt solution to react to form a solid, and then the nano-powder is obtained by burning. However, it is found during production that When preparing nano-rare earth oxide powder, the powder is unevenly dispersed and agglomerated seriously, which is not conducive to the application of back-end products

Method used

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  • Preparation method for dysprosium oxide powder
  • Preparation method for dysprosium oxide powder
  • Preparation method for dysprosium oxide powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1) Prepare dysprosium-containing material liquid, the acidity and dysprosium chloride concentration of the dysprosium-containing material liquid are shown in Table 1;

[0038] 2) Take sodium carbonate and composite dispersant to form a mixed solution of deionized water. The composite dispersant is composed of citric acid and polyacrylic acid. The concentrations of sodium carbonate, composite dispersant and citrate in the mixed solution of deionized water are as shown in Table 1. Show

[0039] 3) While stirring the deionized water mixed solution, drip the dysprosium-containing material liquid at a rate of 30ml / min per liter of the deionized water mixed solution until the amount of dysprosium chloride in the dysprosium-containing material liquid is equal to that of the sodium carbonate material. The volume ratio is 1:1, the reaction temperature is controlled to 40°C, and the reaction solution is filtered to obtain a white precipitate; at this time, the pH of the reaction solut...

Embodiment 2

[0044] 1) Prepare dysprosium-containing material liquid, the acidity and dysprosium nitrate concentration of the dysprosium-containing material liquid are shown in Table 2;

[0045] 2) Take ammonium carbonate and a composite dispersant to form a mixed solution of deionized water. The composite dispersant is composed of ammonium citrate and polyvinyl alcohol with a purity of 95%. In the mixed solution of deionized water, ammonium carbonate, composite dispersant and lemon The acid radical concentration is shown in Table 2;

[0046] 3) While stirring the deionized water mixed solution, drip the dysprosium-containing material solution at a rate of 40ml / min per liter of the deionized water mixed solution to the amount of dysprosium nitrate and ammonium carbonate in the dysprosium-containing material solution The ratio is 1:2.0, the reaction temperature is controlled at 45°C, and the reaction solution is filtered to obtain a white precipitate; at this time, the pH of the reaction solutio...

Embodiment 3

[0051] 1) Prepare dysprosium-containing material liquid, the acidity and dysprosium chloride concentration of the dysprosium-containing material liquid are shown in Table 3;

[0052] 2) Take ammonium bicarbonate and a composite dispersant to form a deionized water mixed solution. The composite dispersant is composed of citric acid and polyethylene glycol 2000. In the deionized water mixed solution, ammonium bicarbonate, composite dispersant and citrate The concentration is shown in Table 3;

[0053] 3) While stirring the deionized water mixed solution, drip the dysprosium-containing material liquid at a rate of 50ml / min per liter of the deionized water mixed solution until the amount of dysprosium chloride and ammonium bicarbonate in the dysprosium-containing material liquid The ratio of the amount is 1:1.6, the reaction temperature is controlled to 50°C, and the reaction liquid is filtered to obtain a white precipitate; at this time, the pH of the reaction liquid is acidic;

[0054...

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Abstract

The invention discloses a preparation method for dysprosium oxide powder. The preparation method comprises the steps that 1) a dysprosium-containing stock solution with the acidity of 0.03-1 mol / L andthe concentration of dysprosium chloride and / or dysprosium nitrate of 0.3-1 mol / L is prepared; 2) a deionized water mixed solution with the concentration of carbonate ions of 0.3-0.6 mol / L and the concentration of a composite dispersing agent of 0.0045-0.08 mol / L is prepared, wherein the composite dispersing agent comprises citrate ions with the concentration of 0.002-0.048 mol / L; 3) the dysprosium-containing stock solution is dropwise added into the deionized water mixed solution while stirring is carried out, the temperature of the reaction process is controlled to be 40-50 DEG C so as to obtain a white precipitate; and 4) the white precipitate is filtered, washed, dried and fired so as to obtain the dysprosium oxide powder. The dysprosium oxide powder prepared through the preparation method has the advantages of being small in particle size, low in apparent density, high in dispersion and less in agglomeration.

Description

Technical field [0001] The invention belongs to the field of preparation of rare earth powder materials, and particularly relates to a preparation method of dysprosium oxide powder. Background technique [0002] In addition to the chemical activity shared by rare earth elements, Dysprosium can be used as a miscellaneous rare earth metal and compound. It also has excellent optical, electrical and magnetic properties. It can be used to produce a variety of functional materials, and it is increasingly used in many high-tech fields. The more important the unique role. Dysprosium oxide is an indispensable material in MLCC ceramic capacitors. Since the coating of the ceramic capacitor itself is about 1.3μm, there are strict requirements on the particle size of dysprosium oxide and the uniformity of powder particle size. [0003] At present, the preparation technology of nano-rare earth oxide powder is divided into physical method and chemical method. [0004] The physical method generall...

Claims

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Application Information

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IPC IPC(8): C01F17/00B82Y30/00
CPCB82Y30/00C01P2004/64C01F17/206
Inventor 朱世清余建勇曾辉辉张榕贵赵德森
Owner FUJIAN CHANGJIANG GOLDEN DRAGON RARE EARTH CO LTD
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