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Microwave preparation method of lanthanum-cerium-terbium oxide fluorescent powder

A technology of terbium oxide and fluorescent powder, which is applied in the field of preparation of rare earth oxides. It can solve the problems of difficulty in obtaining products with uniform composition, poor crystal growth particle size, and difficulty in controlling the shape, so as to achieve easier control of shape growth and lower surface charge. Good consistency of sex and shape

Active Publication Date: 2020-04-24
GUANGXI ACAD OF SCI +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lanthanum cerium terbium oxide is a main three-color fluorescent material. The traditional preparation method is to form lanthanum cerium terbium oxalate by co-precipitation of lanthanum cerium terbium salt solution and oxalic acid solution, and then use lanthanum cerium terbium oxalate as the precursor Lanthanum cerium terbium oxide is obtained by burning at high temperature for 5-7 hours. In order to control the growth of the crystal form, various additives are added to it to help control the growth of the crystal form; research shows that lanthanum cerium terbium oxalate The morphology of lanthanum, cerium and terbium oxides has a great influence on the morphology of lanthanum, cerium and terbium oxides; at the same time, high-temperature solid-phase methods are often used for preparation. When burning at high temperatures, the heat transfer is from the surface to the inside, which is easy to cause The grain size of crystal growth is poor, the morphology is difficult to control, and it is difficult to obtain products with uniform composition
At present, most of the lanthanum, cerium and terbium oxides sold on the market are hexagonal columnar particles, with different particle sizes, uneven shapes, and too many gaps, resulting in poor luminous efficiency and poor performance.

Method used

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  • Microwave preparation method of lanthanum-cerium-terbium oxide fluorescent powder

Examples

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Effect test

Embodiment 1

[0026] A microwave preparation method of lanthanum cerium terbium oxide fluorescent powder, comprising the following steps,

[0027] (1) The lanthanum cerium terbium salt solution is mixed to obtain a raw material solution, the ion concentration ratio in the raw material solution is lanthanum: cerium: terbium = 5:2.5:2, and the concentration of rare earth metal ions is 0.8mol / L; The ratio of 1:4 is dissolved and mixed with water evenly as a precipitant;

[0028] (2) Use water as the bottom liquid, preheat the raw material liquid, precipitant, and bottom liquid to 55°C before use, and add PAMMA polyacrylate in the bottom liquid as a surface additive;

[0029] (3) Under the action of ultrasonic waves and stirring, the raw material liquid and the precipitant are added dropwise to the bottom liquid twice respectively, and the ratio of the added substances of the raw material liquid and the precipitant is raw material liquid: precipitant = 1:2; When adding the raw material solutio...

Embodiment 2

[0032] A microwave preparation method of lanthanum cerium terbium oxide fluorescent powder, comprising the following steps,

[0033] (1) The lanthanum cerium terbium salt solution is mixed to obtain a raw material solution, the ion concentration ratio in the raw material solution is lanthanum: cerium: terbium = 5:2:2, and the rare earth metal ion concentration is 0.7mol / L; Dissolve and mix with water at a ratio of 1:3 as a precipitant;

[0034] (2) Use ethanol as the base solution, preheat the raw material solution, precipitant, and base solution to 50°C before use, and add SDBS sodium dodecylbenzenesulfonate to the base solution as a surface additive;

[0035] (3) Under ultrasonic action and stirring, the raw material solution and the precipitant are added dropwise to the bottom solution twice respectively, and the ratio of the amount of the added substance between the raw material solution and the precipitant is raw material solution:precipitant=1:2.5; When adding the raw m...

Embodiment 3

[0038] A microwave preparation method of lanthanum cerium terbium oxide fluorescent powder, comprising the following steps,

[0039] (1) Mix the lanthanum, cerium and terbium salt solution to obtain a raw material solution, the ion concentration ratio in the raw material solution is lanthanum: cerium: terbium = 5:3:2, and the concentration of rare earth metal ions is 0.6mol / L; Dissolve and mix with water at a ratio of 1:3 as a precipitant;

[0040] (2) Water and ethanol are used as the bottom liquid, the volume ratio of water and ethanol is water: ethanol = 1:1.5, the raw material liquid, precipitant, and bottom liquid are preheated to 60°C before use, and CTAB sixteen is added to the bottom liquid Alkyltrimethylammonium bromide as a surface additive;

[0041](3) Under the action of ultrasonic waves and stirring, the raw material solution and the precipitating agent are respectively added dropwise to the bottom liquid twice, and the ratio of the amount of substances added bet...

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Abstract

The invention discloses a microwave preparation method of lanthanum-cerium-terbium oxide fluorescent powder, which comprises the following steps: taking oxalic acid, oxalate or ammonium bicarbonate asa precipitant; taking water and / or ethanol as a base solution, and adding a surface additive into the base solution; dropwise adding the raw material solution and a precipitant into the base solutionin twice under the action of ultrasonic waves and stirring, and aging, filtering and drying the obtained precipitate to obtain a lanthanum-cerium-terbium co-precipitate; putting the lanthanum-cerium-terbium co-precipitate into a microwave reactor for microwave heating; wherein the microwave power is 1-10 kW, the microwave heating frequency is 433-5900+ / -50 MHz, a microwave output mode comprises one or a combination of continuous waves and pulse waves, the working time is 12-60 min, and performing heat preservation for 1-2 h to obtain the lanthanum-cerium-terbium oxide. The lanthanum-cerium-terbium oxide prepared by the method is consistent in particle size and uniform in morphology.

Description

technical field [0001] The invention relates to the field of preparation of rare earth oxides, in particular to a microwave preparation method of fluorescent powder of lanthanum cerium terbium oxide. Background technique [0002] The luminous intensity, luminous efficiency and resolution of the fluorescent material have a great relationship with the morphology of the phosphor powder. The higher the sphericity of the phosphor powder morphology, the better the luminous performance of the phosphor particles. Lanthanum cerium terbium oxide is a main three-color fluorescent material. The traditional preparation method is to form lanthanum cerium terbium oxalate by co-precipitation of lanthanum cerium terbium salt solution and oxalic acid solution, and then use lanthanum cerium terbium oxalate as the precursor Lanthanum cerium terbium oxide is obtained by burning at high temperature for 5-7 hours. In order to control the growth of the crystal form, various additives are added to i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/229C01F17/235C01F17/206C09K11/78
CPCC09K11/7769C01P2004/61C01P2006/80
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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