Co-precipitation method for preparing rare earth cerium ion-doped yttrium aluminum garnet fluorescent powder

A technology of yttrium aluminum garnet and ion doping, applied in chemical instruments and methods, luminescent materials, etc., can solve problems such as affecting the stability of fluorescence method, achieve precise control of chemical calculation, easy, reduce the chance of doping impurities, The effect of relative strength improvement

Inactive Publication Date: 2010-10-06
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The most important thing is that the product is relatively pure and has few impurities, but the high requirements for equipment and operation are the main factors that limit its wide application
For luminous bodies, the most ideal particle shape is spherical. In order to prepare spherical luminescent particles, people have tried many methods, such as spray pyrolysis (Zhou Yonghui, Lin Jun, Yu Min, et al. Progress in luminescent material prepared by spray pyrolysis process[J].Chin.J.Lumin., 2002,23(5):503-508) is one of the most effective and common methods, but the spray pyrolysis method is easy to form hollow particles, and this The hollow state will seriously affect the stability of the fluorescence method, so the use of it to prepare high-performance and high-stability fluorescent materials remains to be studied

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) Preparation of metal ion solution: Weigh a certain amount of yttrium oxide powder, dissolve it with excess concentrated sulfuric acid, and then mix it with cerium nitrate and aluminum nitrate solution to form a metal ion solution, wherein the molar ratio (the same below) is controlled Y 3+ : Ce 3+ : Al 3+ =2.94:0.06:5

[0023] 2) Selection of precipitant: choose NH 4 HCO 3 as a precipitant.

[0024] 3) Add the metal ion solution obtained in step 1) dropwise into the precipitant at a rate of 2 mL / min, and stir continuously at a pH value of 8 to obtain a coprecipitate.

[0025] 4) Wash the co-precipitate obtained in step 3) twice with water and then with alcohol twice, then filter with suction, and dry at 60° C. to obtain a precursor.

[0026] 5) The precursor obtained in step 4) was raised to 700° C. at a heating rate of 1° C. / min, and kept at a constant temperature for 100 minutes to obtain a calcined powder.

[0027] 6) Calcinate the pre-calcined powder obtai...

Embodiment 2

[0030] Raw material and technological process are with embodiment 1. The proportion of metal ions in the metal ion solution is Y 3+ : Ce 3+ :Al 3+ =2.94:0.06:5, the choice of precipitant is NH 4 HCO 3 , the dropping rate of the metal ion solution was 3mL / min, and the pH value was controlled at 9. The co-precipitate after washing with water and alcohol was dried at 70°C, and the temperature of the precursor was raised to 750°C at a rate of 2°C / min. 200min, the temperature of calcining the pre-calcined powder is 900°C, and the holding time is 200min. The particles of the obtained YAG:Ce phosphor with a particle size of about 150nm account for 85% of the total particle size, its color rendering index Ra=65, and the relative intensity Y / Y0=5.300, the phosphor can be effectively excited by blue light (460nm) and near ultraviolet light (330-350nm), and when excited by visible light of 460nm, it can emit an emission spectrum with a dominant wavelength of 568nm.

Embodiment 3

[0032] Raw material and technological process are with embodiment 1. The proportion of metal ions in the metal ion solution is Y 3+ : Ce 3+ :Al 3+ =2.94:0.06:5, the choice of precipitant is NH 4 HCO 3 , the dropping rate of the metal ion solution was 4mL / min, and the pH value was controlled at 8. The coprecipitate after washing with water and alcohol was dried at 80°C, and the temperature of the precursor was raised to 650°C at a rate of 3°C / min. 300min, the temperature of calcining the pre-calcined powder is 1000°C, and the holding time is 300min, the particles of the obtained YAG:Ce phosphor particle size are about 90nm account for 75% of the total particle size, the color rendering index Ra=75, and the relative intensity Y / Y0=5.300, the fluorescent powder can be effectively excited by blue light (460nm) and near-ultraviolet light (330-350nm), and can emit an emission spectrum with a dominant wavelength of 520nm when excited by visible light of 460nm.

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Abstract

The invention discloses a co-precipitation method for preparing rare earth cerium ion-doped yttrium aluminum garnet fluorescent powder and relates to fluorescent powder. The method comprises the following steps of: dissolving yttrium oxide powder in excessive concentrated sulfuric acid and mixing dissolved yttrium oxide with solution of cerous nitrate and solution of aluminum nitrate to prepare metal ion solution, wherein the ratio of Y<3+> to Ce<3+> to Al<3+> is 2.94:0.06:5; adding the metal ion solution into a precipitator to obtain a co-precipitate; cleaning, filtering and drying the co-precipitate to obtain a precursor; pre-sintering the precursor to obtain pre-sintered powder; and calcining the pre-sintered powder to obtain the rare earth cerium ion-doped yttrium aluminum garnet fluorescent powder. In the used co-precipitation method, mixing is performed under the ionic condition, so the mixing is more uniform compared with that of a mechanical mixing method, impurity doping possibility is reduced, accurate control of chemical calculation becomes easier and granularity can be controlled according to a reaction condition. The precipitator and the like are preferably selected and the co-precipitation method is implemented to form a pure YAG phase at the temperature of 1,100 DEG C, which is about 500 DEG C lower than that of a conventional high temperature solid phase reaction method.

Description

technical field [0001] The invention relates to a fluorescent powder, in particular to a method for preparing rare earth cerium ion-doped yttrium aluminum garnet fluorescent powder by a co-precipitation method. Background technique [0002] Fluorescent substances are widely used in fluorescent lamps, cathode ray tubes (Cathode Ray Tube, CRT), fluorescent screens of televisions, and scintillation counters. In recent years, with the wide application of CRTs, the amount of fluorescent substances has also increased. Moreover, fluorescent screens are developing toward large areas and high resolutions, and CRTs also put forward higher requirements for the phosphor materials used. Traditionally used fluorescent materials are single-crystal powders with a particle size of 1-5 μm and a powder shape that tends to be spherical. Today, in order to improve the life of the screen and withstand the impact of higher electron energy, there is a need for Luminescence Efficiency and Brightnes...

Claims

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Application Information

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IPC IPC(8): C09K11/80
Inventor 罗学涛吴浩李锦堂刘春佳龚惟扬
Owner XIAMEN UNIV
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