Preparation method of cerium-doped yttrium aluminum garnet spherical fluorescent powder

A technology of yttrium aluminum garnet and fluorescent powder, which is applied in the field of preparation of functional nanomaterials, can solve the problems of large particle size, uneven distribution of powder components, irregular agglomeration shapes, etc., and achieves good repeatability and wide and easy access to reagents , the effect of easily controllable conditions

Inactive Publication Date: 2018-03-06
CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

[0007] The present invention will solve prior art preparation YAG: Ce 3+ In order to solve the technical problems of uneven distribution of powder components, large particle size, serious agglomeration and irregular shape, a preparation method of cerium-doped yttrium aluminum garnet spherical phosphor powder is provided. The preparation method obtains the precursor by co-precipitation After solidification, the solvothermal reaction is carried out in the reactor, and the size and shape of the material can be controlled at a relatively low temperature and pressure by selecting a suitable solvent ethylenediamine or ethylenediamine-alcohol solution

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  • Preparation method of cerium-doped yttrium aluminum garnet spherical fluorescent powder
  • Preparation method of cerium-doped yttrium aluminum garnet spherical fluorescent powder
  • Preparation method of cerium-doped yttrium aluminum garnet spherical fluorescent powder

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preparation example Construction

[0058] The preparation method of the cerium-doped yttrium aluminum garnet spherical phosphor body provided by the present invention specifically comprises the following steps:

[0059] (1) Configure the precursor reaction solution

[0060] Step 1-1: According to chemical formula Y 3-x Ce x al 5 o 12 , 03+ Concentration of 0.025 ~ 0.5mol / L mixed mother solution, NH 4 HCO 3 Soluble in ethanol-water mixed solvent, the volume ratio of ethanol to water is 0.2:1~1.5:1, to prepare NH 4 HCO 3 The concentration is 0.5~2.2mol / L precipitant solution;

[0061] Or step 1-2: according to chemical formula Y 3 al 5 o12 Metering ratio, that is, weigh the yttrium salt and the aluminum salt according to the molar ratio of Y and Al as 3:5, dissolve the yttrium salt and the aluminum salt in deionized water, and prepare the Al 3+ Concentration of 0.025 ~ 0.5mol / L mixed mother solution, NH 4 HCO 3 Soluble in ethanol-water mixed solvent, the volume ratio of ethanol to water is 0.2:1~1.5:1...

Embodiment 1

[0075] 0.0441mol Y (NO 3 ) 3 , 0.0009mol Ce(NO 3 ) 3 and 0.0765mol Al(NO 3 ) 3 Dissolved in 180mL deionized water, configured as Al 3+ Concentration is 0.425mol / L mixed salt solution, prepare 1500mL of NH with a concentration of 0.5mol / L with ethanol-water composite solvent with a volume ratio of ethanol and water of 3:2 4 HCO 3 The solution was stirred continuously during the titration. After the titration, it was aged at normal pressure and 20°C for 24 hours; the aged precipitation solution was centrifuged to obtain a milky white precipitate, and then the milky white precipitate was washed 3 times with deionized water to remove impurity ions. Wash twice with water and ethanol to remove water; put the washed white precipitate in an oven, and dry at normal pressure and 60°C for 24 hours to obtain Y 2.94 Ce 0.06 al 5 o 12 Precursor. weighing Y 2.94 Ce 0.06 al 5 o 12 0.40 g of the precursor was dispersed into 60 mL of ethylenediamine by stirring and ultrasonicati...

Embodiment 2

[0077] 0.0297mol YCl 3 , 0.0003mol Ce(NO 3 ) 3 and 0.05mol Al(NO 3 ) 3 Dissolved in 600mL deionized water, configured as Al 3+ Concentration is 0.083mol / L mixed salt solution, prepare 2000mL of NH with a concentration of 0.5mol / L with ethanol-water composite solvent with a volume ratio of ethanol and water of 1:1 4 HCO 3 The solution was stirred continuously during the titration. After the titration, age at normal pressure and 15°C for 8 hours; centrifuge the aged precipitate solution to obtain a milky white precipitate, then wash the precipitate with deionized water 3 times to remove impurity ions, and then use anhydrous Wash with ethanol twice to remove water; put the washed white precipitate in an oven, and dry at normal pressure and 60°C for 24 hours to obtain Y 2.97 Ce 0.03 al 5 o 12 Precursor. weighing Y 2.97 Ce 0.03 al 5 o 12 4.5g of the precursor was dispersed into a mixed solution of 72mL of ethylenediamine and 8mL of ethanol by stirring and ultrasonica...

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Abstract

The invention discloses a preparation method of cerium-doped yttrium aluminum garnet nano / micro-scale spherical fluorescent powder. The material is Y3-xCexAl5O12, wherein x is greater than 0 and smaller than or equal to 0.3. The preparation method provided by the invention is a co-precipitation-solvothermal method and comprises the following steps: firstly, preparing a YAG:Ce<3+> or a YAG precursor by using a co-precipitation method; secondly, carrying out solvothermal reaction in a reaction kettle, with ethylenediamine or an ethylenediamine-alcoholic solution as a solvent, reacting at the temperature of 260 to 290DEG C for 12 to 48 hours; and dissolving and recrystallizing to generate single-phase Y3-xCexAl5O12 fluorescent powder with high yield, high repeatability, higher illumination brightness and high crystallization degree. Without subsequent high-temperature roasting or atmosphere reduction, particle agglomeration caused by calcining is effectively reduced. The preparation method has the advantages that control over size and morphology of materials is realized at relatively-low temperature and pressure; the size of a powder material can be adjusted and controlled within therange of 0.1 to 2.0 [mu]m according to the demand; the process is simple, conditions are easily to control and no special expensive equipment is needed; the materials are stable in performance, regular in spherical morphology and high in dispersity; and a selected reagent is wide in source and easy to obtain.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional nanometer materials, in particular to a preparation method of cerium-doped yttrium aluminum garnet spherical fluorescent powder. Background technique [0002] Yttrium aluminum garnet (Y 3 Al 5 o 12 , YAG) is a photonic material with excellent comprehensive optical, mechanical and thermal properties. It has a stable matrix, high melting point, high hardness, and is resistant to electron beam and ultraviolet photon bombardment; the YAG crystal structure belongs to the equiaxed crystal system, with uniform optics and no birefringence effect. . doped with different rare earth activating ions Ln 3+ , such as Nd 3+ , Yb 3+ 、Er 3+ 、Tm 3+ 、Ce 3+ etc.) into YAG, luminescent materials with different properties (laser crystals, transparent ceramics, phosphors) can be obtained, and their applications can be extended to optical materials, such as white LED lighting, scintillators for...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/80B82Y30/00B82Y40/00H01L33/50
Inventor 潘国徽张霞武华君张亮亮郝振东张家骅
Owner CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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