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A kind of preparation method of rare earth doped gadolinium oxysulfide fluorescent powder

A technology of doping gadolinium oxysulfide and rare earth, which is applied in the field of material science, can solve the problems of high product cost and difficulty in purifying sulfate, and achieves the effect that the technical solution is simple and easy to implement.

Active Publication Date: 2019-02-05
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Rare earth sulfur oxides can also be prepared by direct calcination of sulfate commercial powder. Although the raw materials used in this method are simple and easy to obtain, the purification of sulfate is relatively difficult, resulting in high product costs and the inevitable release of H 2 S harmful gas
The use of environmentally harmful sulfur-containing raw materials and the discharge of harmful products have remained a challenging problem in the preparation of such materials

Method used

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  • A kind of preparation method of rare earth doped gadolinium oxysulfide fluorescent powder
  • A kind of preparation method of rare earth doped gadolinium oxysulfide fluorescent powder
  • A kind of preparation method of rare earth doped gadolinium oxysulfide fluorescent powder

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Experimental program
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Effect test

Embodiment 1

[0051] A preparation method of rare earth-doped gadolinium oxysulfide fluorescent powder, comprising the following steps:

[0052] (1) Gd(NO 3 ) 3 ·6H 2 O and Tb(NO 3 ) 3 ·6H 2 O was added to deionized water and stirred at room temperature to obtain RE 3+ The concentration is 0.1mol / L RE(NO 3 ) 3 solution; where, in molar ratio, Gd 3+ :Tb 3+ =99:1;

[0053] (2) Dissolve 0.8g ammonium sulfate in 0.1mol / L RE(NO 3 ) 3 In solution, RE(NO 3 ) 3 The volume of the solution is 60mL, stirred for 15min, at 4°C, continued to stir and added ammonia water dropwise to adjust the pH value to 9.0 to obtain a suspension; wherein, by molar ratio, sulfate: RE 3+ =1:1;

[0054] (3) The suspension was continuously stirred and reacted at 4°C for 4 hours to obtain a reaction product;

[0055] (4) Centrifuge the reaction product, add water to wash three times, then add absolute ethanol to wash once, and dry at 50°C to obtain an amorphous white powder precursor-sulfate-type rare earth ...

Embodiment 2

[0058] A preparation method of rare earth-doped gadolinium oxysulfide fluorescent powder, comprising the following steps:

[0059] (1) Gd(NO 3 ) 3 ·6H 2 O and Tb(NO 3 ) 3 ·6H 2 O was added to deionized water and stirred at room temperature to obtain RE 3+ The concentration is 0.1mol / L RE(NO 3 ) 3 solution; where, in molar ratio, Gd 3+ :Tb 3+ =99:1;

[0060] (2) Dissolve 0.8g ammonium sulfate in 0.1mol / L RE(NO 3 ) 3 In solution, RE(NO 3 ) 3 The volume of the solution is 60mL, stirred for 15min, at 30°C, continued to stir and added ammonia water dropwise, adjusted the pH value to 7.0, to obtain a suspension; wherein, in molar ratio, sulfate radical: RE 3+ =1:1;

[0061] (3) react the suspension with continuous stirring at 30° C. for 1 hour to obtain the reaction product;

[0062] (4) Centrifuge the reaction product, add water to wash three times, then add absolute ethanol to wash once, and dry at 70 ° C to obtain a white powder precursor - sulfate-type rare earth...

Embodiment 3

[0065] A preparation method of rare earth-doped gadolinium oxysulfide fluorescent powder, comprising the following steps:

[0066] (1) Gd(NO 3 ) 3 ·6H2 O and Tb(NO 3 ) 3 ·6H 2 O was added to deionized water and stirred at room temperature to obtain RE 3+ The concentration is 0.1mol / L RE(NO 3 ) 3 solution; where, in molar ratio, Gd 3+ :Tb 3+ =99:1;

[0067] (2) Dissolve 0.8g ammonium sulfate in 0.1mol / L RE(NO 3 ) 3 In solution, RE(NO 3 ) 3 The volume of the solution is 60mL, stirred for 20min, at 25°C, continued to stir and added ammonia water dropwise, adjusted the pH value to 7.0, to obtain a suspension; wherein, by molar ratio, sulfate radical: RE 3+ =1:1;

[0068] (3) Move the suspension to a reaction kettle, and conduct a hydrothermal reaction at 100° C. for 72 hours. After the reaction, cool naturally to room temperature to obtain a reaction product;

[0069] (4) Centrifuge the reaction product, add water to wash three times, then add absolute ethanol to wa...

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Abstract

The invention discloses a preparing method of rare earth-doped gadolinium oxysulfide fluorescent powder, and belongs to the technical field of materials. The preparing method comprises the first step of preparing a RE(NO3)3 solution, wherein the RE(NO3)3 solution is mixed liquid of Gd(NO3)3 and activating agent nitrate; the second step of dissolving ammonium sulfate into the RE(NO3)3 solution, continuously stirring the mixture and adding ammonium hydroxide into the mixture, and adjusting a pH value to obtain turbid liquid; the third step of conducting reaction on the turbid liquid at the temperature of minus 1-150 DEG C for 1-72 hours to obtain a reaction product; the fourth step of conducting centrifugal separation, cleaning and drying on the reaction product to obtain a white powder precursor; roasting the white powder precursor in reducing atmosphere to obtain (Gd,Tb)202S or (Gd,Pr)202S fluorescent powder. According to the technical scheme, the preparing method is simple and easy to operate, in the process of preparing (Gd,Tb)202S or (Gd,Pr)202S, sulfocompound which is harmful to the environment is not involved; in addition, (Gd,Tb)202S or (Gd,Pr)202S of various morphologies (nano-particles, agglomerated balls and standard hexagon micron sheet bars) can be obtained.

Description

technical field [0001] The invention belongs to the field of material science, in particular to a preparation method of rare earth-doped gadolinium oxysulfide fluorescent powder. Background technique [0002] Rare earth sulfur oxides (RE 2 o 2 S) has a wide band gap (4.6-4.8 eV), is a very important class of luminescent host materials, and has excellent light absorption and energy transfer efficiency. RE 2 o 2 S is chemically stable in an inert atmosphere, its melting point exceeds 2000°C and it is not easy to deliquesce and oxidize, so it is used as a radiation laser material, long afterglow material, cathode ray luminescent material, X-ray luminescent material, up / down conversion luminescent material and light storage material. It has been widely used in many fields. [0003] Among them, in rare earth-doped gadolinium oxysulfide phosphors, terbium-doped gadolinium oxysulfide ((Gd, Tb) 2 o 2 S) and praseodymium-doped gadolinium oxysulfide ((Gd, Pr) 2 o 2 S) is a ve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/84C01F17/00
CPCC01F17/282C01F17/294C01P2002/72C01P2004/03C01P2004/22C01P2004/32C01P2004/60C01P2004/62C09K11/7771
Inventor 李继光王雪娇朱琦李晓东孙旭东
Owner NORTHEASTERN UNIV LIAONING
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