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Preparing 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 achieve the effect of simple and easy technical solution.

Active Publication Date: 2017-03-29
NORTHEASTERN UNIV
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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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  • Preparing method of rare earth-doped gadolinium oxysulfide fluorescent powder
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  • Preparing method of rare earth-doped gadolinium oxysulfide fluorescent powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] A preparation method of rare earth doped gadolinium oxysulfide phosphor includes the following steps:

[0052] (1) Gd(NO 3 ) 3 ·6H 2 O and Tb(NO 3 ) 3 ·6H 2 O add deionized water, stir at room temperature to clarify, get RE 3+ The concentration is 0.1mol / L RE(NO 3 ) 3 Solution; Among them, mole 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, stir for 15min, at 4℃, keep stirring and add ammonia water drop by drop, adjust the pH value to 9.0 to obtain a suspension; wherein, molar ratio, sulfate radical: RE 3+ =1:1;

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

[0055] (4) Centrifugally separate the reaction product, add water for cleaning three times, then add anhydrous ethanol for cleaning once, and dry at 50°C to obtain an amorphous white powder precursor-sulfate type rare earth layered hydroxide (Gd 0.99 Tb 0.01 ) 2...

Embodiment 2

[0058] A preparation method of rare earth doped gadolinium oxysulfide phosphor includes the following steps:

[0059] (1) Gd(NO 3 ) 3 ·6H 2 O and Tb(NO 3 ) 3 ·6H 2 O add deionized water, stir at room temperature to clarify, get RE 3+ The concentration is 0.1mol / L RE(NO 3 ) 3 Solution; Among them, mole 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, stirring for 15min, at 30℃, continuously stirring and adding ammonia water drop by drop to adjust the pH to 7.0 to obtain a suspension; wherein, molar ratio, sulfate radical: RE 3+ =1:1;

[0061] (3) The suspension was stirred and reacted at 30°C for 1 hour to obtain a reaction product;

[0062] (4) Centrifugally separate 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 layered hydroxide (Gd 0.99 Tb 0.01 ) 2 (OH) 4 SO...

Embodiment 3

[0065] A preparation method of rare earth doped gadolinium oxysulfide phosphor includes the following steps:

[0066] (1) Gd(NO 3 ) 3 ·6H 2 O and Tb(NO 3 ) 3 ·6H 2 O add deionized water, stir at room temperature to clarify, get RE 3+ The concentration is 0.1mol / L RE(NO 3 ) 3 Solution; Among them, mole 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, stir for 20min, at 25℃, continue to stir and add ammonia water drop by drop, adjust the pH to 7.0 to obtain a suspension; wherein, molar ratio, sulfate radical: RE 3+ =1:1;

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

[0069] (4) Centrifugally separate 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 precu...

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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 materials science, and particularly relates to a method for preparing rare earth doped gadolinium oxysulfide phosphor. Background technique [0002] Rare Earth Oxides (RE 2 O 2 S) has a wide forbidden band width (4.6-4.8ev), which is a very important type of luminescent matrix material with excellent light absorption and energy transfer efficiency. RE 2 O 2 S is chemically stable in an inert atmosphere, with a melting point of over 2000°C and not easy to deliquesce and oxidize, so it is used as a radiation laser material, long afterglow material, cathodoluminescent 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 the rare earth doped gadolinium oxysulfide phosphor, the terbium doped gadolinium oxysulfide ((Gd, Tb) 2 O 2 S) and praseodymium doped gadolinium oxysulfide ((Gd, Pr) 2 O 2 S) is currently a ve...

Claims

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Application Information

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Patent Type & Authority Applications(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
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