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Preparation method of rare earth-doped gadolinium oxysulfide and gadolinium oxysulfate up-conversion phosphor

A technology of gadolinium oxysulfide and rare earth doping is applied in the field of material science, which can solve the problems of environmental hazards, the use of environmentally harmful sulfur-containing raw materials, and the inability to achieve effective regulation of green preparation morphology.

Active Publication Date: 2019-02-05
NORTHEASTERN UNIV LIAONING
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Problems solved by technology

[0005] For the existing preparation of rare earth doped Gd 2 o 2 The problem of using environmentally harmful sulfur-containing raw materials in the S technical route, the present invention provides a preparation method of rare earth-doped gadolinium oxysulfide up-conversion phosphor, the preparation method adopts a hydrothermal method to prepare rare earth-doped Gd 2 (OH) 4 SO 4 ·nH 2 O and Gd 2 (OH) 4 SO 4 Two types of precursors, and using the molar ratio of RE / S in the two types of precursors and the RE 2 o 2 The completely consistent characteristics in S, calcining the two types of compounds in a reducing atmosphere, the green preparation of rare earth doped Gd 2 o 2 S
This method effectively solves the problem of the use of environmentally harmful sulfur-containing raw materials and the discharge of harmful by-products in conventional methods, and is a green and environmentally friendly preparation technology
[0006] For the existing preparation of rare earth doped Gd 2 o 2 SO 4 In the technical route, there is a problem that the green preparation cannot be realized and the effective control of its morphology can be achieved. The present invention provides a preparation method of rare earth-doped gadolinium oxysulfate up-conversion phosphor. The method is prepared by hydrothermal method rare earth doped Gd 2 (OH) 4 SO 4 ·nH 2 O, rare earth-doped Gd with uniform agglomerated spheres achieved by calcining the compound in air 2 o 2 SO 4 preparation, and provide a quasi-hexagonal micro-plate rare earth-doped sulfate-type rare earth layered hydroxide Gd 2 (OH) 4 SO 4 The hydrothermal preparation method, the compound is calcined in the air to prepare the rare earth-doped Gd of the quasi-hexagonal micron plate 2 o 2 SO 4

Method used

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  • Preparation method of rare earth-doped gadolinium oxysulfide and gadolinium oxysulfate up-conversion phosphor

Examples

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Effect test

Embodiment 1

[0064] A preparation method of rare earth-doped gadolinium oxysulfate up-conversion fluorescent powder is carried out according to the following steps:

[0065] (1) Gd(NO 3 ) 3 ·6H 2 O, Yb(NO 3 ) 3 ·6H 2 O and Ho(NO 3 ) 3 ·6H 2 O mixed, added deionized water, stirred at room temperature until it became transparent, and RE was obtained 3+ The ion concentration is 0.05mol / L RE(NO 3 ) 3 solution;

[0066] Among them, by mass ratio, Gd 3+ :Yb 3+ : Ho 3+ =90:5:5;

[0067] (2) Dissolve 0.4g ammonium sulfate in 0.05mol / L RE(NO 3 ) 3 In solution, RE(NO 3 ) 3 The volume of the solution is 60mL. Stir at room temperature for 20min, then continue to stir and add ammonia water dropwise to adjust the pH value to 7.0 to obtain a suspension;

[0068] Among them, by molar ratio, sulfate radical: RE 3+ =1:1;

[0069] (3) Move the suspension to a reaction kettle, and conduct a hydrothermal reaction at 100°C for 72 hours. After the reaction, take it out, and cool it naturally...

Embodiment 2

[0073] A preparation method of a rare earth-doped gadolinium oxysulfide up-conversion phosphor is carried out according to the following steps:

[0074] Step (1), (2), (3), (4) are the same as embodiment 1;

[0075] (5) Place the white powder precursor in H 2 and N 2 The mixed gas (volume ratio, H 2 :N 2 =50:50) atmosphere, calcined at 800°C for 1h to obtain rare earth sulfur oxide (Gd 0.90 Yb 0.05 Ho 0.05 ) 2 o 2 S phosphor, its XRD see Image 6 (a), it can be seen from the figure that the product is a pure phase; its shape is similar to its precursor, and it is an agglomerated ball with a diameter of 80-110 μm, such as Figure 7 (a) shown.

Embodiment 3

[0077] A preparation method of rare earth-doped gadolinium oxysulfate up-conversion fluorescent powder is carried out according to the following steps:

[0078] (1) Gd(NO 3 ) 3 ·6H 2 O, Yb(NO 3 ) 3 ·6H 2 O and Er(NO 3 ) 3 ·6H 2 O mixed, added deionized water, stirred at room temperature until it became transparent, and RE was obtained 3+ The ion concentration is 0.5mol / L RE(NO 3 ) 3 solution;

[0079] Among them, by mass ratio, Gd 3+ :Yb 3+ :Er 3+ =97:2:1;

[0080] (2) Dissolve 4g of ammonium sulfate in 0.5mol / L RE(NO 3 ) 3 In solution, RE(NO 3 ) 3 The volume of the solution is 60mL. Stir at room temperature for 20min, then continue to stir and add ammonia water dropwise to adjust the pH value to 7.0 to obtain a suspension;

[0081] Among them, by molar ratio, sulfate radical: RE 3+ =1:1;

[0082] (3) Move the suspension to a reaction kettle, and conduct a hydrothermal reaction at 100° C. for 1 hour. After the reaction, take it out and cool it down to room...

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Abstract

The invention provides a preparation method of rare earth-doped gadolinium oxysulfide and oxygen-containing gadolinium sulphate up-conversion phosphor, and belongs to the field of material science. The method comprises the following steps that 1, Gd(NO3)3.6H2O, Yb(NO3)3.6H2O and Ln(NO3)3.6H2O are mixed, deionized water is added, and a RE(NO3)3 solution is obtained; 2, ammonium sulfate is dissolved into the RE(NO3)3 solution, stirring is conducted, stirring continues, ammonia water is added, the pH value is regulated, and suspension is obtained; 3, the suspension is subjected to a hydrothermal reaction for 1-72 h at the temperature of 100 DEG C to 150 DEG C and then naturally cooled to room temperature, and a reaction product is obtained; 4, the reaction product is centrifugally separated, washed and dried, and a white powder precursor is obtained; 5, the white powder precursor is calcined, and the rare earth ion-doped Gd2O2S or Gd2O2SO4 up-conversion phosphor is obtained. According to the method, the problems of usage of sulfur-containing raw materials and discharge of harmful by-products in a conventional method are effectively solved, and the method is a green and environment-friendly preparation technique.

Description

technical field [0001] The invention belongs to the field of material science, and particularly relates to a preparation method of rare earth-doped gadolinium oxysulfide and oxysulfate-containing gadolinium up-conversion fluorescent powder. Background technique [0002] Upconversion luminescent materials are widely used in upconversion lasers, dye-sensitized solar cells, drug delivery, bioluminescence labeling, and infrared anti-counterfeiting due to their unique ability to convert long-wave radiation into short-wave radiation. The current high-efficiency upconversion system is fluoride (such as NaYF 4 : Yb / Er), fluoride has the advantages of low phonon energy and high upconversion efficiency. However, fluoride raw materials are highly toxic, which greatly limits the large-scale production and practical application of fluoride upconversion luminescent materials. Although the rare earth oxide upconversion system is non-toxic, the phonon energy is high and the upconversion e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/84
CPCC09K11/7781C09K11/7789
Inventor 李继光王雪娇朱琦李晓东孙旭东
Owner NORTHEASTERN UNIV LIAONING
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