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Preparation method of Eu<3+> ion-doped gadolinium fluoride/sodium gadolinium fluoride crystal phase-controllable luminescent powder

A technology of sodium gadolinium fluoride and ion doping is applied in the field of preparation of rare earth doped light-emitting materials, and achieves the effect of wide application prospect and strong practicability

Inactive Publication Date: 2014-06-11
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no use of PVP for Eu in the hydrothermal method at home and abroad. 3+ ion-doped GdF 3 / NaGdF 4 Efficient control of crystal phase formation reported

Method used

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  • Preparation method of Eu&lt;3+&gt; ion-doped gadolinium fluoride/sodium gadolinium fluoride crystal phase-controllable luminescent powder
  • Preparation method of Eu&lt;3+&gt; ion-doped gadolinium fluoride/sodium gadolinium fluoride crystal phase-controllable luminescent powder

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: take by weighing 431mg Gd 2 o 3 and 22.0mg Eu 2 o 3 In a beaker, add 5mL of dilute nitric acid and heat to dissolve. After cooling, add 28mL of deionized water to form a rare earth ion solution; weigh 1050mg of sodium fluoride and add it to the mixed solution, adjust the pH to 1, and continue stirring at room temperature for 30 minutes to obtain a mixed solution. Transfer it to a 50mL reactor, react at 180°C for 24 hours, take out the reactor, cool to room temperature naturally, centrifuge, wash with alcohol water several times, and dry at 60°C to obtain GdF 3 :Eu 3+ glow powder. figure 1 (a) is the synthesized GdF 3 :Eu 3+ X-ray diffraction pattern of luminescent powder, indicating that the product is pure phase GdF 3 , belonging to the orthorhombic crystal system.

Embodiment 2

[0019] Embodiment 2: take by weighing 431mg Gd 2 o 3 and 22.0mg Eu 2 o 3 In a beaker, add 5mL of dilute nitric acid and heat to dissolve. After cooling, add 28mL of deionized water to form a rare earth ion solution; weigh 0.1g of polyvinylpyrrolidone and add it to the above solution, stir with a magnetic stirrer at room temperature for 30min to obtain rare earth ions and poly Mixed solution of vinylpyrrolidone; Weigh 1050mg of sodium fluoride and add it to the mixed solution, adjust pH=1, continue to stir at room temperature for 30min to obtain the mixed solution, transfer it to a 50mL reactor, react at 180°C for 24h, take out the reaction kettle, cooled naturally to room temperature, centrifuged, washed several times with alcohol and water, and dried at 60°C to obtain GdF 3 :Eu 3+ / NaGdF 4 :Eu 3+ Crystal phase luminous powder. figure 1 (b) is the X-ray diffraction pattern of the synthesized product, indicating that the product is an orthorhombic GdF 3 and hexagonal Na...

Embodiment 3

[0020] Embodiment 3: take by weighing 431mg Gd 2 o 3 and 22.0mg Eu 2 o 3 In a beaker, add 5mL of dilute nitric acid and heat to dissolve. After cooling, add 27mL of deionized water to form a rare earth ion solution; weigh 0.5g of polyvinylpyrrolidone and add it to the above solution, stir with a magnetic stirrer at room temperature for 30min to obtain rare earth ions and poly Mixed solution of vinylpyrrolidone; Weigh 1050mg of sodium fluoride and add it to the mixed solution, adjust pH=1, continue to stir at room temperature for 30min to obtain the mixed solution, transfer it to a 50mL reactor, react at 180°C for 24h, take out the reaction kettle, cooled naturally to room temperature, centrifuged, washed several times with alcohol and water, and dried at 60°C to obtain NaGdF 4 :Eu 3+ Crystal phase luminous powder. figure 1 (c) is an X-ray diffraction pattern of the synthesized product, indicating that the product is a pure phase of NaGdF 4 , belonging to the hexagonal cr...

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Abstract

The invention discloses a preparation method of Eu<3+> ion-doped gadolinium fluoride / sodium gadolinium fluoride crystal phase-controllable luminescent powder, relating to a preparation method of a rare earth doped luminescent material. In the method, Gd2O3 (99.99 percent), Eu2O3 (99.99 percent), analytically-pure sodium fluoride (NaF) and polyvinylpyrrolidone (PVPMw=58.000) are taken as raw materials. The method comprises the following steps: (1) preparing a rare earth composite nitrate (gadolinium nitrate and europium nitrate) mixed solution; (2) adding polyvinylpyrrolidone and sodium fluoride; (3) performing a hydrothermal reaction on the mixed solution under the condition of different temperatures and different time; (4) washing and drying to obtain a product. A preparation process adopted in the method is simple, the entire reaction is performed in an aqueous solution, an added polymer is environmental friendly, high practicability is realized, and the crystal phase of the product can be controlled effectively under the condition that a basic formula is not changed in order to further control the luminescent property of the luminescent powder. The method is wide in application prospect.

Description

technical field [0001] The invention relates to a method for preparing a rare earth-doped luminescent material, in particular to a Eu 3+ Preparation method of ion-doped gadolinium fluoride / sodium gadolinium fluoride crystal phase controllable luminous powder. Background technique [0002] Fluoride has optical transmission in a wide wavelength range from ultraviolet to far infrared, weak crystal field, small refractive index, especially after the doping of rare earth ions as an activator, because it has lower phonon energy, it can reduce The non-radiative transition probability of rare earth ions in the excited state improves the luminous efficiency, and the rare earth doped fluoride has been widely used in lasers, displays, lighting sources, optical communications, etc. [0003] In rare earth doped fluorides, because Gd 3+ The ions have absorption in the ultraviolet region, which can promote the matrix and Eu 3+ energy transfer between ions, so GdF 3 and NaGdF 4 is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85
Inventor 李艳红张星傲马晶
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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