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Luminescence-enhanced rare earth doped phosphate full-white fluorescent powder and preparation method thereof

A phosphor, based phosphate technology, applied in luminescent materials, chemical instruments and methods, sustainable architecture, etc., can solve the problems of long synthesis cycle, unfavorable commercial production, and reduced luminous intensity

Pending Publication Date: 2021-05-18
CHENGDU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the process steps are complicated and the synthesis period is long (>28h)
In addition, K 5 YP 4 o 14 The matrix contains the relatively expensive rare earth element Y, which is not conducive to subsequent commercial production in large quantities
The paper (Journal of Luminescence 154(2014) 246) prepared Ca 19-x Mg 2 (PO 4 ) 14 :xDy 3+ , but since Dy 3+ to Ca 2+ The unequal substitution caused defects in the crystal lattice, reducing the luminous intensity

Method used

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  • Luminescence-enhanced rare earth doped phosphate full-white fluorescent powder and preparation method thereof
  • Luminescence-enhanced rare earth doped phosphate full-white fluorescent powder and preparation method thereof
  • Luminescence-enhanced rare earth doped phosphate full-white fluorescent powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] a) According to Ca 19-x Zn 2 (PO 4 ) 14-y (SiO 4 ) y :xDy 3+ (x=0.38, y=0) stoichiometric ratio weighs 4.3971g Ca (NO 3 ) 2 4H 2 O, 0.5949g Zn(NO 3 ) 2 ·6H 2 O, 0.1735g Dy(NO 3 ) 3 ·6H 2 O, 1.5759g NH 4 h 2 PO 4 and 8.0694g citric acid (C 6 h 8 o 7 ) was dissolved in deionized water and stirred until all raw materials were completely dissolved to form a solution, and the pH of the solution was adjusted to be 3;

[0039] b) heating the solution obtained in step a to 70° C., and continuously stirring at a speed of 800 rad / min until a sol is obtained;

[0040] c) Transfer the sol obtained in step b to a corundum crucible and keep it in a muffle furnace at 200°C for 0.5h. In this state, the moisture in the sol will disappear quickly, and the metal nitrate and citric acid will react to generate a flame; The temperature of the muffle furnace was raised to 800°C again at 5°C / min and kept for 1h. After the sample is cooled to room temperature with the furn...

Embodiment 2

[0043] a) According to Ca 19-x Zn 2 (PO 4 ) 14-y (SiO 4 ) y :xDy 3+ (x=0.38, y=0.3) stoichiometric ratio weighs 4.3971g Ca (NO 3 ) 2 4H 2 O, 0.5949g Zn(NO 3 ) 2 ·6H 2 O, 0.1735g Dy(NO 3 ) 3 ·6H 2 O, 1.5759g NH 4 h 2 PO 4 and 8.0694g citric acid (C 6 h 8 o 7 ) was dissolved in deionized water and stirred until all the raw materials were completely dissolved to form solution 1; weighed 0.0625g tetraethyl orthosilicate (C 8 h 20 o 4 Si) was dissolved in an ethanol solution to form a solution 2, and the solution 2 was slowly dropped into the solution 1, stirred and mixed evenly, and the pH value of the mixed solution was adjusted to 3;

[0044] b) heating the mixed solution obtained in step a to 70° C., and continuously stirring at a speed of 800 rad / min until a sol is obtained;

[0045] c) Transfer the sol obtained in step b to a corundum crucible and keep it in a muffle furnace at 200°C for 0.5h. In this state, the moisture in the sol will disappear quickl...

Embodiment 3

[0048] a) According to Ca 19-x Zn 2 (PO 4 ) 14-y (SiO 4 ) y :xDy 3+ (x=0.5, y=0.1) stoichiometric ratio weighs 4.3687gCa(NO 3 ) 2 4H 2 O, 0.5949g Zn(NO 3 ) 2 ·6H 2 O, 0.2283g Dy(NO 3 ) 3 ·6H 2 O, 1.5989g NH 4 h 2 PO 4 and 4.0347g citric acid solution (C 6 h 8 o 7 ) in deionized water until all raw materials are completely dissolved to form a solution 1; weigh 0.0208g tetraethyl orthosilicate (C 8 h 20 o 4 Si) was dissolved in an ethanol solution to form a solution 2, and the solution 2 was slowly dropped into the solution 1, stirred and mixed evenly, and the pH value of the mixed solution was adjusted to 5;

[0049] b) heating the mixed solution obtained in step a to 80° C., and continuously stirring at a speed of 500 rad / min until a sol is obtained;

[0050] c) Transfer the sol obtained in step b into a corundum crucible and keep it in a muffle furnace at 200°C for 0.5h. In this state, the moisture in the sol will disappear quickly, and the metal nitrat...

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Abstract

The invention discloses low-cost phosphate fluorescent powder for a white-light LED (light-emitting diode) and a preparation method of the low-cost phosphate fluorescent powder. The general chemical formula of the fluorescent powder is Ca19-xZn2(PO4)14-y (SiO4)y:xDy3+, wherein x is more than or equal to 0.0095 and less than or equal to 0.95, and y is more than or equal to 0 and less than or equal to 0.4. The Ca19Zn2(PO4)14 is adopted as a matrix, so that good stability is achieved. Through charge compensation that PO4<3-> is replaced by SiO4<4->, the luminous intensity of the fluorescent powder is greatly improved, blue light (484nm) and yellow light (575nm) are emitted, and the fluorescent powder can be matched with a near ultraviolet light chip to be applied to a white light LED. In the invention, the fluorescent powder is prepared by adopting a sol combustion method, so that the process of repeated calcination in a high-temperature solid-phase method is avoided, a drying process in a sol-gel method is also avoided, and the preparation period is shortened. The fluorescent powder has the advantages of simple synthesis process, low synthesis temperature, short synthesis period, uniform size distribution of the fluorescent powder, good luminescence property and the like.

Description

technical field [0001] The present invention relates to a kind of Ca 19-x Zn 2 (PO 4 ) 14-y (SiO 4 ) y :xDy 3+ The phosphor material and its preparation method and application belong to the technical field of rare earth luminescent materials. Background technique [0002] Compared with traditional lighting sources such as incandescent lamps and fluorescent lamps, white LEDs have the advantages of high energy efficiency, long life, fast response time, and environmental friendliness. They are called the fourth-generation green lighting methods and are widely used in various industries. [0003] With the global shortage of non-renewable energy and the increasing pressure on environmental protection, various countries have increased the use of white LEDs, and formulated a series of strategic plans around white LED lighting, which fully demonstrates the research and development of white LEDs and the industrialization of results. support. The current commercial white LED i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/71
CPCC09K11/771Y02B20/00
Inventor 张文涛王特深陈显飞许心茹张佩聪黄雪王晓萌张继勇王益群
Owner CHENGDU UNIVERSITY OF TECHNOLOGY
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