Novel red-light fluorescent powder and method for preparing same

A fluorescent powder and red light technology, which is applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems of less red light emitting phosphor powder, low luminous intensity, and poor color rendering, and achieve increased luminous intensity and high luminous intensity. Large, high color rendering index effect

Inactive Publication Date: 2008-06-25
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are too few varieties of red light-emitting phosphors that can be practically used, and the disadvantages of low luminous intensity, poor color purity, and poor color rendering generally limit the further application of red light-emitting materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] (1) Nb 2 o 5 Dissolve in 40% HF at 80-90°C, then drop NH into it 3 ·H 2 O solution to pH 8.5-9.5, forming white Nb(OH) 5 Precipitate, aging at room temperature for 16 hours, the precipitate was filtered, washed and dissolved in citric acid aqueous solution, citric acid and Nb 2 o 5 The molar ratio of is 15: 1, forms transparent Nb-citric acid solution;

[0013] (2) According to the molar ratio Nb 5+ : Ti 4+ : Y 3+ :Eu 3+ : NH 4 NO 3 =1:1:0.996:0.004:54 ratio will be Ti(C 4 h 9 O) 4 , Y(NO 3 ) 3 , Eu(NO 3 ) 3 and NH 4 NO 3 Sequentially added to the Nb-citric acid solution prepared in step (1) to form a transparent solution, heated and stirred at 95-105°C to obtain a light yellow precursor gel;

[0014] (3) Sinter the precursor gel at 480°C for 55 minutes to obtain a fluffy brown amorphous powder, which can be thermally annealed at 1100°C for 3 hours to obtain Eu 3+ Doped YNbTiO 6 red light emitting phosphors.

Embodiment 2

[0016] (1) Nb 2 o 5 Dissolve in 40% HF at 80-90°C, then drop NH into it 3 ·H 2 O solution to pH 8.5-9.5, forming white Nb(OH) 5 Precipitate, aging at room temperature for 12 hours, the precipitate was filtered, washed and dissolved in citric acid aqueous solution, citric acid and Nb 2 o 5 The molar ratio is 9: 1, forming a transparent Nb-citric acid solution;

[0017] (2) According to the molar ratio Nb 5+ : Ti 4+ : Y 3+ :Eu 3+ : NH 4 NO 3 = 1:1:0.97:0.03:36 ratio of Ti(C 4 h 9 O) 4 , Y(NO 3 ) 3 , Eu(NO 3 ) 3 and NH 4 NO 3 Sequentially added to the Nb-citric acid solution prepared in step (1) to form a transparent solution, heated and stirred at 95-105°C to obtain a light yellow precursor gel;

[0018] (3) Sinter the precursor gel at 600°C for 25 minutes to obtain a fluffy brown amorphous powder, which can be thermally annealed at 1250°C for 0.8 hours to obtain Eu 3+ Doped YNbTiO 6 red light emitting phosphors.

Embodiment 3

[0020] (1) Nb 2 o 5 Dissolve in 40% HF at 80-90°C, then drop NH into it 3 ·H 2 O solution to pH 8.5-9.5, forming white Nb(OH) 5 Precipitate, aging at room temperature for 10 hours, the precipitate was filtered, washed and dissolved in citric acid aqueous solution, citric acid and Nb 2 o 5 The molar ratio of is 12: 1, forms transparent Nb-citric acid solution;

[0021] (2) According to the molar ratio Nb 5+ : Ti 4+ : Y 3+ :Eu 3+ : NH 4 NO 3 =1:1:0.89:0.11:44 ratio will be Ti(C 4 h 9 O) 4 , Y(NO 3 ) 3 , Eu(NO 3 ) 3 and NH 4 NO 3 Sequentially added to the Nb-citric acid solution prepared in step (1) to form a transparent solution, heated and stirred at 95-105°C to obtain a light yellow precursor gel;

[0022] (3) The precursor gel was sintered at 750°C for 6 minutes to obtain a fluffy amorphous powder, which was thermally annealed at 950°C for 7.5 hours to obtain Eu3+ Doped YNbTiO 6 red light emitting phosphors.

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Abstract

The invention provides novel red light-emitting fluorescent powder and a preparation method thereof, wherein the fluorescent powder is obtained through doping Eu<3+> or Eu<3+> and Li<+> in YNbTiO6 substrate; when Eu<3+> is doped alone, the general chemical formula is Y1-xNbTiO6:xEu<3+> with the numeric area of x more than 0.001 and less than 0.35; when both Eu<3+> and Li<+> are doped, the general chemical formula is Y1-x-yNbTiO6:xEu<3+>, yLi<+> with the numeric area of x more than 0.001 and less than 0.35 and the numeric area of y more than 0.001 and less than 0.1. The preparation method includes the following steps: firstly, niobium pentaoxide is dissolved in hydrofluoric acid and then ammonia water is instilled in the solution for neutralization; secondly, after aging, filtration and cleaning, the niobium hydroxide deposit is dissolved in citric acid aqueous solution; thirdly, tetrabutyl titanate, yttrium nitrate, europium nitrate, lithium nitrate and ammonium nitrate which are added in the citric acid solution in turn are heated up and stirred; finally, sintering and thermal annealing treatments to the obtained precursor gel are completed. The red light-emitting fluorescent powder prepared by the invention has high color purity, high color rendering index and strong luminous intensity.

Description

technical field [0001] The invention relates to a novel red light-emitting fluorescent powder and a preparation method thereof, belonging to the field of luminescent material research. Background technique [0002] In recent years, Eu 3+ The research on the luminescent properties of red fluorescent activators is attracting attention, mainly because its characteristic emission peaks are rich in the orange-red region of visible light. 5 D. 0 → 7 f J Radiation jump. Especially Eu 3+ Doped Y 2 o 3 , Y 2 o 2 Red luminescent materials such as S have played an important role in various color display and lighting fields. [0003] With the rapid development of white LEDs, it is necessary to study luminescent materials that can be effectively excited by near-ultraviolet and blue light bands. At present, there are too few varieties of red light-emitting phosphors that can be applied practically, and the disadvantages of low luminous intensity, poor color purity, and poor col...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/78
Inventor 吕孟凯马谦张爱玉王兆光杨忠森周广军
Owner SHANDONG UNIV
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