Nitrogen oxide red fluorescent powder and preparation method thereof

A technology of red phosphors and nitrogen oxides, applied in chemical instruments and methods, luminescent materials, sustainable buildings, etc., can solve problems such as excellent color rendering index, lack of red light, etc., and achieve wide process window, The effect of simple operation and low raw material price

Inactive Publication Date: 2013-03-13
IRICO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

YAG:Ce phosphor is currently the most widely used powder in white LEDs. However, due to the lack of red light, it is difficult to make LEDs with excellent color rendering index when superimposed with blue light.

Method used

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  • Nitrogen oxide red fluorescent powder and preparation method thereof
  • Nitrogen oxide red fluorescent powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Follow Y 5.97 Si 3 N 4 o 9 :0.06Sm 3+ Stoichiometric ratio weighs Y 2 o 3 、Si 3 N 4 、Sm 2 o 3 , and 5wt% flux (i.e. catalyst) NaF is placed in a mortar and thoroughly ground and mixed evenly, then placed in a graphite crucible, the crucible is placed in a carbon tube vacuum furnace, under protective gas N / H=3:1 ( (volume ratio) at a rate of 10°C / min to 1550°C, then keep warm for 12 hours, then cool down to room temperature naturally, take out, grind and sieve to obtain a powder with a particle size parameter D50=8 microns, and then wash with 10% dilute hydrochloric acid, And after drying at 80°C for 2 hours, the red phosphor Y was obtained 5.97 Si 3 N 4 o 9 :0.06Sm 3+ .

[0021] Such as figure 1 , for Y 5.97 Si 3 N 4 o 9 :0.06Sm 3+ The emission spectrum and excitation spectrum of the figure; the figure shows that the sample Y is irradiated with 404nm excitation light 5.94 Si 3 N 4 o 9 :0.06Sm 3+ , to obtain the emission spectrum of the fluoresc...

Embodiment 2

[0024] According to YTb 4.9 Si 3 N 4 o 9 :0.1Sm 3+ Stoichiometric ratio weighs Y 2 o 3 , Tb 4 o 7 、Si 3 N 4 、Sm 2 o 3 , and 3wt% flux (i.e. catalyst) NaF is placed in a mortar and thoroughly ground and mixed evenly, then placed in a graphite crucible, the crucible is placed in a carbon tube vacuum furnace, under protective gas N / H=9: 1 ( volume ratio) at a rate of 15°C / min to 1700°C, after 14 hours of heat preservation, it was naturally cooled to room temperature, taken out, ground and sieved to obtain a powder with a particle size parameter D50=12 microns, then washed with 5% dilute hydrochloric acid and dried at 60 After drying at ℃ for 5 hours, the red phosphor YTb can be obtained 4.9 Si 3 N 4 o 9 :0.1Sm 3+ .

Embodiment 3

[0026] According to TbGd 4.99 Si 3 N 4 o 9 :0.01Sm 3+ Stoichiometric ratio weighs Tb 4 o 7 、Gd 2 o 3 、Si 3 N 4 、Sm 2 o 3 , and 1wt% flux (i.e. catalyst) H 3 BO 3 Put it in a mortar, grind and mix well, then put it in a graphite crucible, place the crucible in a carbon tube vacuum furnace, and raise the temperature at a rate of 5°C / min in a protective gas N / H=97:3 (volume ratio) to 1650°C, keep warm for 10 hours, then cool naturally to room temperature, take out, grind and sieve to obtain a powder with a particle size parameter D50=10 microns, then wash with 20% dilute hydrochloric acid and dry at 90°C for 3 hours to obtain the red phosphor TbGd 4.99 Si 3 N 4 o 9 :0.01Sm 3+ .

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Abstract

The invention relates to a nitrogen oxide red fluorescent powder and a preparation method thereof. The fluorescent powder is characterized by having a chemical formula of A6-xSi3N4O9:Sm<3+>; A represents Y, Tb or Gd, or a mixture of the three; and x satisfies the relation of: 0<x<=0.1. The invention has the following advantages and beneficial effects: 1, the method provided by the invention has simple operation, low price of raw materials and wide process window, and is suitable for large-scale industrial production; and 2, the invention provides a novel red fluorescent material. The invention relates to the nitrogen oxide red fluorescent powder and the preparation method thereof. Common cheap compounds are used as raw materials and prepared into the red luminescent fluorescent material through a high temperature sintering method. The fluorescent material is sintered by a high temperature solid sintering method, and is a potential fluorescent material for white LED.

Description

technical field [0001] The invention relates to a nitrogen oxide red fluorescent powder and a preparation method thereof. Background technique [0002] At present, the preparation method of white light LEDs for lighting mainly uses blue light chips to excite yellow phosphor powder. In 1997, Nichia first reported Y 3 Al 5 o 12 : Ce 3+ (YAG:Ce) Yellow Phosphor Material with Blue InGaN Chipset and White Light Emitting Device. YAG:Ce phosphor is currently the most widely used powder in white LEDs. However, due to the lack of red light, it is difficult to produce LEDs with excellent color rendering index when superimposed with blue light. [0003] The red phosphors that have appeared recently can all be in the blue light region and are easily excited, thereby improving the color rendering index. Nitrogen oxides have attracted more attention due to their strong thermal and chemical stability. Contents of the invention [0004] One of the objects of the present invention i...

Claims

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Application Information

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IPC IPC(8): C09K11/79
CPCY02B20/181Y02B20/00
Inventor 苏醒宇
Owner IRICO
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