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Synthetic rare earth doped nitric oxide fluorescent powder and preparation method thereof

A nitrogen oxide, rare earth doping technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of poor aging resistance of phosphors, low crystal phase purity of products, harsh synthesis conditions, etc., and achieve strong operability. , to avoid the formation of nitrogen oxides, the effect of a wide process window

Inactive Publication Date: 2013-07-03
IRICO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The Si-O-N system has stable physical and chemical properties and can effectively solve the problem of poor aging resistance of current phosphors after doping with rare earths. It is an excellent system for preparing green phosphors
via Eu 2+ The conversion efficiency of doped nitrogen oxide phosphor is above 90% and has a high quenching temperature, but the synthesis conditions of conventional methods are relatively harsh, and the crystal phase purity of the obtained product is low

Method used

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  • Synthetic rare earth doped nitric oxide fluorescent powder and preparation method thereof
  • Synthetic rare earth doped nitric oxide fluorescent powder and preparation method thereof
  • Synthetic rare earth doped nitric oxide fluorescent powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] According to Ba 1.96 SiO 4 : 0.04Eu weighed BaCO 3 3.868g, SiO 2 0.601g, Eu 2 o 3 0.070g and 2wt% reaction aid NH 4 Cl was mixed and fully ground (ball milled) and then placed in an alumina crucible, and the crucible was placed in a tube furnace, under H 2 Ba 1.96 SiO 4 :0.04Eu. According to Ba 0.98 Si 2 o 2 N 2 o 4 : The stoichiometric ratio of each element of 0.02Eu will be obtained Ba 1.96 SiO 4 : 0.04Eu ground and sieved and then mixed with 1.823g α-Si 3 N 4 And 3wt% reaction aid NH 4 Cl is mixed and ground (ball milled) and put into a molybdenum crucible, and the crucible is moved into a high-temperature tube furnace. 2 / H 2 Sinter at 1500°C for 3 hours in the atmosphere, cool to room temperature, take out, grind and sieve, wash and dry with ethanol to obtain blue-green phosphor Ba 0.98 Si 2 o 2 N 2 o 4 :0.02Eu.

Embodiment 2

[0032] According to Ca 2 SiO 4 Weigh CaO1.123g, SiO 2 0.601g was mixed and fully ground (ball milled) and then placed in an alumina crucible, placed in a tube furnace, sintered at 950°C for 5 hours in an Ar reducing atmosphere, then cooled to room temperature to obtain Ca 2 SiO 4 . According to Ca 0.97 Si 2 o 2 N 2 : The stoichiometric ratio of 0.03Eu elements will result in Ca 2 SiO 4 Grinding and sieving with α-Si 3 N 4 0.696g, Eu 2 o 3 0.070g and 1wt% reaction aid CaF 2 After mixing and grinding (ball milling), put it into a molybdenum crucible, and move the crucible into a high-temperature tube furnace. 2 / H 2Sinter at 1600°C for 3 hours in the atmosphere, cool to room temperature, take out, grind and sieve, wash and dry with ethylene glycol to obtain yellow-green phosphor Ca 0.97 Si 2 o 2 N 2 : 0.03Eu.

Embodiment 3

[0034] According to Sr 1.92 Li 0.04 SiO 4 : 0.04Eu, 0.04Ce weighed SrCO 3 2.834g, SiO 2 0.601g, Eu 2 o 3 0.070g, Ce(NO 3 )·6H 2 O 0.174g and charge compensator Li 2 CO 3 0.015g, after mixing and fully grinding (ball milling), put it in an alumina crucible, place the crucible in a tube furnace, and 2 / H 2 Sintered at 1500°C for 2 hours in a reducing atmosphere and then cooled to room temperature to obtain Sr 1.92 Li 0.04 SiO 4 : 0.04Eu, 0.04Ce. According to Sr 0.96 Li 0.02 Si 2 o 2 N 2 : 0.02Eu, the stoichiometric ratio of each element of 0.02Ce will be gained Sr 1.92 Li 0.04 SiO 4 : 0.04Eu, 0.04Ce ground and sieved with 1.425g α-Si 3 N and 1wt% reaction aid SrF 2 After mixing and grinding (ball milling), put it into a molybdenum crucible, and move the crucible into a high-temperature tube furnace. 2 Sinter at 1400°C for 5 hours in a protective atmosphere, cool to room temperature, take out, grind and sieve, wash and dry with ethanol aqueous solution to ...

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Abstract

The invention relates to synthetic rare earth doped nitric oxide fluorescent powder and a preparation method thereof, which is characterized in that the general chemical formula of the rare earth doped nitric oxide fluorescent powder is A1-xByOzN2 / 3+4 / 3y-2 / 3z : xRe, wherein A is one or the combination of two or more of Ca ion, Sr ion and Ba ion and comes from the oxide, carbonate or nitrate whichcontains A element; B is one or the combination of Si ion and A1 ion, at least contains Si ion and comes from the nitride which contains B element; Re is one or the combination of two or more of Eu ion, Ce ion, Dy ion and Mn ion and comes from the oxide, nitrate or acetate which contains Re element; and the relations of X is more than or equal to 0 and less than 1.0, Y is more than or equal to 1.0 and less than or equal to 2.0 and Z is more than 0 and less than or equal to 2.0 are satisfied. The luminescent material is of stable physical and chemical properties, strong thermal decay resistance and high quantum efficiency, is suitable for excitation of wavelength at 300nm-600nm and is widely applicable in LED lighting and display devices. The fluorescent powder is synthesized through two-step synthesis by taking cheap compounds as the materials and the fluorescent powder synthesized through the method under normal pressure is of pure phase.

Description

technical field [0001] The invention relates to a method for synthesizing rare earth-doped nitrogen oxide fluorescent powder, in particular to a method for synthesizing rare earth doped nitrogen oxide fluorescent powder by using common cheap compounds as raw materials under normal pressure. Background technique [0002] Phosphor-converted white light diodes (pc-wLEDs), which are expected to replace traditional incandescent lamps and become a new generation of daily lighting sources due to their excellent performances such as energy saving, environmental protection, and high efficiency, have attracted much attention from the academic community. The current mainstream method for realizing white light is blue light (440nm-470nm) chip combined with YAG:Ce phosphor. However, due to the lack of red components, the white LED produced by this mode has the defects of low color rendering and high color temperature, which greatly limits its application field. One of the schemes that c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/59C09K11/64
Inventor 赵金鑫
Owner IRICO
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