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A kind of rare earth ion co-doped aluminosilicate novel green light phosphor and preparation method thereof

A technology of aluminosilicate and rare earth ions, which is applied in the field of rare earth ion co-doped aluminosilicate new-type green phosphors and its preparation, to achieve fine and uniform particles, good surface morphology, and few powder surface defects Effect

Active Publication Date: 2016-08-17
HARBIN INST OF TECH SHENZHEN GRADUATE SCHOOL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, by adding boric acid as a flux, a high-temperature solid-state method was used to prepare Ce 3+ ,Tb 3+ Co-doped mullite-based phosphors have not yet appeared

Method used

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  • A kind of rare earth ion co-doped aluminosilicate novel green light phosphor and preparation method thereof
  • A kind of rare earth ion co-doped aluminosilicate novel green light phosphor and preparation method thereof
  • A kind of rare earth ion co-doped aluminosilicate novel green light phosphor and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Weigh 5.998g (0.588mol) of alumina, 2.352g (0.392mol) of silicon dioxide, and 1.496g (0.02mol) of terbium oxide, mix them, and grind them in an agate mortar for 30 minutes. Pour the fully and uniformly mixed raw materials into a boron nitride crucible, place a corundum sheet under the crucible, put it into a high-temperature tube furnace for sintering, and introduce a reducing atmosphere of 95% N 2 +5%H 2 , set the sintering temperature to 1470°C, and the holding time to 5h. After the furnace cavity is cooled to room temperature, take out the sample and crush and grind for about 30 minutes to obtain Al 6 Si 2 o 13 : Tb phosphor. At this time Tb 3+ The doping concentration is 8mol%, the excitation and emission spectra are as figure 1 shown.

Embodiment 2

[0045] Weigh 5.918g (0.5802mol) of alumina, 2.321g (0.3868mol) of silicon dioxide, 1.496g (0.02mol) of terbium oxide, 0.2236g (0.013mol) of cerium oxide, mix them, and grind them in an agate mortar for 30min . Pour the fully and uniformly mixed raw materials into a boron nitride crucible, place a corundum sheet under the crucible, put it into a high-temperature tube furnace for sintering, and introduce a reducing atmosphere of 95% N 2 +5%H 2 , the sintering temperature is 1470°C, and the holding time is 5h. After the furnace cavity is cooled to room temperature, take out the sample and crush and grind for about 30 minutes to obtain Al 6 Si 2 o 13 : Tb, Ce green phosphor. At this time Ce 3+ and Tb 3+ The doping concentrations are 1.3mol% and 8.0mol%, respectively, and the excitation and emission spectra are as figure 2 shown. With 297nm as the excitation wavelength, the luminous quantum efficiency of the phosphor is 24.21%, and it has good thermal stability: the lumin...

Embodiment 3

[0047] Weigh 5.918g (0.5802mol) of alumina, 2.321g (0.3868mol) of silicon dioxide, 1.496g (0.02mol) of terbium oxide, 0.2236g (0.013mol) of cerium oxide, mix them, and grind them in an agate mortar for 30min . Pour the fully and uniformly mixed raw materials into a boron nitride crucible, place a corundum sheet under the crucible, put it into a high-temperature tube furnace for sintering, and introduce a reducing atmosphere of 95% N 2 +5%H 2 , the sintering temperature is 1470°C, and the holding time is 5h. After the furnace cavity is cooled to room temperature, take out the sample and crush and grind for about 30 minutes to obtain Al 6 Si 2 o 13 : Tb, Ce green phosphor; followed by 15wt% SiO 2 Coating treatment: specifically use the hydrolysis of tetraethyl orthosilicate (TEOS) in acidic solution to produce Si(OH) 4 , and then heat treatment at 600°C for 2 hours, so that the Si(OH) on the surface of the phosphor particles 4 Transformation into continuous dense amorphou...

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Abstract

The invention provides a rare earth ion co-doped aluminosilicate novel green glow fluorescent powder and a preparation method thereof, and belongs to the technical field of luminescent materials. The chemical constitution of the green glow fluorescent powder is aAl2O3.bSiO2.cCeO2.dTb4O7, wherein a, b, c and d are mole fractions; a / b is equal to 3 / 2; c is larger than or equal to 0 and less than or equal to 2.0%; d is larger than or equal to 0 and less than or equal to 5.0%; c and d are not 0 at the same time. The preparation method comprises the following steps: weighing raw materials according to the stoichiometric proportion of the elements in the chemical formula; fully mixing the raw materials; conducting ball milling on the raw materials at indoor temperature; putting the sample conducted by full ball milling in a high-temperature pipe furnace pumped by reducing atmosphere; calcining the sample for 2-6 hours at 1450-1550 DEG C; taking the sample out for crushing grinding after the furnace chamber is cooled to indoor temperature; adding H3BO3 flux, water washing or / and SiO2 coating treatment in following to obtain the fluorescent powder. The fluorescent powder prepared from the method is favorable in crystallinity and particle surface, high in luminous intensity (particularly excellent in temperature resistance), and suitable for being used as ultraviolet light excited LED green glow fluorescent powder.

Description

technical field [0001] The invention belongs to the technical field of preparation of LED luminescent materials, and in particular relates to a novel green fluorescent powder of aluminosilicate co-doped with rare earth ions and a preparation method thereof. Background technique [0002] White light-emitting diodes (WLEDs) are gradually replacing traditional lighting sources and becoming a new generation of lighting sources due to their advantages of high efficiency, long life, energy saving and environmental protection. Phosphor powder can absorb ultraviolet / near ultraviolet or blue light and then emit visible light, which is the key material in LED solid-state lighting technology. At present, there are three main ways to realize white light: (1) package red, green, and blue LED chips together, and obtain white light by mixing various colors of light; (2) blue LED chips excite yellow light phosphors, yellow light and blue light Mix to obtain white light; (3) The ultraviolet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/64
Inventor 汪桂根董立文韩杰才杨奇
Owner HARBIN INST OF TECH SHENZHEN GRADUATE SCHOOL
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