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High-power warm-white light solid illumination SiAlON fluorescent transparent ceramic and preparation method thereof

A solid-state lighting, transparent ceramic technology, applied in energy-saving lighting, chemical instruments and methods, luminescent materials, etc., can solve the problem that it is difficult to ensure the elimination of glass phase, the density is only 90%, the reduction of glass is equal, and the repeatability is achieved. Strong, excellent mechanical properties, good thermal conductivity

Active Publication Date: 2018-12-18
ANHUI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2013, Y.J.Park et al prepared Ca-α-sialon:Eu with different components by pressure sintering at 1800-2000°C 2+ fluorescent ceramics, but the highest density of the sample is only 90% [J.Kor.Ceram.Soc.,2013,50 4 280-287]
In 2002, J.Krevel et al prepared (Ca 0.3125 Ce 0.209 )-α-sialon fluorescent transparent ceramics, but Ca-α-sialon:Eu 2+ Fluorescent transparent ceramics have not been reported [J.Solid State Chem.,2002,165 19-24]
Although the patent (CN201510174020.5) has disclosed Ca-α-sialon:Eu 2+ A method for preparing fluorescent transparent ceramics, but this patent uses a conventional ratio, which is difficult to ensure that most of the glass phase is eliminated
The patent (CN201110178303.9) discloses adding additional nitrides on the basis of the conventional ratio to reduce the glass phase and obtain Ca 2+ The preparation method of stable α-sialon translucent ceramics, but there is no report on the addition of rare earth luminescent ions to obtain luminescent properties

Method used

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  • High-power warm-white light solid illumination SiAlON fluorescent transparent ceramic and preparation method thereof
  • High-power warm-white light solid illumination SiAlON fluorescent transparent ceramic and preparation method thereof
  • High-power warm-white light solid illumination SiAlON fluorescent transparent ceramic and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] α-Si with an oxygen content of 1.5wt% 3 N 4 , AlN with an oxygen content of 1.0 wt%, α-Al 2 o 3 , CaCO 3 and Eu 2 o 3 as raw material, according to Ca m / 2-x-yv / 2 Si 12-m-n Al m+n o n N 16-n :xEu 2+ ,y M v+ The stoichiometric ratio of (m=0.8, n=1.0, x=0.02, y=0) selects the above-mentioned raw materials with a total weight of 50 g, mixes them, and adds 2.5 g of AlN to the mixture, and puts the above-mentioned raw materials in a plastic bottle mixed with Si 3 N 4 The ball is the ball milling medium, the mass ratio of the ball to the material is 4:1, add 400ml of absolute ethanol, and roll the ball mill for 24 hours to obtain the slurry; the slurry is evaporated to dryness in a rotary evaporator at 60°C, and then put into a vacuum drying oven to vacuum Dry for at least 24 hours, then take it out, grind for 20 minutes, and pass through a 100-mesh sieve to obtain the undersize; put the sieved undersize into a graphite mold with a diameter of 48 mm, then put it ...

Embodiment 2

[0036] α-Si with an oxygen content of 1.5wt% 3 N 4 , AlN with an oxygen content of 1.0 wt%, α-Al 2 o 3 , CaCO 3 、Eu 2 o 3 and Y 2 o 3 as raw material, according to Ca m / 2-x-yv / 2 Si 12-m-n Al m+n o n N 16-n :xEu 2+ ,y M v+The stoichiometric ratio of (m=0.8, n=1.0, x=0.02, y=0.05) selects the above-mentioned raw materials with a total weight of 50 g, and additionally adds 20 g of AlN to the mixture, mixes the above-mentioned raw materials in a plastic bottle, and Si 3 N 4 The ball is the ball milling medium, the ball-to-material ratio is 4:1, add 400ml of absolute ethanol, and roll the ball mill for 24 hours to obtain the slurry; the slurry is evaporated to dryness in a rotary evaporator at 60°C, and then placed in a vacuum drying oven for vacuum drying At least 24 hours, then take it out, grind for 20min, and pass through a 100-mesh sieve to obtain the undersize; put the sieved undersize into a graphite mold with a diameter of 48mm, and then put it into a hot-pr...

Embodiment 3

[0039] α-Si with an oxygen content of 1.5wt% 3 N 4 , AlN with an oxygen content of 1.0 wt%, α-Al 2 o 3 , CaCO 3 、Eu 2 o 3 and Sc 2 o 3 as raw material, according to Ca m / 2-x-yv / 2 Si 12-m-n al m+n o n N 16 -n:xEu 2+ ,yM v+ The stoichiometric ratio of (m=1.6, n=2.0, x=0.04, y=0.03) is selected as a total weight of 50 g of the above raw materials, and an additional 16 g of Si is added to the mixture 3 N 4 and 4gAlN complex, mix the above raw materials in a plastic bottle, and use Si 3 N 4 The ball is the ball milling medium, the ball-to-material ratio is 4:1, add 400ml of absolute ethanol, and roll the ball mill for 24 hours to obtain the slurry; the slurry is evaporated to dryness in a rotary evaporator at 60°C, and then placed in a vacuum drying oven for vacuum drying At least 24 hours, then take it out, grind for 20min, and pass through a 100-mesh sieve to obtain the undersize; put the sieved undersize into a graphite mold with a diameter of 48mm, and then put...

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Abstract

The invention relates to high-power warm-white light solid illumination SiAlON fluorescent transparent ceramic and a preparation method thereof, wherein the method includes: 1) according to the general formula of Ca<m / 2-x-yv / 2>Si<12-m-n>Al<m+n>O<n>N<1>6-n: xEu<2+>, yM<v+>, wherein v refers to chemical valence, 0.8 <= m <= 2.0, 1.0 <= n <= 2.0, 0 < x <= m / 4 and 0 <= y <= m / 2v-2x / v, mixing alpha-Si3N4, AlN, alpha-Al2O3, CaCO3, Eu2O3 and a raw material containing M to form a mixture A, and adding a mixture B with mixing, wherein the mixture B includes AlN and alpha-Si3N4, the mass of the mixtureB is 5-50% of the mixture A and the weight ratio of the Si3N4 to AlN in the mixture B is 0-5:1; 2) ball-milling and drying the mixture and sintering the mixture through hot pressed sintering or sparkplasma sintering to obtain a sintered product; 3) cutting and grinding the sintered product and polishing the sintered product to a mirror surface, thus obtaining Ca-alpha-sialon: Eu<2+> fluorescent transparent ceramic, which has broadband transmission under activation by blue light, is 570-600 nm in main wavelength and is adjustable in wavelength. The method has simple process and good repeatability. The fluorescent transparent ceramic has high heat conductivity and excellent heat quenching performance, and is suitable for high-power warm-white light solid illumination.

Description

technical field [0001] The invention relates to a SiAlON fluorescent transparent ceramic for high-power warm white solid-state lighting and a preparation method thereof, belonging to the field of rare earth luminescent materials and solid-state lighting preparation. Background technique [0002] Solid-state lighting has the advantages of energy saving and environmental protection, high luminous efficiency, long life, high reliability, and small size. It is the green light source with the most development potential. White LED lighting is currently the mainstream of solid-state lighting, and the combination of "blue LED chip + yellow phosphor" is the most common way to achieve white LED lighting. However, the further development of high-power white LEDs is limited by the epoxy resin or silicone encapsulation materials used, which are prone to aging, poor high temperature resistance, and the resulting decrease in LED luminous efficacy, color shift, and shortened lifespan. Ther...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/584C04B35/622C04B35/626C09K11/77
CPCC04B35/584C04B35/622C04B35/62605C04B2235/3208C04B2235/3217C04B2235/3224C04B2235/3865C04B2235/6562C04B2235/6567C04B2235/9653C09K11/7728Y02B20/00
Inventor 杨章富徐刘鑫王燕王金梅花清照戴紫阳
Owner ANHUI UNIV OF SCI & TECH
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