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Preparation method of yellow fluorescent powder for light-emitting diode (LED)

A technology of yellow fluorescent powder and light-emitting diodes, applied in the direction of luminescent materials, chemical instruments and methods, electrical components, etc., can solve the problems of low luminous rate, high synthesis temperature, high hardness, etc., achieve low temperature, good uniformity, The effect of small particle size

Inactive Publication Date: 2013-05-22
HENAN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a kind of adopting sol-gel method (sol-gol) and microwave method to solve problems such as coarse particles, high hardness, low luminous rate, high synthesis temperature and large energy consumption in the prior art. Metal nitrate is used as raw material, cerium ion is used as activator, and citric acid is used as complexing agent to prepare Y 3 Al 5 o 12 : Ce 3+ The Yellow Phosphor Method

Method used

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  • Preparation method of yellow fluorescent powder for light-emitting diode (LED)
  • Preparation method of yellow fluorescent powder for light-emitting diode (LED)
  • Preparation method of yellow fluorescent powder for light-emitting diode (LED)

Examples

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Embodiment 1

[0019] Use Ce oxides or nitrates as activators, weigh Y, Al, Ce oxides or Y, Al, Ce nitrates according to a certain material ratio, and dissolve Y, Al, Ce oxides in nitric acid Or Y, Al, Ce nitrates are dissolved in nitric acid or water to make Y, Al, Ce nitrates; add citric acid to the Y, Al, Ce nitrate solutions and mix well; Stir in a water bath until the precursor is formed; put the generated precursor in a vacuum oven at 120°C and dry for 12 to 24 hours, so that the water is gradually volatilized and a large amount of gas is released, and the sample becomes a xerogel; the xerogel is taken out, and the After the dry gel is ground in an agate mortar, it is sintered in a high-temperature resistance furnace at a temperature of 800° C. to 1200° C. and kept for 1 to 4 hours to obtain a sample.

[0020] Said weighing the oxide of Y, Al, Ce or the nitrate of Y, Al, Ce, wherein the material ratio of metal ion is Y: Al: Ce=3-x: 5: x, wherein x is between 0.04~ 0.07

[0021] The a...

Embodiment 2

[0026] Weigh Y according to the stoichiometric ratio 1.47:5:0.06 2 o 3 (purity ≥ 99.99%), Al(NO 3 ) 3 9H 2 O (purity ≥ 99%) and Ce (NO 3 ) 3 ·6H 2 O (purity ≥ 99.99%). Will Y 2 o 3 Soluble in dilute nitric acid, dubbed Y(NO 3 ) 3 solution. Al(NO 3 ) 3 9H 2 O was added to the stirring Y (NO 3 ) 3 solution, the mixture is added to the dissolved Ce(NO 3 ) 3 in solution. Add citric acid to the metal solution, the ratio of citric acid to total metal ions is 1:1; when the above mixed solution is placed in a household microwave oven for microwave heating to prepare the precursor, the heating power is 120W-385W, and the The time is between 2 minutes and 4 minutes. Put the generated precursor into a vacuum drying oven at 120°C for 12 hours to make the moisture gradually volatilize and release a large amount of gas, and the sample becomes a xerogel. The sample was taken out, ground in an agate mortar, and then sintered in a high-temperature resistance furnace at 900...

Embodiment 3

[0028]Weigh Y according to the stoichiometric ratio 1.48:5:0.04 2 o 3 (purity ≥ 99.99%), Al(NO 3 ) 3 9H 2 O (purity ≥ 99%) and Ce (NO 3 ) 3 ·6H 2 O (purity ≥ 99.99%). Will Y 2 o 3 Soluble in dilute nitric acid, dubbed Y(NO 3 ) 3 solution. Al(NO 3 ) 3 9H 2 O was added to the stirring Y (NO 3 ) 3 solution, the mixture is added to the dissolved Ce(NO 3 ) 3 in solution. Add citric acid to the metal solution, the ratio of citric acid to total metal ions is 1:1; stir in a water bath at 85°C until the precursor is formed; put the stirred precursor into a vacuum oven at 120°C After 12 hours, the water is gradually volatilized and a large amount of gas is released, and the sample becomes a xerogel. The sample was taken out, ground in an agate mortar, and then sintered in a high-temperature resistance furnace at 900° C. and kept warm for 2 hours to obtain a yellow phosphor for light-emitting diodes. All the other are with embodiment 1.

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Abstract

The invention discloses a method for preparing Y3Al5O12:Ce<3+> yellow fluorescent powder by adopting a sol-gel method and a microwave method. The method of the invention comprises the following steps: taking oxides or nitrates of Y and Al as raw materials and an oxide or nitrate of Ce as an activating agent, weighing the oxides or nitrates of Y, Al and Ce, and dissolving in nitric acid or water to prepare the nitrates of Y, Al and Ce; adding citric acid, and evenly mixing; stirring the mixed liquor in 80-85 DEG C water batch until forming a precursor, or placing and heating the mixed liquor in a household microwave oven to obtain the precursor; drying the precursor to form xerogel; and taking out the xerogel, levigating the xerogel in a mortar, sintering in a high-temperature resistance furnace and carrying out heat preservation to prepare a sample. The invention has the advantages that the required reaction temperature is low, the energy consumption is small, the component content can be accurately controlled, the reacting components can be mixed in an atom level, and the synthesis process is simple and practicable and is favorable for industrialized production.

Description

technical field [0001] The invention belongs to an aluminate luminescent material and a preparation method thereof, in particular to a preparation method of a yellow fluorescent powder for a light-emitting diode. Background technique [0002] The yellow fluorescent powder involved in the present invention is yttrium aluminum garnet structure (YAG). Yttrium aluminum garnet is a rare earth aluminate garnet synthesized by the reaction of yttrium oxide and aluminum oxide. It belongs to the cubic crystal system. It is a crystal with high hardness and high melting point. It has good mechanical strength and chemical stability. , Thermal conductivity, is a single crystal material with excellent performance. It is precisely because of these excellent properties of YAG that it shows excellent application prospects no matter it is used as a structural material or a functional material. In addition, YAG powder is doped with Ce 3+ , Tb 3+ 、Eu 3+ Rare earth ions can also be used as u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/80H01L33/00
Inventor 关荣锋赵文卿李帅谋
Owner HENAN POLYTECHNIC UNIV