Preparation method of yttrium aluminum garnet yellow fluorescent powder for white light LED

A technology of yttrium aluminum garnet type and yellow phosphor, which is applied in chemical instruments and methods, luminescent materials, and the use of gas discharge lamps. Effects of preventing particle agglomeration, excellent luminous performance, and short synthesis time

Active Publication Date: 2013-06-05
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adding flux related to the present invention to promote YAG:Ce 3+ The literature on phase formation and particle size control mainly includes: the Chinese invention patents whose authorized announcement numbers are CN1277901C and CN1318540C use chemical co-precipitation method or sol-gel method to control the preparation of small particle size precursors, and then add flux in solid form, It needs a certain mixing time, it is not easy to mix evenly, and the preparation process of the precursor is complicated and difficult to control
In 2007, Huang Yan also used the precipitation method to make the precursor, and then mixed the obtained precursor with a certain amount of inorganic salt to grind evenly, and then calcined at 1500°C for 2 hours to obtain a high-performance YAG product with a particle size of 3~5μm ; In 2010, Huan Jiao et al. used the sol-gel method to prepare the precursor, and then mixed the precursor with a certain amount of LiF. After grinding and mixing evenly, the phase could be formed at 700°C, but the luminescence was poor, and the sol-gel method It takes a long time and it is difficult to get industrial application (Powder Technology, 2010,198:229–232)
[0005] The existing solution combustion method uses the heat release of the redox reaction itself to complete the reaction. Once the reaction is initiated, no heat provided by the outside is needed. It is characterized by uniform mixing of component ions, fast reaction speed, and short time. The high temperature can be reached in an instant, but this method has the problems of serious particle sintering and agglomeration, large particles and irregular shape

Method used

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  • Preparation method of yttrium aluminum garnet yellow fluorescent powder for white light LED
  • Preparation method of yttrium aluminum garnet yellow fluorescent powder for white light LED
  • Preparation method of yttrium aluminum garnet yellow fluorescent powder for white light LED

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Embodiment 1

[0036] Weigh out 0.0258 g CeO 2 , placed in 20 ml of 1:1 nitric acid solution, added dropwise 5 ml of 30% hydrogen peroxide, heated and stirred until completely dissolved, then weighed 0.3375 g Al powder and 0.8306 g Y 2 O 3 , added to it, heated and dissolved to obtain a mixed solution of nitrates. Add 1.0440 g KF and 1.8600 g ethylene glycol to the mixed solution obtained above, heat and stir to dissolve it, and concentrate it to a nearly viscous state, then put it in a microwave oven to heat and ignite, and the combustion product is put into a mixture of nitrogen and hydrogen. Mixed gas (H 2 : 5 V%) in a tubular atmosphere furnace at 1100 °C for 120 min. The heat-treated product is washed, dried, ground and sieved to obtain Y 2.94 Al 5 O 12 : 0.06 Ce 3+ phosphor.

Embodiment 2

[0038] Weigh out 0.0258 g CeO 2 , placed in 20 ml of 1:1 nitric acid solution, added dropwise 5 ml of 30% hydrogen peroxide, heated and stirred until completely dissolved, then weighed 0.3375 g Al powder and 0.8306 g Y 2 O 3 , added to it, heated and dissolved to obtain a mixed solution of nitrates. Add 1.053 g NaCl and 1.8600 g ethylene glycol to the mixed solution obtained above, heat and stir to dissolve it, and concentrate it to a nearly viscous state, then put it in a microwave oven to heat and ignite, and the combustion product is put into a mixture of nitrogen and hydrogen. Mixed gas (H 2 : 5 V%) in a tubular atmosphere furnace at 1100 °C for 120 min. The heat-treated product is washed, dried, ground and sieved to obtain Y 2.94 Al 5 O 12 : 0.06 Ce 3+ phosphor.

Embodiment 3

[0040] Weigh out 0.0258 g CeO 2 , placed in 20 ml of 1:1 nitric acid solution, added dropwise 5 ml of 30% hydrogen peroxide, stirred while heating until completely dissolved, and then weighed 0.975g of Al(OH) 3 and 0.8306 g Y 2 O 3 , added to it, heated and dissolved to obtain a mixed solution of nitrates. Add 1.0440 g KF and 2.5000 g glycine to the mixed solution obtained above, heat and stir to dissolve it, and concentrate it to a nearly viscous state, then put it into a microwave oven to heat and ignite, and the combustion product is put into a mixed gas of nitrogen and hydrogen. (H 2 : 5 V%) in a tubular atmosphere furnace at 1100 °C for 120 min. The heat-treated product is washed, dried, ground and sieved to obtain Y 2.94 Al 5 O 12 : 0.06 Ce 3+ phosphor.

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Abstract

The invention relates to a preparation method of yttrium aluminum garnet yellow fluorescent powder for white light LED (light-emitting diode). The method comprises the steps of: according to a stoichiometric ratio of each metallic element in Y3-x-yGdxAl5O12: yCe<3+>, preparing a mixed nitrate solution of metals contained in a target product; adding a soluble salt, an organic fuel and ammonium nitrate, heating the solution for dissolution till approximately a sticky state, conducting microwave irradiation so as to initiate self-propagating combustion; carrying out washing, drying, grinding andsieving, thus obtaining the yttrium aluminum garnet yellow fluorescent powder of a necessary particle size. The yttrium aluminum garnet yellow fluorescent powder prepared in the invention has controllable particle size, uniform size, regular appearance, and excellent light-emitting performance, and has the advantages of convenient implementation, simple equipment, short synthesis time, no need for long-time material mixing, high-temperature calcination, and ball-milling crushing. Therefore, the preparation method of the invention is a rapid and energy-saving new method for controlling the synthesis of yttrium aluminum garnet yellow fluorescent powder of different particle sizes.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and particularly relates to a preparation method of rare earth luminescent materials. Background technique [0002] Light-emitting diode (LED) is a new type of solid-state lighting electric light source, which has the advantages of high efficiency and energy saving, green environmental protection, long life, small size, shock resistance, fast luminous response and low operating voltage. and other fields have been widely used, and now white LED has begun to challenge the solid position of incandescent lamps and fluorescent lamps in the lighting field, and is expected to gradually replace them, thus showing a huge market prospect. [0003] There are two main ways for white light LEDs to generate white light: the first is to combine red, green and blue LEDs to generate white light; the second is to use LEDs to excite light-converting phosphors and mix them to form white light. There are...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/80
CPCY02B20/181Y02B20/00
Inventor 陈伟凡柯于胜吴骏飞刘铭
Owner NANCHANG UNIV
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