CN103571487A - Synthesis method of blue-light conversion material of white light-emitting diode (LED) - Google Patents

Synthesis method of blue-light conversion material of white light-emitting diode (LED) Download PDF

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Publication number
CN103571487A
CN103571487A CN201310547054.5A CN201310547054A CN103571487A CN 103571487 A CN103571487 A CN 103571487A CN 201310547054 A CN201310547054 A CN 201310547054A CN 103571487 A CN103571487 A CN 103571487A
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transition material
blue light
white led
synthetic method
led blue
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CN201310547054.5A
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韦胜国
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Abstract

The invention relates to a synthesis method of a blue-light conversion material of a white light-emitting diode (LED). The method comprises the following steps: evenly mixing oxides Y2O3, CeO2, Gd2O3 and AlO3; adding cosolvents HBO3 and CH3CH2OH to the mixed oxides, and encapsulating into an agate jar; putting the agate jar on a planetary ball mill and carrying out ball-milling at a constant speed; drying in an oven and loading in a corundum boat after ball-milling is ended; sintering in a carbon reduction atmosphere, drawing a charge after cooling, and grinding to obtain the conversion material YAG:Ce, Gd(Y3-x-yCexGdyAl5O12). The synthesis method disclosed by the invention is simple and easy to implement, and low in cost; the white LED with stable performance can be prepared from the obtained inorganic conversion material.

Description

A kind of synthetic method of White LED Blue Light transition material
Technical field
The present invention relates to luminescent material technical field, relate in particular to a kind of synthetic method of White LED Blue Light transition material.
Background technology
Early 1990s, Nakmura adopts MOCVD method successfully to prepare high brightness InGaN blue-ray LED, makes LED form the complete luminescence system of three primary colours.The blue light that the LED of take produces is excitaton source, coordinates suitable light-converting material, can obtain the white light LEDs that luminous efficiency is high and be suitable for throwing light on.This class white light source has the plurality of advantages such as driving voltage is low, the life-span is long, energy consumption is low, pollution-free, therefore, people estimate white light LEDs will replace incandescent, luminescent lamp, become lighting source of new generation.The light-converting material of preparing white light LEDs is divided into inorganic and organic two classes, and organic materials is with high-visibility pigment and metal chelate; Inorganic materials is with yttrium aluminum garnet (Y3A1.012, be called for short YAG) and alkaline earth sulfide, the rare earth doped fluor of silicate be main, after comprehensive various physics, chemistry and the characteristics of luminescence, YAG becomes first-selected luminescent material matrix.Because the blue-light-emitting Spectral matching of their absorption and excitation spectrum and InGaN chip, has met photon energy conversion requirement to greatest extent; Emmission spectrum scope is very wide, covers from the very wide visible light of a green one yellow orange light; Stokes shift is moderate, and luminous efficiency is high; Stable performance, radiation hardness.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of synthetic method of White LED Blue Light transition material.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of synthetic method of White LED Blue Light transition material, comprises the steps:
By oxide compound Y 2o 3, CeO 2, Gd 2o 3, A1 2o 3according to mass ratio, be that 1:1:1:1～1:1:1:3 evenly mixes;
In mixed mixture, add the fusing assistant HBO that relatively whole mixture quality is 20%～50% 3and CH 3cH 2oH also packs agate jar into;
Agate jar is placed on planetary ball mill at the uniform velocity ball milling;
Ball milling is complete dries and packs in corundum boat in baking oven;
Sintering under carbon reducing atmosphere, comes out of the stove after cooling, grinds and obtains transition material YAG:Ce, Gd (Y 3-x-yce xgd yal 5o 12).
On the basis of technique scheme, the present invention can also do following improvement.
Further, material therefor purity is: Y 2o 3(99.99%), CeO 2(99.99%), Gd 2o 3(99.99%), A1 2o 3(analytical pure), HBO 3(analytical pure), CH 3cH 2oH (analytical pure).
Described analytical pure (AR) refers to that principal constituent content is very high, purity higher interference impurity is very low, is applicable to technical analysis and chemical experiment.
Further, described by oxide compound Y 2o 3, CeO 2, Gd 2o 3, A1 2o 3in even mixing step, described oxide compound Y 2o 3, CeO 2, Gd 2o 3, A1 2o 3according to mass ratio, be that 1:1:1:1 mixes.
Further, described in mixed mixture, add the fusing assistant HBO that relatively whole mixture quality is 20%～50% 3and CH 3cH 2oH also packs in agate jar step, described fusing assistant HBO 3and CH 3cH 2the mass ratio of OH is 1:1～1:2.
Further, described agate jar is placed on planetary ball mill at the uniform velocity ball milling step, described planetary ball mill is with 300～500rmin -1speed ball milling and keep 2～3h.
Further, described ball milling is complete dries and packs in corundum boat in step in baking oven, and described oven temperature is 70～90 ℃.
Further, described under carbon reducing atmosphere in sintering step, described sintering temperature is 1200～1500 ℃.
The invention has the beneficial effects as follows: synthetic method of the present invention is simple and easy to implement, with low cost, and the inorganic transition material of gained all can the stable white light LEDs of processability.
Accompanying drawing explanation
Fig. 1 is the synthetic method schema of a kind of White LED Blue Light transition material of the present invention.
Embodiment
Below in conjunction with accompanying drawing, principle of the present invention and feature are described, example, only for explaining the present invention, is not intended to limit scope of the present invention.
As shown in Figure 1, a kind of synthetic method of White LED Blue Light transition material, comprises the steps:
By oxide compound Y 2o 3, CeO 2, Gd 2o 3, A1 2o 3according to mass ratio, be that 1:1:1:1～1:1:1:3 evenly mixes;
In mixed mixture, add the fusing assistant HBO that relatively whole mixture quality is 20%～50% 3and CH 3cH 2oH also packs agate jar into;
Agate jar is placed on planetary ball mill at the uniform velocity ball milling;
Ball milling is complete dries and packs in corundum boat in baking oven;
Sintering under carbon reducing atmosphere, comes out of the stove after cooling, grinds and obtains transition material YAG:Ce, Gd (Y 3-x-yce xgd yal 5o 12).
Embodiment 1:
Synthetic 10g transition material YAG:Ce, Gd (Y 3-x-yce xgd yal 5o 12): by 10g Y 2o 3, 10g CeO 2, 10g Gd 2o 3, 10g A1 2o 3oxide compound evenly mixes; In mixed oxide compound, add 4g fusing assistant HBO 3with 4g CH 3cH 2oH also packs agate jar into; Agate jar is placed on planetary ball mill with 300rmin -1speed ball milling keep 2h at the uniform velocity; Ball milling is complete dries and packs in corundum boat in 70 ℃ of baking ovens; 1200 ℃ of sintering under carbon reducing atmosphere, come out of the stove after cooling, grind and obtain transition material YAG:Ce, Gd (Y 3-x-yce xgd yal 5o 12).
Embodiment 2:
Synthetic 10g transition material YAG:Ce, Gd (Y 3-x-yce xgd yal 5o 12): by 10g Y 2o 3, 10g CeO 2, 10g Gd 2o 3, 10g A1 2o 3oxide compound evenly mixes; In mixed oxide compound, add 4g fusing assistant HBO 3with 6g CH 3cH 2oH also packs agate jar into; Agate jar is placed on planetary ball mill with 400rmin -1speed ball milling keep 2.5h at the uniform velocity; Ball milling is complete dries and packs in corundum boat in 80 ℃ of baking ovens; 1300 ℃ of sintering under carbon reducing atmosphere, come out of the stove after cooling, grind and obtain transition material YAG:Ce, Gd (Y 3-x-yce xgd yal 5o 12).
Embodiment 3:
Synthetic 10g transition material YAG:Ce, Gd (Y 3-x-yce xgd yal 5o 12): by 10g Y 2o 3, 10g CeO 2, 10g Gd 2o 3, 10g A1 2o 3oxide compound evenly mixes; In mixed oxide compound, add 7g fusing assistant HBO 3with 14g CH 3cH 2oH also packs agate jar into; Agate jar is placed on planetary ball mill with 500rmin -1speed ball milling keep 3h at the uniform velocity; Ball milling is complete dries and packs in corundum boat in 90 ℃ of baking ovens; 1500 ℃ of sintering under carbon reducing atmosphere, come out of the stove after cooling, grind and obtain transition material YAG:Ce, Gd (Y 3-x-yce xgd yal 5o 12).
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.

Claims (7)

1. a synthetic method for White LED Blue Light transition material, is characterized in that, comprises the steps:
By oxide compound Y 2o 3, CeO 2, Gd 2o 3, A1 2o 3according to mass ratio, be that 1:1:1:1～1:1:1:3 evenly mixes;
In mixed mixture, add the fusing assistant HBO that relatively whole mixture quality is 20%～50% 3and CH 3cH 2oH also packs agate jar into;
Agate jar is placed on planetary ball mill at the uniform velocity ball milling;
Ball milling is complete dries and packs in corundum boat in baking oven;
Sintering under carbon reducing atmosphere, comes out of the stove after cooling, grinds and obtains transition material YAG:Ce, Gd (Y 3-x-yce xgd yal 5o 12).
2. a kind of synthetic method of White LED Blue Light transition material according to claim 1, is characterized in that, material therefor purity is: Y 2o 3(99.99%), CeO 2(99.99%), Gd 2o 3(99.99%), A1 2o 3(analytical pure), HBO 3(analytical pure), CH 3cH 2oH (analytical pure).
3. a kind of synthetic method of White LED Blue Light transition material according to claim 1, is characterized in that, described in mixed mixture, adds the fusing assistant HBO that relatively whole mixture quality is 20%～50% 3and CH 3cH 2oH also packs in agate jar step, described fusing assistant HBO 3and CH 3cH 2the mass ratio of OH is 1:1～1:2.
4. a kind of synthetic method of White LED Blue Light transition material according to claim 1, is characterized in that, described agate jar is placed on planetary ball mill at the uniform velocity ball milling step, and described planetary ball mill is with 300～500rmin -1speed ball milling and keep 2～3h.
5. a kind of synthetic method of White LED Blue Light transition material according to claim 1, is characterized in that, described ball milling is complete dries and packs in corundum boat in step in baking oven, and described oven temperature is 70～90 ℃.
6. according to the synthetic method of a kind of White LED Blue Light transition material described in claim 1 to 5, it is characterized in that, described under carbon reducing atmosphere in sintering step, described sintering temperature is 1200～1500 ℃.
7. the White LED Blue Light transition material synthetic according to any method of claim 1 to 7.
CN201310547054.5A 2013-11-07 2013-11-07 Synthesis method of blue-light conversion material of white light-emitting diode (LED) Pending CN103571487A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109486490A (en) * 2018-11-29 2019-03-19 江苏博睿光电有限公司 Garnet-based superfine fluorescent powder and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8459832B2 (en) * 2008-09-10 2013-06-11 Samsung Electronics Co., Ltd. Light emitting device and system providing white light with various color temperatures

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8459832B2 (en) * 2008-09-10 2013-06-11 Samsung Electronics Co., Ltd. Light emitting device and system providing white light with various color temperatures

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
褚明辉等: "高掺杂Ce，Gd(Y3-x-yCexGdy)Al5O12荧光粉的发光下降及温度猝灭特性", 《无机化学学报》, vol. 26, no. 2, 28 February 2010 (2010-02-28), pages 183 - 189 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109486490A (en) * 2018-11-29 2019-03-19 江苏博睿光电有限公司 Garnet-based superfine fluorescent powder and preparation method thereof

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Application publication date: 20140212