CN103571488A - Preparation method of co-doped single crystal fluorescent material of light-emitting diode (LED) - Google Patents
Preparation method of co-doped single crystal fluorescent material of light-emitting diode (LED) Download PDFInfo
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- CN103571488A CN103571488A CN201310547481.3A CN201310547481A CN103571488A CN 103571488 A CN103571488 A CN 103571488A CN 201310547481 A CN201310547481 A CN 201310547481A CN 103571488 A CN103571488 A CN 103571488A
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- fluorescent material
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Abstract
The invention relates to a preparation method of a co-doped single crystal fluorescent material of a light-emitting diode (LED), and belongs to the technical field of luminescent materials. The method comprises the following steps: adopting a medium-frequency induction pulling method; pre-sintering and drying Y2O3, Al2O3, CeO2, Eu2O3 and Gd2O3 powder in air; mixing and evenly pressing the powder into a block body; pre-sintering at a constant temperature; loading the block body into an iridium crucible to carry out crystal growth, so as to obtain the co-doped single crystal fluorescent material (Cex, GdyY1-x-y)3Al5O12 (x=0.01 and y=0.3), and (Cex, EuyY1-x-y)3Al5O12 (x=y=0.01). The preparation method disclosed by the invention is simple; the obtained co-doped single crystal fluorescent material has high red light emission capability, and can be applied to preparation of a white LED with high color rendering indexes.
Description
Technical field
The present invention relates to luminescent material technical field, relate in particular to a kind of LED codoped single crystal fluorescent material preparation method.
Background technology
Semi-conductor White-light LED illumination is 21 century to have one of high-technology field of development prospect most.As the 4th generation lighting source, LED has solidification, volume is little, thermal value is low, current consumption is little, the life-span is long, speed of response is fast and the advantage such as environmental protection, will be widely used in the fields such as general illumination and backlight.At present, LED enjoys the whole world to attract attention in the prospect of illumination market, and manufactures the active demand that has become white light LEDs development towards high-level efficiency, high color rendering index (CRI), low colour temperature, the large power white light LED of general illumination application.
In the preparation process of white light LED part, fluorescent material is a very important gordian technique, and the performance of fluorescent material is directly determining the performances such as luminous efficiency, efficiency of conversion, chromaticity coordinates, colour temperature and color developing of white light LEDs.At present, the white-light LED fluorescence material of widespread use mainly be take fluorescent material as main body, and commercialization white light LEDs product be take blue chip and Ce:YAG phosphor combination, and to produce white light be Developing mainstream.Present stage, company and research institution all concentrate on fluorescent material mostly to the research of white light LEDs fluorescent material both at home and abroad, and the fluorescent material of exploitation high brightness, high-luminous-efficiency, high-color rendering has become the study hotspot of white light LEDs field fluorescent material.Yet, towards the phosphor material powder of large power white light LED illumination, but exist following problems to fail effectively to be solved: the homogeneity of fluorescent powder grain and dispersion is difficult to obtain sound solution always; Fluorescent material physical and chemical performance is poor, makes its light decay larger for a long time under the high radiation parameter of high temperature, and the white light LEDs life-span is short: fluorescent material lacks emitting red light composition, is difficult to prepare the white light LEDs of high color rendering index (CRI); Fluorescent material patented technology by abroad monopolization etc.Therefore, research can meet the required highly efficient fluorescent material of large power white light LED part of future generation, promotes the performance of fluorescent material, has extremely important actual application prospect and scientific meaning.In recent years, the Japan always taking advantage on fluorescent material has started to seek novel white-light LED fluorescence material and has substituted conventional fluorescent powder, successively successfully prepare novel YAG class glass-ceramic, the fluorescent materials such as Ce:YAG crystalline ceramics, LED device light efficiency also reaches 80lm/Wt, at present still in constantly researching and developing.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of LED codoped single crystal fluorescent material preparation method.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of LED codoped single crystal fluorescent material preparation method, comprises the steps:
Adopt Medium frequency induction crystal pulling method, by Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder pre-burning in air is dry;
By Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder is that 0.69～0.98:1:0.01:0.01:0.3 mixes and is pressed into block according to mass ratio, then carries out constant temperature pre-burning;
Packing block into iridium crucible carries out crystal growth and obtains codoped single crystal fluorescent material (Ce
x, Gd
yy
1-x-y)
3al
5o
12, x=0.01, y=0.3 and (Ce
x, Eu
yy
1-x-y)
3al
5o
12, x=y=0.01.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described by Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder in air in pre-burning drying step, described raw material Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3purity is: Y
2o
3(99.999%), Al
2o
3(99.999%), CeO
2(99.999%), Eu
2o
3(99.99%), Gd
2o
3(99.99%).
Further, described by Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder is in air in pre-burning drying step, and described pre-burning drying temperature is 800～1000 ℃.
Further, described by Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder is that 0.69～0.98:1:0.01:0.01:0.3 mixes and is pressed into block according to mass ratio, then carries out in constant temperature burn in step, and described constant temperature calcined temperature is 1200～1400 ℃, keeps 10～15h.
Further, describedly pack block into iridium crucible and carry out crystal growth and obtain codoped single crystal fluorescent material (Ce
x, Gd
yy
1-x-y)
3al
5o
12, x=0.01, y=0.3 and (Ce
x, Eu
yy
1-x-y)
3al
5o
12, in x=y=0.01 step, the described crystal brilliant rotational speed rate of growing is 12～25r/min, growth velocity 1～2.5mm/h.
The invention has the beneficial effects as follows: preparation method of the present invention is simple, gained codoped single crystal fluorescent material has higher red emission ability, can be used for preparing the white light LEDs of high color rendering index (CRI).
Accompanying drawing explanation
Fig. 1 is a kind of LED codoped of the present invention single crystal fluorescent material preparation method schema.
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 LED codoped single crystal fluorescent material preparation method, comprises the steps:
Adopt Medium frequency induction crystal pulling method, by Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder pre-burning in air is dry;
By Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder is that 0.69～0.98:1:0.01:0.01:0.3 mixes and is pressed into block according to mass ratio, then carries out constant temperature pre-burning;
Packing block into iridium crucible carries out crystal growth and obtains codoped single crystal fluorescent material (Ce
x, Gd
yy
1-x-y)
3al
5o
12, x=0.01, y=0.3 and (Ce
x, Eu
yy
1-x-y)
3al
5o
12, x=y=0.01.
Embodiment 1:
Preparation 10g codoped single crystal fluorescent material (Ce
x, Gd
yy
1-x-y)
3al
5o
12, x=0.01, y=0.3 and (Ce
x, Eu
yy
1-x-y)
3al
5o
12, x=y=0.01: adopt Medium frequency induction crystal pulling method, by Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder in air at 800 ℃ pre-burning dry; By 6.9g Y
2o
3, 10g Al
2o
3, 0.1gCeO
2, 0.1g Eu
2o
3, 3g Gd
2o
3mix and be pressed into block, at 1200 ℃ of constant temperature pre-burning 10h; Packing block into iridium crucible, is 12r/min at brilliant rotational speed rate, and growth velocity is under 1mm/h condition, to carry out crystal growth to obtain codoped single crystal fluorescent material (Ce
x, Gd
yy
1-x-y)
3al
5o
12, x=0.01, y=0.3 and (Ce
x, Eu
yy
1-x-y)
3al
5o
12, x=y=0.01.
Embodiment 2:
Preparation 10g codoped single crystal fluorescent material (Ce
x, Gd
yy
1-x-y)
3al
5o
12, x=0.01, y=0.3 and (Ce
x, Eu
yy
1-x-y)
3al
5o
12, x=y=0.01: adopt Medium frequency induction crystal pulling method, by Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder in air at 900 ℃ pre-burning dry; By 7.5g Y
2o
3, 10g Al
2o
3, 0.1gCeO
2, 0.1g Eu
2o
3, 3g Gd
2o
3mix and be pressed into block, at 1300 ℃ of constant temperature pre-burning 12h; Packing block into iridium crucible, is 18r/min at brilliant rotational speed rate, and growth velocity is under 1.5mm/h condition, to carry out crystal growth to obtain codoped single crystal fluorescent material (Ce
x, Gd
yy
1-x-y)
3al
5o
12, x=0.01, y=0.3 and (Ce
x, Eu
yy
1-x-y)
3al
5o
12, x=y=0.01.
Embodiment 3:
Preparation 10g codoped single crystal fluorescent material (Ce
x, Gd
yy
1-x-y)
3al
5o
12, x=0.01, y=0.3 and (Ce
x, Eu
yy
1-x-y)
3al
5o
12, x=y=0.01: adopt Medium frequency induction crystal pulling method, by Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder in air at 1000 ℃ pre-burning dry; By 9.8g Y
2o
3, 10g Al
2o
3, 0.1gCeO
2, 0.1g Eu
2o
3, 3g Gd
2o
3mix and be pressed into block, at 1400 ℃ of constant temperature pre-burning 15h; Packing block into iridium crucible, is 25r/min at brilliant rotational speed rate, and growth velocity is under 2.5mm/h condition, to carry out crystal growth to obtain codoped single crystal fluorescent material (Ce
x, Gd
yy
1-x-y)
3al
5o
12, x=0.01, y=0.3 and (Ce
x, Eu
yy
1-x-y)
3al
5o
12, x=y=0.01.
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 (6)
1. a LED codoped single crystal fluorescent material preparation method, is characterized in that, comprises the steps:
Adopt Medium frequency induction crystal pulling method, by Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder pre-burning in air is dry;
By Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder is that 0.69～0.98:1:0.01:0.01:0.3 mixes and is pressed into block according to mass ratio, then carries out constant temperature pre-burning;
Packing block into iridium crucible carries out crystal growth and obtains codoped single crystal fluorescent material (Ce
x, Gd
yy
1-x-y)
3al
5o
12, x=0.01, y=0.3 and (Ce
x, Eu
yy
1-x-y)
3al
5o
12, x=y=0.01.
2. a kind of LED codoped single crystal fluorescent material preparation method according to claim 1, is characterized in that, described by Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder in air in pre-burning drying step, described raw material Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3purity is: Y
2o
3(99.999%), Al
2o
3(99.999%), CeO
2(99.999%), Eu
2o
3(99.99%), Gd
2o
3(99.99%).
3. a kind of LED codoped single crystal fluorescent material preparation method according to claim 1, is characterized in that, described by Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder is in air in pre-burning drying step, and described pre-burning drying temperature is 800～1000 ℃.
4. a kind of LED codoped single crystal fluorescent material preparation method according to claim 1, is characterized in that, described by Y
2o
3, Al
2o
3, CeO
2, Eu
2o
3, Gd
2o
3powder is that 0.69～0.98:1:0.01:0.01:0.3 mixes and is pressed into block according to mass ratio, then carries out in constant temperature burn in step, and described constant temperature calcined temperature is 1200～1400 ℃, keeps 10～15h.
5. according to the arbitrary described a kind of LED codoped single crystal fluorescent material preparation method of claim 1 to 4, it is characterized in that, describedly pack block into iridium crucible and carry out crystal growth and obtain codoped single crystal fluorescent material (Ce
x, Gd
yy
1-x-y)
3al
5o
12, x=0.01, y=0.3 and (Ce
x, Eu
yy
1-x-y)
3al
5o
12, in x=y=0.01 step, the described crystal brilliant rotational speed rate of growing is 12～25r/min, growth velocity 1～2.5mm/h.
6. according to the prepared LED codoped of any LED codoped single crystal fluorescent material preparation method of claim 1 to 5 single crystal fluorescent material.
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| CN201310547481.3A CN103571488A (en) | 2013-11-07 | 2013-11-07 | Preparation method of co-doped single crystal fluorescent material of light-emitting diode (LED) |
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|---|---|---|---|
| CN201310547481.3A CN103571488A (en) | 2013-11-07 | 2013-11-07 | Preparation method of co-doped single crystal fluorescent material of light-emitting diode (LED) |
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| CN103571488A true CN103571488A (en) | 2014-02-12 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108360062A (en) * | 2018-02-02 | 2018-08-03 | 北京中材人工晶体研究院有限公司 | A kind of method that multistep is synthetically prepared rear-earth-doped gadolinium gallium aluminium crystal raw material repeatedly |
| US11926922B2 (en) | 2020-04-14 | 2024-03-12 | Meishan Boya Advanced Materials Co., Ltd. | Methods for crystal growth by replacing a sublimated target source material with a candidate source material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1482208A (en) * | 2002-09-13 | 2004-03-17 | 北京有色金属研究总院 | Blue light-excitated white phosphor powder for LED and production method thereof |
| JP4779384B2 (en) * | 2005-02-28 | 2011-09-28 | 三菱化学株式会社 | Ce-activated rare earth aluminate-based phosphor and light emitting device using the same |
-
2013
- 2013-11-07 CN CN201310547481.3A patent/CN103571488A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1482208A (en) * | 2002-09-13 | 2004-03-17 | 北京有色金属研究总院 | Blue light-excitated white phosphor powder for LED and production method thereof |
| JP4779384B2 (en) * | 2005-02-28 | 2011-09-28 | 三菱化学株式会社 | Ce-activated rare earth aluminate-based phosphor and light emitting device using the same |
Non-Patent Citations (1)
| Title |
|---|
| 华伟等: "白光LED用新型Eu或Gd共掺杂的Ce:YAG单晶荧光材料的光谱性能研究", 《稀有金属材料与工程》, 31 August 2012 (2012-08-31) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108360062A (en) * | 2018-02-02 | 2018-08-03 | 北京中材人工晶体研究院有限公司 | A kind of method that multistep is synthetically prepared rear-earth-doped gadolinium gallium aluminium crystal raw material repeatedly |
| CN108360062B (en) * | 2018-02-02 | 2021-11-12 | 中材人工晶体研究院有限公司 | Method for preparing rare earth doped gadolinium gallium aluminum single crystal raw material by multi-step repeated synthesis |
| US11926922B2 (en) | 2020-04-14 | 2024-03-12 | Meishan Boya Advanced Materials Co., Ltd. | Methods for crystal growth by replacing a sublimated target source material with a candidate source material |
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Application publication date: 20140212 |