CN102965108A - Aluminate doped fluorescent powder and preparation method thereof - Google Patents
Aluminate doped fluorescent powder and preparation method thereof Download PDFInfo
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- CN102965108A CN102965108A CN2012104290979A CN201210429097A CN102965108A CN 102965108 A CN102965108 A CN 102965108A CN 2012104290979 A CN2012104290979 A CN 2012104290979A CN 201210429097 A CN201210429097 A CN 201210429097A CN 102965108 A CN102965108 A CN 102965108A
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- 239000000843 powder Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 150000004645 aluminates Chemical class 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 22
- 150000001875 compounds Chemical class 0.000 claims abstract description 20
- 239000000126 substance Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims description 29
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 3
- 238000009837 dry grinding Methods 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 238000009766 low-temperature sintering Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000001238 wet grinding Methods 0.000 claims description 2
- 230000005284 excitation Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000007858 starting material Substances 0.000 description 10
- 238000001035 drying Methods 0.000 description 5
- 230000000630 rising effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical group [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
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Abstract
The invention relates to an aluminate doped fluorescent powder and a preparation method thereof. The aluminate doped fluorescent powder is characterized by having a chemical formula of Y3-xAl5-ySiyO12-y / 2:xCe, wherein x and y satisfy the relations of 0 <x<=0.3, and y<=0 <0.6. The invention provides the aluminate doped fluorescent powder material and the preparation method thereof; and cheap and stable compounds are used as raw materials, and the synthesis process is simple and suitable for industrial mass production. The obtained fluorescent powder material is suitable for excitation by excitation sources such as ultraviolet, near ultraviolet and blue light, emits yellow light with wavelength of 540-560nm, and is a fluorescent powder with high performance for LED.
Description
Technical field
The present invention relates to a kind of doping aluminate fluorescent powder and preparation method thereof.
Background technology
The LED photodiode not only can with electric energy directly high efficiency be converted into luminous energy but also have reach tens thousand of hours work-ing life, possessed simultaneously difficult fragmentation, energy-conservation advantage.Appearance along with new generation of semiconductor material GaN and processing technology thereof, the LED luminous efficiency promotes rapidly, external advanced LED production company is the LED product of volume production light efficiency more than 160lm/w, Technology Potential and development trend with regard to photodiode see that its light efficiency is expected to reach 400lm/w and becomes the brightest in the world light source, and industry thinks that semiconductor lighting will create the 4th revolution of lighting field.
Current LED adopts the mode of blue chip coupling yellow fluorescent powder to realize white light, and the yttrium aluminum garnet structure fluorescent material that Ce activates has high luminous efficiency and chemical stability is good, and excitation wavelength range is wide, is a kind of desirable LED yellow fluorescent powder.
Summary of the invention
One of purpose of the present invention provides a kind of LED doping aluminate fluorescent powder of excellent property;
Two of purpose of the present invention provides a kind of preparation method of above-mentioned fluorescent material, and the method synthesis technique is simple, is suitable for industrialized mass production.
A kind of doping aluminate fluorescent powder, its special feature is: the chemical general formula of this fluorescent material is Y
3-xAl
5-ySi
yO
12-y/2: xCe, wherein x, y satisfy 0＜x≤0.3,0＜y≤0.6.
A kind of preparation method of the aluminate fluorescent powder that mixes, its special feature is, comprises the steps:
(1) according to the proportioning of claim 1, will contain the Y compound, contain the A1 compound, contain the Ce compound, and SiO
2Fully mix through ball milling as raw material;
(2) the gained mixture is carried out low-temperature sintering first in protective atmosphere, then improve sintering temperature and carry out the synthetic rear cooling of high temperature sintering;
(3) sintered product that obtains is washed, broken, classification gets final product.
Wherein contain oxide compound or nitrate that the Y compound is Y, contain oxyhydroxide or oxide compound that the Al compound is Al, contain oxide compound or nitrate that the Ce compound is Ce.
Wherein ball milling adopts wet-milling or dry grinding.
Wherein low sintering temperature is 900 ℃-1000 ℃, and sintering time is 2-4 hour; Shielding gas was selected N during high temperature sintering was synthetic
2/ H
2=75:25-95:5 (v/v), sintering temperature is 1300 ℃-1800 ℃, sintering time is 2-5 hour.
Wherein dilute hydrochloric acid is adopted in washing.
The invention provides a kind of adulterated al hydrochlorate phosphor material powder and preparation method, adopting cheapness, stable compound is raw material, and synthesis technique is simple, is suitable for industrialized mass production.The gained phosphor material powder is fit to ultraviolet, near ultraviolet or blue light equal excitation source excitation, and emission wavelength is Yellow luminous 540-560nm's, is a kind of LED fluorescent material of excellent property.
Description of drawings
Fig. 1 is the Y of preparation in the embodiment of the invention 1
2.7Al
4.8Si
0.2O
11.9: the XRD of 0.3Ce fluorescent material (X-ray diffraction) figure, wherein X-coordinate is the X ray input angle, and ordinate zou is the relative intensity of diffraction peak, and a small amount of mixing of Si element do not have influence on its yttrium aluminum garnet constructional feature;
Fig. 2 is the Y of preparation in the embodiment of the invention 1
2.7Al
4.8Si
0.2O
11.9: the utilizing emitted light spectrogram of 0.3Ce fluorescent material.
Embodiment
Embodiment 1:
Y
2.7Al
4.8Si
0.2O
11.9: the preparation of 0.3Ce fluorescent material:
With Y
2O
3, Al (OH)
3, SiO
2, CeO
2Be starting material, the ratio of the amount of substance of above-mentioned substance is Y:Al:Si:Ce=2.7:4.8:0.2:0.3, above-mentioned starting material is carried out abundant ball milling mix rear taking-up, puts into crucible, at N
2/ H
21000 ℃ of sintering are after 2 hours in=75:25 (v/v) atmosphere, rising sintering temperature to 1600 ℃ continuation sintering 3 hours, naturally cooling takes out in aforementioned atmosphere, will wash with hydrochloric acid (37wt%) after the fragmentation of gained sample, the classification, and then 120 ℃ of oven dry namely got Y after the drying in 2 hours
2.7Al
4.8Si
0.2O
11.9: 0.3Ce fluorescent material.
Embodiment 2:
Y
2.9Al
4.6Si
0.4O
11.8: the preparation of 0.1Ce fluorescent material:
With Y
2O
3, Al
2O
3, SiO
2, CeO
2Be starting material, the ratio of the amount of substance of above-mentioned substance is Y:Al:Si:Ce=2.9:4.6:0.4:0.1, and above-mentioned starting material are carried out taking out after abundant ball milling mixes, and puts into crucible, at N
2/ H
2900 ℃ of sintering are after 3 hours in=90:10 (v/v) atmosphere, rising sintering temperature to 1300 ℃ continuation sintering 4 hours, naturally cooling takes out in the reducing atmosphere, will wash with hydrochloric acid (37wt%) after the broken classification of gained sample, and 120 ℃ of oven dry namely got Y after the drying in 2 hours
2.9Al
4.6Si
0.4O
11.8: 0.1Ce fluorescent material.
Embodiment 3:
Y
2.8Al
4.8Si
0.2O
11.9: the preparation of 0.2Ce fluorescent material:
With Y (NO
3)
3, Al
2O
3, SiO
2, Ce (NO
3)
4Be starting material, the ratio of the amount of substance of above-mentioned substance is Y:Al:Si:Ce=2.8:4.8:0.2:0.2, and above-mentioned starting material are carried out taking out after abundant ball milling mixes, and puts into crucible, at N
2/ H
2950 ℃ of sintering are after 3 hours in=95:5 (v/v) atmosphere, rising sintering temperature to 1500 ℃ continuation sintering 5 hours, naturally cooling takes out in the reducing atmosphere, will wash with hydrochloric acid (37wt%) after the broken classification of gained sample, and 120 ℃ of oven dry namely got Y after the drying in 2 hours
2.8Al
4.8Si
0.2O
11.9: 0.2Ce fluorescent material.
Embodiment 4:
Y
2.85Al
4.8Si
0.2O
11.9: the preparation of 0.15Ce fluorescent material:
With Y
2O
3, Al
2O
3, SiO
2, CeO
2Be starting material, the ratio of the amount of substance of above-mentioned substance is Y:Al:Si:Ce=2.85:4.8:0.2:0.15, and above-mentioned starting material are carried out taking out after abundant ball milling mixes, and puts into crucible, at N
2/ H
2900 ℃ of sintering are after 4 hours in=90:10 (v/v) atmosphere, rising sintering temperature to 1400 ℃ continuation sintering 5 hours, naturally cooling takes out in the reducing atmosphere, will wash with hydrochloric acid (37wt%) after the broken classification of gained sample, and 120 ℃ of oven dry namely got Y after the drying in 2 hours
2.85Al
4.6Si
0.4O
11.8: 0.15Ce fluorescent material.
Embodiment 5:
Y
2.8Al
4.9Si
0.1O
11.95: the preparation of 0.2Ce fluorescent material:
With Y
2O
3, Al (OH)
3, SiO
2, CeO
2Be starting material, the ratio of the amount of substance of above-mentioned substance is Y:Al:Si:Ce=2.8:4.9:0.1:0.2, and above-mentioned starting material are carried out taking out after abundant ball milling mixes, and puts into crucible, at N
2/ H
21000 ℃ of sintering are after 3 hours in=95:5 (v/v) atmosphere, rising sintering temperature to 1800 ℃ continuation sintering 2 hours, naturally cooling takes out in the reducing atmosphere, will wash with hydrochloric acid (37wt%) after the broken classification of gained sample, and 120 ℃ of oven dry namely got Y after the drying in 2 hours
2.85Al
4.6Si
0.4O
11.8: 0.15Ce fluorescent material.
Claims (6)
1. doping aluminate fluorescent powder, it is characterized in that: the chemical general formula of this fluorescent material is Y
3-xAl
5-ySi
yO
12-y/2: xCe, wherein x, y satisfy 0＜x≤0.3,0＜y≤0.6.
2. the preparation method of the aluminate fluorescent powder that mixes is characterized in that, comprises the steps:
(1) according to the proportioning of claim 1, will contain the Y compound, contain the Al compound, contain the Ce compound, and SiO
2Fully mix through ball milling as raw material;
(2) the gained mixture is carried out low-temperature sintering first in protective atmosphere, then improve sintering temperature and carry out the synthetic rear cooling of high temperature sintering;
(3) sintered product that obtains is washed, broken, classification gets final product.
3. the preparation method of a kind of aluminate fluorescent powder that mixes as claimed in claim 2, it is characterized in that: wherein contain oxide compound or nitrate that the Y compound is Y, contain oxyhydroxide or oxide compound that the Al compound is Al, contain oxide compound or nitrate that the Ce compound is Ce.
4. the preparation method of a kind of aluminate fluorescent powder that mixes as claimed in claim 2 is characterized in that: wherein ball milling employing wet-milling or dry grinding.
5. the preparation method of a kind of aluminate fluorescent powder that mixes as claimed in claim 2, it is characterized in that: wherein low sintering temperature is 900 ℃-1000 ℃, and sintering time is 2-4 hour; Shielding gas was selected N during high temperature sintering was synthetic
2/ H
2=75:25-95:5 (v/v), sintering temperature is 1300 ℃-1800 ℃, sintering time is 2-5 hour.
6. the preparation method of a kind of aluminate fluorescent powder that mixes as claimed in claim 2 is characterized in that: wherein wash and adopt dilute hydrochloric acid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012104290979A CN102965108A (en) | 2012-10-31 | 2012-10-31 | Aluminate doped fluorescent powder and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012104290979A CN102965108A (en) | 2012-10-31 | 2012-10-31 | Aluminate doped fluorescent powder and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN102965108A true CN102965108A (en) | 2013-03-13 |
Family
ID=47795545
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103160280A (en) * | 2011-12-08 | 2013-06-19 | 陈引幹 | Yttrium aluminum garnet fluorescent material, preparation method thereof and light emitting diode device comprising yttrium aluminum garnet fluorescent material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1455960A (en) * | 2001-01-24 | 2003-11-12 | 日亚化学工业株式会社 | Light emitting diode, optical semiconductor element and epoxy resin composition suitable for optical semiconductor element and production methods therefor |
| US7252787B2 (en) * | 2003-10-29 | 2007-08-07 | General Electric Company | Garnet phosphor materials having enhanced spectral characteristics |
| CN101134896A (en) * | 2007-10-16 | 2008-03-05 | 厦门大学 | Method for preparing rare earth-doped yttrium aluminum garnet phosphor by heterogeneous precipitation of oxalic acid |
| CN101137738A (en) * | 2005-03-08 | 2008-03-05 | 皇家飞利浦电子股份有限公司 | Illumination system comprising a radiation source and a luminescent material |
| JP2009079094A (en) * | 2007-09-25 | 2009-04-16 | Toshiba Corp | Phosphor and LED lamp using the same |
-
2012
- 2012-10-31 CN CN2012104290979A patent/CN102965108A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1455960A (en) * | 2001-01-24 | 2003-11-12 | 日亚化学工业株式会社 | Light emitting diode, optical semiconductor element and epoxy resin composition suitable for optical semiconductor element and production methods therefor |
| US7252787B2 (en) * | 2003-10-29 | 2007-08-07 | General Electric Company | Garnet phosphor materials having enhanced spectral characteristics |
| CN101137738A (en) * | 2005-03-08 | 2008-03-05 | 皇家飞利浦电子股份有限公司 | Illumination system comprising a radiation source and a luminescent material |
| JP2009079094A (en) * | 2007-09-25 | 2009-04-16 | Toshiba Corp | Phosphor and LED lamp using the same |
| CN101134896A (en) * | 2007-10-16 | 2008-03-05 | 厦门大学 | Method for preparing rare earth-doped yttrium aluminum garnet phosphor by heterogeneous precipitation of oxalic acid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103160280A (en) * | 2011-12-08 | 2013-06-19 | 陈引幹 | Yttrium aluminum garnet fluorescent material, preparation method thereof and light emitting diode device comprising yttrium aluminum garnet fluorescent material |
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Application publication date: 20130313 |