CN101747893A - Aluminate red fluorescent powder and preparation method thereof - Google Patents
Aluminate red fluorescent powder and preparation method thereof Download PDFInfo
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- CN101747893A CN101747893A CN200910254515A CN200910254515A CN101747893A CN 101747893 A CN101747893 A CN 101747893A CN 200910254515 A CN200910254515 A CN 200910254515A CN 200910254515 A CN200910254515 A CN 200910254515A CN 101747893 A CN101747893 A CN 101747893A
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Abstract
The invention discloses an aluminate red fluorescent powder and a preparation method thereof, wherein, the aluminate red fluorescent powder has the chemical components of SrAl(12-2x)MnxMgxO19, and 0.06<=x<=0.6. The aluminate red fluorescent powder is a new photon conversion material coated on an ultraviolet or blue light semiconductor chip, the excitation wavelength of the powder is 460nm, the emission peak wavelength is 665nm, and the excitation and emission properties are suitable for the requirement of packaging high-color gamut white light LEDs.
Description
Technical field
The invention belongs to LED fluorescent material technical field, relate to aluminate red fluorescent powder and preparation method thereof.
Background technology
Along with the reduction gradually with cost of improving constantly of LED (photodiode) efficiency lf illumination, LED will become illumination and show main flow with light source by feat of work-ing life of overlength.Realize that LED enters general lighting and demonstration field, then must obtain white light LEDs efficiently.
Realize the 3 kinds of approach that mainly contain of White-light LED illumination at present.First kind of approach is to be combined to form white light by red, green and blue look led chip.But realize relatively difficulty of white light by this method, will consider the drive characteristic of three different colours chips because will realize the white light of stability and high efficiency, very complicated on the circuit layout.Second kind of approach is that the utilization quantum effect realizes Single chip white light, and the same a kind of semiconductor fabrication chip that promptly uses the different-grain diameter size is to realize white light, and the white light LEDs that this method realizes has higher efficient, but cost is higher, and technical immature.The third approach is to use the chip of sending out UV-light or blue light to add that fluorescent material realizes white light, this method be cost minimum, simple, also be the most sophisticated method simultaneously.
Summary of the invention
The problem that the present invention solves is to provide a kind of aluminate red fluorescent powder and preparation method thereof, and this aluminate red fluorescent powder is to be coated in ultraviolet or the light-converting material above the blue-light semiconductor chip, has better thermostability and chemical stability.
The present invention is achieved through the following technical solutions:
A kind of aluminate red fluorescent powder, its chemical constitution are SrAl
12-2xMn
xMg
xO
19, wherein, 0.006≤x≤0.6.
A kind of preparation method of aluminate red fluorescent powder may further comprise the steps:
1) is SrCO in molar ratio
3: Al
2O
3: MnO
2: MgO: H
3BO
3=1: (6～x): x: x: (0.36～0.06x) ratio obtains the fluorescent material presoma with five kinds of compound after evenly, fully grinding, wherein, 0.006≤x≤0.6;
2) with fluorescent material presoma sintering in oxidizing atmosphere, the temperature rise rate during sintering is 3～5 ℃/min, keeps 2～5h when the agglomerating temperature reaches 150～200 ℃; Temperature rise rate with 3～5 ℃/min continues to heat up then, keeps 4～8h when the agglomerating temperature reaches 1350～1450 ℃; Reduce to room temperature with the cooling rate of 3～5 ℃/min at last;
3) the sintering products therefrom is adopted ball mill or beater pulverize 3～12h, obtain aluminate red fluorescent powder, the revolution of ball mill or beater is 100～300r/min.
Described SrCO
3Purity be 99.5%～99.9%, Al
2O
3Purity be 99.99%～99.999%, MnO
2Purity be 99.9%～99.99%, the purity of MgO is 99.9%～99.99%, H
3BO
3Purity be 99%～99.5%.
Described oxidizing atmosphere is air or oxygen atmosphere.
The means of abrasion of described ball mill or beater is made by stupalith, is perhaps made by the agate material.
Compared with prior art, the present invention has following beneficial technical effects:
Aluminate red fluorescent powder provided by the invention is a kind of ultraviolet or new light-converting material above the blue-light semiconductor chip of being coated in.
Because as the backlight white light LEDs, must have high colour gamut and high luminous efficiency, especially high colour gamut is even more important; And high colour gamut requires fluorescent material can launch long wavelength's ruddiness, has short wavelength's blue light.Aluminate red fluorescent powder provided by the invention, its excitation wavelength is 460nm, emission wavelength is 665nm; Exciting with emission characteristic like this is fit to the requirement that high colour gamut white light LEDs encapsulates.
Mainly use SrS:Eu with present white light LEDs
2+Compare as red fluorescence powder, the red fluorescence powder among the present invention has better thermostability and chemical stability.
Description of drawings
Fig. 1 is the red fluorescence powder SrAl that the present invention prepares
12-2xMn
xMg
xO
19XRD figure spectrum; X-coordinate is angle of diffraction 2 θ among the figure, and ordinate zou is relative diffracted intensity;
Fig. 2 is the red fluorescence powder SrAl that the present invention prepares
12-2xMn
xMg
xO
19Excite and emmission spectrum figure, X-coordinate is the wavelength that excites or launch among the figure, ordinate zou is the relative intensity that excites or launch;
Fig. 3 is with SrS:Eu
2+As red fluorescence powder in contrast, the red fluorescence powder SrAl of the present invention's preparation
12-2xMn
xMg
xO
19Emissive porwer with variation of temperature figure.
Embodiment
Below in conjunction with specific embodiment and accompanying drawing the present invention is described in further details, the explanation of the invention is not limited.
In the middle of the related raw material of following embodiment, SrCO
3Purity be 99.5%～99.9%, Al
2O
3Purity be 99.99%～99.999%, MnO
2Purity be 99.9%～99.99%, the purity of MgO is 99.9%～99.99%, H
3BO
3Purity be 99%～99.5%.
The related ball mill or the means of abrasion of beater are made by stupalith, are perhaps made by the agate material.
Embodiment 1
1) with 1mol SrCO
3, 5.994mol Al
2O
3, 0.006mol MnO
2, 0.006mol MgO and 0.35964mol H
3BO
3Mix, then mixture is put into and rolled a bottle machine and grind 5h, obtain the fluorescent material presoma;
2) the fluorescent material presoma is put into High Temperature Furnaces Heating Apparatus in the air atmosphere sintering, sintering temperature heats up with the speed of 3 ℃/min, keeps 2h when the agglomerating temperature reaches 200 ℃; Continuation heats up with the speed of 3 ℃/min, keeps 4h then when the agglomerating temperature reaches 1350 ℃; Reduce to room temperature with the cooling rate of 3 ℃/min at last;
3) sinter with gained carries out ball milling with ball mill, and the time of ball milling is 3h, and revolution is 180r/min; After finishing, ball milling obtains red fluorescence powder SrAl
11.988Mn
0.006Mg
0.006O
19
Embodiment 2
1) with 1mol SrCO
3, 5.4mol Al
2O
3, 0.6mol MnO
2, 0.6mol MgO and 0.324molH
3BO
3Mix, then mixture is put into and rolled a bottle machine and grind 15h, obtain the fluorescent material presoma;
2) the fluorescent material presoma is put into High Temperature Furnaces Heating Apparatus and be carried out at purity oxygen atmosphere sintering, sintering temperature heats up with the speed of 3 ℃/min, keeps 2h when the agglomerating temperature reaches 200 ℃; Continuation heats up with the speed of 3 ℃/min, keeps 4h then when the agglomerating temperature reaches 1350 ℃; Reduce to room temperature with the cooling rate of 5 ℃/min at last;
3) sinter with gained carries out ball milling with ball mill, and the time of ball milling is 10h, and revolution is 180r/min; After finishing, ball milling obtains red fluorescence powder SrAl
10.8Mn
0.6Mg
0.6O
19
Embodiment 3
With 1mol SrCO
3, 5.7mol Al
2O
3, 0.3mol MnO
2, 0.3mol MgO and 0.342molH
3BO
3Mix, then mixture is put into grinding in ball grinder 8h, obtain the fluorescent material presoma;
2) the fluorescent material presoma is put into High Temperature Furnaces Heating Apparatus and be carried out at the air atmosphere sintering, sintering temperature heats up with the speed of 4 ℃/min, keeps 2h when the agglomerating temperature reaches 150 ℃; Continuation heats up with the speed of 4 ℃/min, keeps 4h then when the agglomerating temperature reaches 1450 ℃; Reduce to room temperature with the cooling rate of 4 ℃/min at last;
3) sinter of gained is pulverized with rolling a bottle machine, the time of pulverizing is 10h, and revolution is 200r/min; After finishing, ball milling obtains red fluorescence powder SrAl
11.4Mn
0.3Mg
0.3O
19
Embodiment 4
1) with 1mol SrCO
3, 5.95mol Al
2O
3, 0.05mol MnO
2, 0.05mol MgO and 0.357molH
3BO
3Mix, mixture is put into agate mortar grind 5h, obtain the fluorescent material presoma;
2) the fluorescent material presoma is put into High Temperature Furnaces Heating Apparatus and be carried out at the air atmosphere sintering, sintering temperature heats up with the speed of 5 ℃/min, keeps 4h when the agglomerating temperature reaches 180 ℃; Continuation heats up with the speed of 5 ℃/min, keeps 6h then when the agglomerating temperature reaches 1400 ℃; Reduce to room temperature with the cooling rate of 5 ℃/min at last;
3) sinter with gained carries out ball milling with ball mill, and the time of ball milling is 10h, and revolution is 260r/min; After finishing, ball milling obtains red fluorescence powder SrAl
11.9Mn
0.05Mg
0.05O
19
Embodiment 5
1) with 1mol SrCO
3, 5.4mol Al
2O
3, 0.6mol MnO
2, 0.6mol MgO and 0.324molH
3BO
3Mix, then mixture is put into grinding in ball grinder 15h, obtain the fluorescent material presoma;
2) the fluorescent material presoma is put into High Temperature Furnaces Heating Apparatus and be carried out at the air atmosphere sintering, sintering temperature heats up with the speed of 5 ℃/min, keeps 5h when the agglomerating temperature reaches 160 ℃; Continuation heats up with the speed of 5 ℃/min, keeps 8h then when the agglomerating temperature reaches 1380 ℃; Reduce to room temperature with the cooling rate of 5 ℃/min at last;
3) sinter of gained is pulverized with rolling a bottle machine, the pulverizing of ball milling is 12h, and revolution is 100r/min; After finishing, ball milling obtains red fluorescence powder SrAl
10.8Mn
0.6Mg
0.6O
19
Embodiment 6
1) with 1mol SrCO
3, 5.9mol Al
2O
3, 0.01mol MnO
2, 0.01mol MgO and 0.354molH
3BO
3Mix, then mixture is put into grinding in ball grinder 15h, obtain the fluorescent material presoma;
2) the fluorescent material presoma is put into High Temperature Furnaces Heating Apparatus and be carried out at the air atmosphere sintering, sintering temperature heats up with the speed of 5 ℃/min, keeps 5h when the agglomerating temperature reaches 150 ℃; Continuation heats up with the speed of 5 ℃/min, keeps 5h then when the agglomerating temperature reaches 1420 ℃; Reduce to room temperature with the cooling rate of 5 ℃/min at last;
3) sinter of gained is pulverized with rolling a bottle machine, the pulverizing of ball milling is 12h, and revolution is 100r/min; After finishing, ball milling obtains red fluorescence powder SrAl
11.8Mn
0.01Mg
0.01O
19
The present invention specifically with embodiment 1 gained red fluorescence powder, the thing of having tested sample mutually and luminescent spectrum, concrete outcome as depicted in figs. 1 and 2:
Wherein Fig. 1 is the X-ray diffractogram of sample, and diffractogram is corresponding consistent with standard card (#80-1195), and the thing of interpret sample is pure mutually;
Fig. 2 excites and emmission spectrum figure for sample, and interpret sample has absorption and (is absorbed in 250～500nm), at red light district emission (625～700nm) arranged in the visible region;
Among Fig. 3 curve a for the emissive porwer of sample among the present invention with variation of temperature figure, curve b is SrS:Eu
2+The sample emissive porwer is with variation of temperature figure, and the emission of sample has better thermostability and chemical stability among correlation curve a, b explanation the present invention.
Claims (5)
1. aluminate red fluorescent powder, it is characterized in that: its chemical constitution is SrAl
12-2xMn
xMg
xO
19, wherein, 0.006≤x≤0.6.
2. the preparation method of an aluminate red fluorescent powder is characterized in that, may further comprise the steps:
1) is SrCO in molar ratio
3: Al
2O
3: MnO
2: MgO: H
3BO
3=1: (6～x): x: x: (0.36～0.06x) ratio obtains the fluorescent material presoma with five kinds of compound after fully grinding, wherein, 0.006≤x≤0.6;
2) with fluorescent material presoma sintering in oxidizing atmosphere, the temperature rise rate during sintering is 3～5 ℃/min, keeps 2～5h when the agglomerating temperature reaches 150～200 ℃; Temperature rise rate with 3～5 ℃/min continues to heat up then, keeps 4～8h when the agglomerating temperature reaches 1350～1450 ℃; Reduce to room temperature with the cooling rate of 3～5 ℃/min at last;
3) the sintering products therefrom is adopted ball mill or beater pulverize 3～12h, obtain aluminate red fluorescent powder, the revolution of ball mill or beater is 100～300r/min.
3. the preparation method of aluminate red fluorescent powder as claimed in claim 2 is characterized in that: described SrCO
3Purity be 99.5%～99.9%, Al
2O
3Purity be 99.99%～99.999%, MnO
2Purity be 99.9%～99.99%, the purity of MgO is 99.9%～99.99%, H
3BO
3Purity be 99%～99.5%.
4. the preparation method of aluminate red fluorescent powder as claimed in claim 2, it is characterized in that: described oxidizing atmosphere is air or oxygen atmosphere.
5. the preparation method of aluminate red fluorescent powder as claimed in claim 2, it is characterized in that: the means of abrasion of described ball mill or beater is made by stupalith, is perhaps made by the agate material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102545153A CN101747893B (en) | 2009-12-25 | 2009-12-25 | Aluminate red fluorescent powder and preparation method thereof |
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|---|---|---|---|
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| Publication Number | Publication Date |
|---|---|
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| CN101747893B CN101747893B (en) | 2013-01-16 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321472A (en) * | 2011-09-08 | 2012-01-18 | 华南理工大学 | Tetravalent manganese ion doped strontium magnesium aluminate red phosphor, and preparation method thereof |
| CN103146381A (en) * | 2013-01-29 | 2013-06-12 | 广州有色金属研究院 | Aluminate red phosphor activated by manganese ion and preparation method thereof |
| WO2015018638A1 (en) * | 2013-08-09 | 2015-02-12 | Osram Gmbh | Red phosphor, white light source, light-emitting device, and method of forming the red phosphor |
| CN106536677A (en) * | 2014-06-17 | 2017-03-22 | 欧司朗光电半导体有限公司 | Phosphor, light-emitting device containing a phosphor and method for producing a phosphor |
| CN106833636A (en) * | 2017-02-28 | 2017-06-13 | 江苏师范大学 | Can be by near ultraviolet and blue light activated red fluorescence powder, preparation method and application |
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| JP2022078773A (en) * | 2020-11-13 | 2022-05-25 | 住友化学株式会社 | Phosphor |
| JP2022078771A (en) * | 2020-11-13 | 2022-05-25 | 住友化学株式会社 | Phosphor |
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Family Cites Families (2)
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|---|---|---|---|---|
| CN1664058A (en) * | 2005-02-21 | 2005-09-07 | 东南大学 | Process for preparing aluminate green fluorescent powder for plasma display device |
| CN101402857B (en) * | 2008-10-29 | 2012-03-28 | 华南理工大学 | Red luminous material for LED and producing process thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321472A (en) * | 2011-09-08 | 2012-01-18 | 华南理工大学 | Tetravalent manganese ion doped strontium magnesium aluminate red phosphor, and preparation method thereof |
| CN102321472B (en) * | 2011-09-08 | 2013-11-13 | 华南理工大学 | Tetravalent manganese ion doped strontium magnesium aluminate red phosphor, and preparation method thereof |
| CN103146381A (en) * | 2013-01-29 | 2013-06-12 | 广州有色金属研究院 | Aluminate red phosphor activated by manganese ion and preparation method thereof |
| WO2015018638A1 (en) * | 2013-08-09 | 2015-02-12 | Osram Gmbh | Red phosphor, white light source, light-emitting device, and method of forming the red phosphor |
| CN106536677A (en) * | 2014-06-17 | 2017-03-22 | 欧司朗光电半导体有限公司 | Phosphor, light-emitting device containing a phosphor and method for producing a phosphor |
| CN106536677B (en) * | 2014-06-17 | 2019-04-05 | 欧司朗光电半导体有限公司 | Phosphor, the light emitting device comprising phosphor and the method for manufacturing phosphor |
| CN106833636A (en) * | 2017-02-28 | 2017-06-13 | 江苏师范大学 | Can be by near ultraviolet and blue light activated red fluorescence powder, preparation method and application |
| CN106833636B (en) * | 2017-02-28 | 2019-03-15 | 江苏师范大学 | It can be by near ultraviolet and blue light activated red fluorescence powder, preparation method and application |
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