CN101948692A - Mixed fluorescent powder matched with blue-light chip and preparation method thereof - Google Patents
Mixed fluorescent powder matched with blue-light chip and preparation method thereof Download PDFInfo
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- CN101948692A CN101948692A CN 201010296849 CN201010296849A CN101948692A CN 101948692 A CN101948692 A CN 101948692A CN 201010296849 CN201010296849 CN 201010296849 CN 201010296849 A CN201010296849 A CN 201010296849A CN 101948692 A CN101948692 A CN 101948692A
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Abstract
The invention discloses mixed fluorescent powder matched with a blue-light chip and a preparation method thereof. The method comprises the following steps of: mixing red fluorescent powder A1-xByOzN2/3+4/3y-2/3z:xRe and yellow fluorescent powder Y3-a-bAl5Baa012:Ceb3+ according to a mass ratio of 50-35:100 in ethanol in the mass which is 2 to 10 times that of the yellow fluorescent powder, adding polyvinyl alcohol in the mass which is 5 to 10 times that of the yellow fluorescent powder and polyacrylamide in the mass which is 5 to 10 times that of the yellow fluorescent powder, and fully mixing to form a gelatinous mixture. In the method, two conventional fluorescent powders are mixed in absolute ethyl alcohol, and the polyvinyl alcohol and the polyacrylamide are added to be prepared into a supermolecular template for auxiliary mixing, so that the two fluorescent powders are uniformly dispersed to form a low-color temperature mixed fluorescent powder gel with stable homogeneous phase.
Description
Technical field
The invention belongs to the fluorescent powder for white LED technical field, particularly a kind of mixed fluorescent powder that cooperates the blue chip use and preparation method thereof.
Background technology
Fluorescent material conversion of white light diode (pc-wLED) is because of it has energy-saving and environmental protection, premium properties such as efficient is expected to become lighting source of new generation.The main flow means of current realization white light are blue light (the chips incorporate YAG:Ce yellow fluorescent powders of 440nm～470nm).There is the defective of low color developing and high colour temperature in the white light LEDs that this mode of manufacture goes out because of lacking ruddiness, has limited its Application Areas greatly.For the white light LEDs that obtains high color rendering index (CRI), low colour temperature, low dazzle one of can the employing scheme be exactly that blue chip adds Huang, red fluorescent material.
And because red fluorescence powder belongs to the oxynitride system, the yellow fluorescent powder of shape characteristic, proportion and YAG system has very big difference, simple mixed two kinds of fluorescent material in water or ethanol are in the process of packing accumulating and use, two kinds of fluorescent material are because lack necessary linking agent, be easy to spread out, cause the homogeneity of product that encapsulates very poor, also can't reach and specify the colour gamut requirement.
In addition, because each producer, the fluorescent material of each batch production all has difference on chromaticity coordinates, emission peak, and the technical indicator that provides of manufacturer is not accurately yet, can't satisfy the demand that colour temperature fluorescent material is specified in accurate preparation.So rely on commodity powder model to come modulation ratio merely, the mixed type fluorescent material of preparation target colour temperature, target colour rendering index is inaccurate.This will have a strong impact on the LED consistency of product, cause large-tonnage product not meet colour temperature and colour rendering index requirement.
Summary of the invention
The problem that the present invention solves is a kind of mixed fluorescent powder that cooperates the blue chip use and preparation method thereof is provided, and red fluorescence powder rare earth doped nitric oxide and yellow fluorescent powder yttrium aluminum garnet is mixed with into the low colour temperature mixed fluorescent powder of homodisperse, homogeneous stability.
The present invention is achieved through the following technical solutions:
A kind of mixed fluorescent powder that cooperates blue chip to use is with red fluorescence powder A
1-xB
yO
zN
2/3+4/3y-2/3z: xRe and yellow fluorescent powder Y
3-a-bAl
5Ba
aO
12: Ce
b 3+According to 35～50: 100 mass ratio, mixing in the ethanol of 2～10 times of yellow fluorescent powder quality adds the polyvinyl alcohol of 5～10 times of yellow fluorescent powder quality, 5～10 times polyacrylamide again, fully formed gelatinous mixture behind the mixing;
Wherein, A is one or more among Mg, Ca, Sr, the Ba, and B is that Si or Si mix with Al, and Re is one or both among Eu, the Mn, 0≤x＜1.0,1.0≤y≤3.0,0＜z≤2.0; 0.01≤a≤0.05,0.05≤b≤0.10.
The chromaticity coordinates of described yellow fluorescent powder is: 0.427≤X≤0.437,0.537≤Y≤0.547 is 550≤λ≤560 by the emission wavelength after blue-light excited;
The chromaticity coordinates of described red fluorescence powder is: 0.630≤X≤0.640,0.360≤Y≤0.370 is 615≤λ≤625 by the emission wavelength after blue-light excited.
A kind of preparation method who cooperates the mixed fluorescent powder of blue chip use may further comprise the steps:
With red fluorescence powder A
1-xB
yO
zN
2/3+4/3y-2/3z: xRe and yellow fluorescent powder Y
3-a-bAl
5Ba
aO
12: Ce
b 3+According to 50～35: 100 mass ratio, after in the ethanol of 2～10 times of yellow fluorescent powder quality, mixing, under ultrasonic oscillation, stir, be heated to 100～200 ℃, keep 0.5～1h; Add the polyvinyl alcohol of 5～10 times of yellow fluorescent powder quality, 5～10 times polyacrylamide then, treat that it dissolves fully after, stir, form gelatinous mixture, obtain the mixed fluorescent powder that cooperates blue chip to use;
Wherein, A is one or more among Mg, Ca, Sr, the Ba, and B is that Si or Si mix with Al, and Re is one or both among Eu, the Mn, 0≤x＜1.0,1.0≤y≤3.0,0＜z≤2.0; 0.01≤a≤0.05,0.05≤b≤0.10.
The chromaticity coordinates of described yellow fluorescent powder is: 0.427≤X≤0.437,0.537≤Y≤0.547 is 550≤λ≤560 by the emission wavelength after blue-light excited;
The chromaticity coordinates of described red fluorescence powder is: 0.630≤X≤0.640,0.360≤Y≤0.370 is 615≤λ≤625 by the emission wavelength after blue-light excited.
The relative molecular weight of described polyvinyl alcohol is 250,000～300,000; The relative molecular weight of polyacrylamide is 8,000,000～10,000,000.
Compared with prior art, the present invention has following beneficial technical effects:
The present invention passes through the fluorescent material with two kinds of routines: red fluorescence powder A
1-xB
yO
zN
2/3+4/3y-2/3z: xRe and yellow fluorescent powder Y
3-a-bAl
5Ba
aO
12: Ce
b 3+In dehydrated alcohol behind the mixing, polyvinyl alcohol is poly-by adding, acrylamide makes that the supramolecule masterplate is auxiliary to be mixed, and makes two kinds of fluorescent material homodisperse, forms the low colour temperature mixed fluorescent powder gel of homogeneous stability.
Prepared mixed fluorescent powder, physicochemical property are stable, and the quantum yield height is with LED packaging plastic favorable dispersity, easy to use; Encapsulation back is photochromic evenly, does not have the differ reunion that causes and disperse the unbalanced hot spot inequality that causes of phosphor's density; Be a kind of suitable 440nm～blue-light excited luminescent material of 460nm wavelength, can be widely used in the extraordinary LED illumination and the display device of low colour temperature high color rendering index (CRI), such as the exhibition illumination of artwork jewelry etc., the fields such as graphicprocessing working spaces illumination of specialty.
Further red fluorescence powder, yellow fluorescent powder before mixing are screened, test the chromaticity coordinates and the emission wavelength of two kinds of fluorescent material respectively, screening meets the fluorescent material of specified conditions, can prepare and cooperate the 460nm blue chip to reach colour temperature 3000～3500K, the mixed fluorescent powder of Ra 〉=85, and can guarantee to prepare the precision of powder mix, in particular for middle power-type LED, be significantly increased for the colour rendering index of encapsulation back product; Overcome dependence commodity powder model and come modulation ratio, the inaccurate defective of mixed type fluorescent material of preparation target colour temperature, target colour rendering index.
It is the raw material synthetizing phosphor powder that the present invention adopts common cheap compound, uses the common device mixed fluorescent powder, and simple to operate, process window is wide, is suitable for large-scale industrial production.
Description of drawings
Fig. 1 cooperates one of spectral power distribution of mixed fluorescent powder encapsulation for blue chip;
Fig. 2 cooperate for blue chip the mixed fluorescent powder encapsulation spectral power distribution two.
Embodiment
The present invention passes through the fluorescent material with two kinds of routines: red fluorescence powder A
1-xB
yO
zN
2/3+4/3y-2/3z: xRe and yellow fluorescent powder Y
3-a-bAl
5Ba
aO
12: Ce
b 3+Auxiliary by polymeric stencil, in ethanol, mix the preparation mixed fluorescent powder.The present invention is described in further detail with the spectral power distribution that cooperates blue chip below in conjunction with specific embodiment, and the explanation of the invention is not limited.
As primary fluorescent material, red fluorescence powder is A
1-xB
yO
zN
2/3+4/3y-2/3z: xRe, wherein, A is one or more among Mg, Ca, Sr, the Ba, and B is that Si or Si mix with Al, and Re is one or both among Eu, the Mn, 0≤x＜1.0,1.0≤y≤3.0,0＜z≤2.0; Its preparation is specifically referring to " a kind of LED red fluorescence powder and preparation method thereof and made electric light source ", patent publication No. CN1539914.
Yellow fluorescent powder is Y
3-a-bA
L5Ba
aO
12: Ce
b 3+, wherein, 0.01≤a≤0.05,0.05≤b≤0.10, it prepares specifically referring to " preparation method of yellow luminescent powder for blue light emission diode ", patent publication No. CN1827734.
The relative molecular weight of the concrete polyvinyl alcohol that is adopted is 250,000～300,000; The relative molecular weight of polyacrylamide is 8,000,000～10,000,000.
Embodiment 1
Cooperate the preparation of the mixed fluorescent powder of blue chip use, may further comprise the steps:
With red fluorescence powder A
1-xB
yO
zN
2/3+4/3y-2/3z: xRe and yellow fluorescent powder Y
3-a-bA
L5Ba
aO
12: Ce
b 3+According to 50: 100 mass ratio, after in the ethanol of 2 times of yellow fluorescent powder quality, mixing, under ultrasonic oscillation, stir, be heated to 150 ℃, keep 0.5h; Add the polyvinyl alcohol of 5 times of yellow fluorescent powder quality, 5 times polyacrylamide then, treat that it dissolves fully after, stir, form gelatinous mixture, obtain the mixed fluorescent powder that cooperates blue chip to use.
Embodiment 2
Cooperate the preparation of the mixed fluorescent powder of blue chip use, may further comprise the steps:
Test two kinds of fluorescent material red fluorescence powder A respectively
1-xB
yO
zN
2/3+4/3y-2/3z: xRe, yellow fluorescent powder Y
3-a-bAl
5Ba
aO
12: Ce
b 3+Chromaticity coordinates and emission wavelength, the screening chromaticity coordinates be: 0.427≤X≤0.437,0.537≤Y≤0.547 is the yellow fluorescent powder of 550≤λ≤560 by the emission wavelength after blue-light excited; The screening chromaticity coordinates is: 0.630≤X≤0.640,0.360≤Y≤0.370 is the red fluorescence powder of 615≤λ≤625 by the emission wavelength after blue-light excited;
With red fluorescence powder and the yellow fluorescent powder of screening mass ratio according to 38: 100, after in the ethanol of 5 times of yellow fluorescent powder quality, mixing, under ultrasonic oscillation, stir, be heated to 100 ℃, maintenance 1h; Add the polyvinyl alcohol of 6 times of yellow fluorescent powder quality, 6 times polyacrylamide then, treat that it dissolves fully after, stir, form gelatinous mixture, obtain the mixed fluorescent powder that cooperates blue chip to use.
Embodiment 3
Cooperate the preparation of the mixed fluorescent powder of blue chip use, may further comprise the steps:
Red fluorescence powder A
1-xB
yO
zN
2/3+4/3y-2/3z: xRe, yellow fluorescent powder Y
3-a-bAl
5Ba
aO
12: Ce
b 3+Screening identical with embodiment 2;
With red fluorescence powder and the yellow fluorescent powder of screening mass ratio according to 45: 100, after in the ethanol of 6 times of yellow fluorescent powder quality, mixing, under ultrasonic oscillation, stir, be heated to 120 ℃, maintenance 0.8h; Add the polyvinyl alcohol of 8 times of yellow fluorescent powder quality, 10 times polyacrylamide then, treat that it dissolves fully after, stir, form gelatinous mixture, obtain the mixed fluorescent powder that cooperates blue chip to use.
Embodiment 4
Cooperate the preparation of the mixed fluorescent powder of blue chip use, may further comprise the steps:
Red fluorescence powder A
1-xB
yO
zN
2/3+4/3y-2/3z: xRe, yellow fluorescent powder Y
3-a-bAl
5Ba
aO
12: Ce
b 3+Screening identical with embodiment 2;
With red fluorescence powder and the yellow fluorescent powder of screening mass ratio according to 40: 100, after in the ethanol of 10 times of yellow fluorescent powder quality, mixing, under ultrasonic oscillation, stir, be heated to 150 ℃, maintenance 1h; Add the polyvinyl alcohol of 10 times of yellow fluorescent powder quality, 10 times polyacrylamide then, treat that it dissolves fully after, stir, form gelatinous mixture, obtain the mixed fluorescent powder that cooperates blue chip to use.
Embodiment 5
Cooperate the preparation of the mixed fluorescent powder of blue chip use, may further comprise the steps:
Red fluorescence powder A
1-xB
yO
zN
2/3+4/3y-2/3z: xRe, yellow fluorescent powder Y
3-a-bA
L5Ba
aO
12: Ce
b 3+Screening identical with embodiment 2;
With red fluorescence powder and the yellow fluorescent powder of screening mass ratio according to 42: 100, after in the ethanol of 3 times of yellow fluorescent powder quality, mixing, under ultrasonic oscillation, stir, be heated to 200 ℃, maintenance 0.6h; Add the polyvinyl alcohol of 5 times of yellow fluorescent powder quality, 5 times polyacrylamide then, treat that it dissolves fully after, stir, form gelatinous mixture, obtain the mixed fluorescent powder that cooperates blue chip to use.
Embodiment 2 prepared mixed fluorescent powders are cooperated with blue chip, after the encapsulation of LED packaging plastic, detect mixed fluorescent powder with spectral power distribution after blue chip cooperates, the result as shown in Figure 1, wherein, X-coordinate is emission peak wavelength (360nm-800nm), ordinate zou is the emmission spectrum relative intensity, as can be seen: use this method encapsulated LED product emission peak width, from all there being tangible fluorescent material emission peak to exist between the 550nm-680nm, colour rendering index Ra can reach 88.7, and colour temperature is 3065k, has illustrated that the mixed fluorescent powder of this method preparation is suitable for the LED of high color rendering index (CRI) low color warm white light.。
Embodiment 3 prepared mixed fluorescent powders cooperate with blue chip, after the encapsulation of LED packaging plastic, detect mixed fluorescent powder with spectral power distribution after blue chip cooperates, the result as shown in Figure 2, wherein, X-coordinate is emission peak wavelength (360nm-800nm), ordinate zou is the emmission spectrum relative intensity, as can be seen: use this method encapsulated LED product emission peak width, from all there being tangible fluorescent material emission peak to exist between the 550nm-700nm, colour rendering index Ra can reach 91.5, and colour temperature is 3400k, has illustrated that the mixed fluorescent powder of this method preparation is suitable for the LED of high color rendering index (CRI) low color warm white light.
Claims (7)
1. a mixed fluorescent powder that cooperates blue chip to use is characterized in that, is with red fluorescence powder A
1-xB
yO
zN
2/3+4/3y-2/3z: xRe and yellow fluorescent powder Y
3-a-bAl
5Ba
aO
12: Ce
b 3+According to 35～50: 100 mass ratio, mixing in the ethanol of 2～10 times of yellow fluorescent powder quality adds the polyvinyl alcohol of 5～10 times of yellow fluorescent powder quality, 5～10 times polyacrylamide again, fully formed gelatinous mixture behind the mixing;
Wherein, A is one or more among Mg, Ca, Sr, the Ba, and B is Si or Si and the mixing of Al, and Re is one or both among Eu, the Mn, 0≤x＜1.0,1.0≤y≤3.0,0＜z≤2.0; 0.01≤a≤0.05,0.05≤b≤0.10.
2. the mixed fluorescent powder that cooperation blue chip as claimed in claim 1 uses, it is characterized in that the chromaticity coordinates of described yellow fluorescent powder is: 0.427≤X≤0.437,0.537≤Y≤0.547 is 550≤λ≤560 by the emission wavelength after blue-light excited;
3. the mixed fluorescent powder that cooperation blue chip as claimed in claim 1 or 2 uses, it is characterized in that, the chromaticity coordinates of described red fluorescence powder is: 0.630≤X≤0.640,0.360≤Y≤0.370 is 615≤λ≤625 by the emission wavelength after blue-light excited.
4. a preparation method who cooperates the mixed fluorescent powder of blue chip use is characterized in that, may further comprise the steps:
With red fluorescence powder A
1-xB
yO
zN
2/3+4/3y-2/3z: xRe and yellow fluorescent powder Y
3-a-bAl
5Ba
aO
12: Ce
b 3+According to 50～35: 100 mass ratio, after in the ethanol of 2～5 times of yellow fluorescent powder quality, mixing, under ultrasonic oscillation, stir, be heated to 100～200 ℃, keep 0.5～1h; Add the polyvinyl alcohol of 5～10 times of yellow fluorescent powder quality, 5～10 times polyacrylamide then, treat that it dissolves fully after, stir, form gelatinous mixture, obtain the mixed fluorescent powder that cooperates blue chip to use;
Wherein, A is one or more among Mg, Ca, Sr, the Ba, and B is that Si or Si mix with Al, and Re is one or both among Eu, the Mn, 0≤x＜1.0,1.0≤y≤3.0,0＜z≤2.0; 0.01≤a≤0.05,0.05≤b≤0.10.
5. the preparation method of the mixed fluorescent powder that cooperation blue chip as claimed in claim 4 uses, it is characterized in that, the chromaticity coordinates of described yellow fluorescent powder is: 0.427≤X≤0.437,0.537≤Y≤0.547 is 550≤λ≤560 by the emission wavelength after blue-light excited;
6. the preparation method of the mixed fluorescent powder that uses as claim 4 or 5 described cooperation blue chips, it is characterized in that, the chromaticity coordinates of described red fluorescence powder is: 0.630≤X≤0.640,0.360≤Y≤0.370 is 615≤λ≤625 by the emission wavelength after blue-light excited.
7. the preparation method of the mixed fluorescent powder that cooperation blue chip as claimed in claim 4 uses is characterized in that the relative molecular weight of described polyvinyl alcohol is 250,000～300,000; The relative molecular weight of polyacrylamide is 8,000,000～10,000,000.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102810605A (en) * | 2011-06-01 | 2012-12-05 | 红蝶科技(深圳)有限公司 | Fluorescent powder based light emitting diode packaging method |
| CN105154081A (en) * | 2015-10-10 | 2015-12-16 | 惠州学院 | YAG phosphor powder doped with Ce<3+>, Pr<3+> and Cr<3+> and preparation method thereof |
| CN110504348A (en) * | 2019-08-23 | 2019-11-26 | 旭宇光电（深圳）股份有限公司 | White light LEDs and Healthy Lighting lamps and lanterns |
| WO2021026959A1 (en) * | 2019-08-14 | 2021-02-18 | 广州硅能照明有限公司 | Cob encapsulation device |
| CN112608687A (en) * | 2020-12-18 | 2021-04-06 | 广州光联电子科技有限公司 | Inorganic adhesive for LED packaging and packaging method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1827734A (en) * | 2005-02-28 | 2006-09-06 | 宜兴新威集团有限公司 | Process for preparing yellow luminescent powder for blue light emission diode |
-
2010
- 2010-09-29 CN CN 201010296849 patent/CN101948692A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1827734A (en) * | 2005-02-28 | 2006-09-06 | 宜兴新威集团有限公司 | Process for preparing yellow luminescent powder for blue light emission diode |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102810605A (en) * | 2011-06-01 | 2012-12-05 | 红蝶科技(深圳)有限公司 | Fluorescent powder based light emitting diode packaging method |
| CN102810605B (en) * | 2011-06-01 | 2016-05-25 | 红蝶科技(深圳)有限公司 | A kind of method for packing of the light emitting diode based on fluorescent material |
| CN105154081A (en) * | 2015-10-10 | 2015-12-16 | 惠州学院 | YAG phosphor powder doped with Ce<3+>, Pr<3+> and Cr<3+> and preparation method thereof |
| WO2021026959A1 (en) * | 2019-08-14 | 2021-02-18 | 广州硅能照明有限公司 | Cob encapsulation device |
| CN110504348A (en) * | 2019-08-23 | 2019-11-26 | 旭宇光电（深圳）股份有限公司 | White light LEDs and Healthy Lighting lamps and lanterns |
| WO2020200327A1 (en) * | 2019-08-23 | 2020-10-08 | 旭宇光电（深圳）股份有限公司 | White light led and lamp for healthy lighting |
| CN112608687A (en) * | 2020-12-18 | 2021-04-06 | 广州光联电子科技有限公司 | Inorganic adhesive for LED packaging and packaging method |
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Application publication date: 20110119 |