CN102643644A - Light emitting diode (LED) fluorescent powder with single matrix white light excited by near ultraviolet and preparation method thereof - Google Patents
Light emitting diode (LED) fluorescent powder with single matrix white light excited by near ultraviolet and preparation method thereof Download PDFInfo
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- CN102643644A CN102643644A CN2012101108279A CN201210110827A CN102643644A CN 102643644 A CN102643644 A CN 102643644A CN 2012101108279 A CN2012101108279 A CN 2012101108279A CN 201210110827 A CN201210110827 A CN 201210110827A CN 102643644 A CN102643644 A CN 102643644A
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Abstract
The invention discloses a light emitting diode (LED) fluorescent powder with single matrix white light excited by near ultraviolet and a preparation method thereof, the chemical formula of fluorescent powder is that: NM1-x-y-zPO4:xR, yG, zB, wherein N is freely selected from at least one of a group formed by Li, Na and K; M is freely selected from at least one of a group formed by Mg, Ca, Sr, Ba and Zn; R is freely selected from at least one of a group formed by Mn and Sm; G is Tb; and B is freely selected from at least one of a group formed by Ce and Eu, and x is higher than 0 but lower than 0.25, y is higher than 0 but lower than 0.25, and z is higher than 0 but lower than 0.25. The particle size of the prepared fluorescent according to the method provided by the invention is small and uniform, doping of fluorescent material activator on a molecule level is realized, three bands of red, green and blue can be emitted by excitation of near ultraviolet of 350-410nm, the color display index is high, and can be used in the white light LED excited by near ultraviolet.
Description
Technical field
The present invention relates to a kind of fluorescent material and preparation method thereof, particularly a kind of single-matrix white fluorescent powder that is used near ultraviolet excitated white light LEDs and preparation method thereof.
Background technology
Light conversion hysteria white light LEDs has power saving, volume is little, thermal value is low, the life-span is long, response is fast, antidetonation is anti-ly dashed, but recyclable, pollution-free planar package, easy exploiting becomes advantages such as compact product, is the new light sources of 21 century most worthy.
At present the realization approach of light conversion hysteria white light LEDs mainly contains following three kinds: 1. blue chip+yellow fluorescent powder: with blue-light LED chip is basic light source, excites yellow fluorescent powder, utilizes lens principle that complementary gold-tinted and blue light are obtained white light.This method is simple in structure, and manufacturing process requirement is lower, but the white light LEDs glow color that obtains can be with driving voltage and fluorescent coating variation in thickness, and owing to lack the ruddiness composition, is not easy to realize low color temperature white light, and color reducibility is poor, and colour rendering index is low.2. blue chip+green and red fluorescence powder are basic light source with blue-light LED chip, and simultaneous excitation is red, two kinds of fluorescent material of green, and obtain white light with unabsorbed blue light.This mode has increased the composition of green glow and ruddiness; Therefore color reducibility and colour rendering index have effectively been improved; But still exist the glow color can be with the shortcoming of driving voltage and fluorescent coating variation in thickness, in addition, the fluorescent material that can be complementary with blue-light LED chip at present also seldom.3. near ultraviolet chip+RGB fluorescent material: excite three kinds of fluorescent material of red, green, blue with high brightness near ultraviolet LED chip, produce the three primary colours light emission, the compound white light that obtains.The white light LEDs glow color that this method obtains only by the decision of fluorescent material proportioning, is realized the white light that glow color is stable more easily, and its luminous efficiency and colour rendering index are all well a lot of than blue chip+yellow fluorescent powder.But owing to mixed multiple fluorescent material, there are color absorption again, energy waste, proportioning regulation and control and rate of ageing different problems between mixture, cause luminous efficiency and color rendition performance to be a greater impact, also increased cost simultaneously.
If can adopt the near ultraviolet LED chip; Excite single-matrix fluorescent material with three emission peaks of red, green, blue; It is poor that this method has promptly overcome the color reducibility of blue chip+yellow fluorescent powder; The shortcoming that colour rendering index is low simultaneously owing to only have single-matrix, can solve color absorption again between the mixture of near ultraviolet chip+RGB fluorescent material, energy waste, proportioning regulation and control and the equal problem of rate of ageing again.
Can be used near ultraviolet excitated single-matrix white fluorescent powder many cases type and transmission ofenergy type two big classes are arranged at present.For example, (luminous journal, 2005, the 26:404-406) Sr of report such as Sun Xiaoyuan
2MgSiO
5: Eu
2+, (Journal of Alloys and Compounds, 2010, the 498:139-142) BaSrMg (PO of report such as Zhan-Chao Wu
4)
2: Eu
2+And the disclosed A of the Chinese patent of application number 200910021829.9
1-x-yDy
xBi
yMg
1-zZn
zAl
11O
19(A=La, Ce, Y, Gd) fluorescent material etc. belongs to many cases type list substrate fluorescent powder, and the emmission spectrum of this type fluorescent material forms white light by blue light and yellow light mix, and because of having only a kind of activator, its mixing color is difficulty comparatively.(Optics & Laser Technology, 2011, the 43:1351-1354) NaSr of report such as Chongfeng Guo
4(BO
3)
3: Ce
3+, Tb
3+, (Inorg.Chem.2009,48:11525-11532) Ca of report such as Ki Hyuk Kwon
6-x-yMg
X-z(PO
4)
4: Eu
y 2+, Mn
z 2+, the disclosed Sr of the Chinese patent of application number 200910272541.9
2-mMg
3-nP
4O
15: Eu
m 2+, Mn
n 2+, the disclosed Ca of the Chinese patent of application number 201010576944.5
8Mg (SiO
4)
4Cl
2: Eu
2+, Mn
2+, the disclosed Ca of the Chinese patent of application number 201010241854.0
2SiO
3Cl
2: xEu
2+, yMn
2+Homenergic transmission type list substrate fluorescent powder has only blueness, red two luminescence center, and the LED color developing that encapsulation forms is not high; Single substrate fluorescent powder of three activator has the few of report at present, and application number is that 200500142908 Taiwan patent discloses (Y
1-xGd
x) BO
3: Ce
3+, Tb
3+, Eu
3+, Y
2SiO
5: Ce
3+, Tb
3+, Eu
3+Two kinds of fluorescent material, (ACS Appl.Mater.Interfaces, 2012,4:296-305 such as Guogang Li; J.Phys.Chem.C, 2011,115:21882-21892) reported Ca
4Y
6(SiO
4)
6O:Ce
3+/ Mn
2+/ Tb
3+, Mg
2Y
8(SiO
4)
6O
2: Ce
3+/ Mn
2+/ Tb
3+Fluorescent material, (J.Phys.Chem.C 2011,115,2349-2355) wait and reported Ca for Chien-Hao Huang
3Y (GaO)
3(BO
3)
4: Ce
3+, Mn
2+, Tb
3+Fluorescent material, and Wei L ü etc. (Inorg.Chem.2011,50,7846-7851) reported BaMg
2Al
6Si
9O
30: Eu
2+, Tb
3+, Mn
2+Fluorescent material, and Xi Chen etc. (Journal of Luminescence, 2011,131:2697-2702) reported Sr
1.5Ca
0.5SiO
4: Eu
3+, Tb
3+, Eu
2+Fluorescent material, the single substrate fluorescent powder colour rendering index of this type is high, but mostly it is silicate borate matrix; Its compound method is confined to solid sintering technology more, and preparation temperature is higher, and pattern is inhomogeneous; The fluorescent material particle diameter is bigger, need repeatedly ball milling, and ball milling can reduce the luminous intensity of fluorescent material.
Summary of the invention
The present invention aims to provide a kind of single-matrix white fluorescent powder that is used near ultraviolet excitated white light LEDs and preparation method thereof.
Chemical expression according to the single-matrix white fluorescent powder of near ultraviolet excited white light LED of the present invention is: NM
1-x-y-zPO
4: xR, yG, zB, wherein N is selected from by Li, Na, at least a in the group that K formed; M is selected from by Mg, Ca, Sr, Ba, at least a in the group that Zn formed; R is selected from by Mn, at least a in the group that Sm formed; G is Tb; B is selected from by Ce, at least a in the group that Eu formed, and 0＜x＜0.25,0＜y＜0.25,0＜z＜0.25.
Fluorescent material median size of the present invention is preferably 50-60nm, and colour rendering index Ra is 86-87.5.
The preparation method of above-mentioned fluorescent material comprises:
Take by weighing N respectively by the stoichiometric ratio in the above-mentioned chemical expression, M, R, G, the oxide compound of B, nitrate salt or carbonate, and NH
4H
2PO
4
Add rare nitric acid and make the N that takes by weighing, M, R, G, the oxide compound of B, nitrate salt or carbonate are dissolved in the deionized water fully, and then add complexing agent formation 0.1-0.4mol/L metal ion solution;
With the NH that takes by weighing
4H
2PO
4Be dissolved in the PO that deionized water forms 0.1-0.4mol/L
4 3-Solution, add coupling agent then and form anion solutions;
Metal ion solution is joined in 70-90 ℃ of water-bath and the anion solutions with the 100-300rpm stirring with 0.01-0.1L/Min speed; After adding metal ion solution; Continue to stir,, filter then and in 120-180 ℃ of oven dry 2-10h until forming transparent gel; And
Product after the oven dry is being obtained said fluorescent material under the reducing atmosphere behind 900-1100 ℃ of following roasting 1-10h.
In preferred version of the present invention, complexing agent is a Hydrocerol A, and the molar concentration rate of itself and metals ion is 0.25-4, and coupling agent is a Macrogol 2000 0, and the mass ratio of itself and complexing agent is 0.1-10.
In another preferred version of the present invention, reducing atmosphere is carbon monoxide, hydrogen or nitrogen/hydrogen gas mixture.
Can launch the bands of a spectrum of three wave bands of red, green, blue after by the 350-410nm near ultraviolet excitation by the fluorescent material of the present invention preparation, thereby three bands of a spectrum stacks have realized white light emission in single-matrix; Fluorescent powder grain by the present invention's preparation is tiny even, has realized the doping on the fluorescent material activator molecular level, and synthetic fluorescent material colour rendering index is high, can be used near ultraviolet excitated white light LEDs.
Embodiment
For better explanation the present invention, provide following examples and set forth.It will be appreciated by those skilled in the art that the present invention is not limited to the embodiment that is lifted.
Embodiment 1
Take by weighing LiNO
3, Ca (NO
3)
24H
2O, Tb (NO
3)
36H
2O, Eu (NO
3)
36H
2O, MnCO
3Each 0.6895g, 2.1254g, 0.1360g, 0.0089g, 0.0553g add an amount of rare nitric acid it are dissolved in the deionized water fully, form the 0.1mol/L metal ion solution, add the 2.1g Hydrocerol A and stir subsequent use.Take by weighing the NH of 1.1503g
4H
2PO
4, be dissolved in deionized water and form 0.4mol/L solution, in solution, add the Macrogol 2000 0 of 0.2g then, form anion solutions, stir; Metal ion solution is joined in 85 ℃ of water-baths and the anion solutions with the 200rpm stirring with 0.02L/Min speed, be stirred to always and form transparent gel.Filter, 180 ℃ of oven dry 2h, the sample after the oven dry is under 95% nitrogen/5% hydrogen mixed atmosphere, in 1050 ℃ of following roasting 3h.Fluorescent material median size 50nm, colour rendering index Ra are 86.
Embodiment 2
Take by weighing KNO
3, Sr (NO
3)
2, Ce (NO
3)
36H
2O, Tb (NO
3)
36H
2O, Sm (NO
3)
36H
2Each 1.011g of O, 1.8624g, 0.0868g, 0.1812g, 0.1778g are dissolved in the deionized water fully, form the 0.3mol/L metal ion solution, add the 3.5g Hydrocerol A and stir subsequent use.Take by weighing the NH of 1.1503g
4H
2PO
4, be dissolved in deionized water and form 0.2mol/L solution, in solution, add the Macrogol 2000 0 of 0.2g then, form anion solutions, stir; Metal ion solution is joined in 80 ℃ of water-baths and the anion solutions with the 250rpm stirring with 0.01L/Min speed, be stirred to always and form transparent gel.Filter, 160 ℃ of oven dry 3h, the sample after the oven dry is under carbon monoxide atmosphere, in 1000 ℃ of following roasting 4h.Fluorescent material median size 60nm, colour rendering index Ra are 87.5.
Embodiment 3
Take by weighing Na
2CO
3, Zn (NO
3)
26H
2O, Tb (NO
3)
36H
2O, Eu (NO
3)
36H
2O, MnCO
3Each 1.0539g, 2.5287g, 0.1812g, 0.0089g, 0.1035g add an amount of rare nitric acid it are dissolved in the deionized water fully, form the 0.4mol/L metal ion solution, add the 4.2g Hydrocerol A and stir subsequent use.Take by weighing the NH of 1.1503g
4H
2PO
4, be dissolved in deionized water and form 0.3mol/L solution, in solution, add the Macrogol 2000 0 of 0.5g then, form anion solutions, stir; Metal ion solution is joined in 90 ℃ of water-baths and the anion solutions with the 200rpm stirring with 0.1L/Min speed, be stirred to always and form transparent gel.Filter, 130 ℃ of oven dry 5h, the sample after the oven dry is under hydrogen atmosphere, in 950 ℃ of following roasting 8h.Fluorescent material median size 56nm, colour rendering index Ra are 87.
Claims (5)
1. the single-matrix white fluorescent powder of a near ultraviolet excited white light LED, its chemical expression is: NM
1-x-y-zPO
4: xR, yG, zB, wherein N is selected from by Li, Na, at least a in the group that K formed; M is selected from by Mg, Ca, Sr, Ba, at least a in the group that Zn formed; R is selected from by Mn, at least a in the group that Sm formed; G is Tb; B is selected from by Ce, at least a in the group that Eu formed, and 0＜x＜0.25,0＜y＜0.25,0＜z＜0.25.
2. the fluorescent material of claim 1, wherein the fluorescent material median size is 50-60nm, colour rendering index Ra is 86-87.5.
3. method of making claim 1 or 2 described fluorescent material comprises:
Stoichiometric ratio by in the described chemical expression of claim 1 takes by weighing N respectively, M, R, G, the oxide compound of B, nitrate salt or carbonate, and NH
4H
2PO
4
Add rare nitric acid and make the N that takes by weighing, M, R, G, the oxide compound of B, nitrate salt or carbonate are dissolved in the deionized water fully, and then add complexing agent formation 0.1-0.4mol/L metal ion solution;
With the NH that takes by weighing
4H
2PO
4Be dissolved in the PO that deionized water forms 0.1-0.4mol/L
4 3-Solution, add coupling agent then and form anion solutions;
Metal ion solution is joined in 70-90 ℃ of water-bath and the anion solutions with the 100-300rpm stirring with 0.01-0.1L/Min speed; After adding metal ion solution; Continue to stir,, filter then and in 120-180 ℃ of oven dry 2-10h until forming transparent gel; And
Product after the oven dry is being obtained said fluorescent material under the reducing atmosphere behind 900-1100 ℃ of following roasting 1-10h.
4. the method for claim 3, wherein complexing agent is a Hydrocerol A, and the molar concentration rate of itself and metals ion is 0.25-4, and coupling agent is a Macrogol 2000 0, and the mass ratio of itself and complexing agent is 0.1-10.
5. the method for claim 3, wherein reducing atmosphere is carbon monoxide, hydrogen or nitrogen/hydrogen gas mixture.
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Cited By (10)
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| CN102863958A (en) * | 2012-10-22 | 2013-01-09 | 中国科学院新疆理化技术研究所 | Lithium phosphate magnesium photoexitation luminescent material doped with rare earth and preparation method thereof |
| CN102911663A (en) * | 2012-09-29 | 2013-02-06 | 浙江工业大学 | White light phosphor powder using calcium carbonate as only substrate and preparation method thereof |
| CN103087714A (en) * | 2013-01-23 | 2013-05-08 | 重庆大学 | Single matrix white phosphor for LED (light emitting diode) and preparation method thereof |
| CN103087712A (en) * | 2013-01-23 | 2013-05-08 | 重庆大学 | Single matrix white phosphor and preparation method thereof |
| CN103194230A (en) * | 2013-04-23 | 2013-07-10 | 中国科学院新疆理化技术研究所 | Europium and samarium-doped lithium magnesium phosphate photostimulated luminescent material and preparation method thereof |
| CN103666468A (en) * | 2014-01-08 | 2014-03-26 | 轻工业部南京电光源材料科学研究所 | Purple light LED (Light-emitting Diode) excited broadband spectrum fluorescent powder and preparation method thereof |
| CN110229669A (en) * | 2019-06-30 | 2019-09-13 | 齐齐哈尔大学 | Lithium phosphate barium red fluorescence powder and preparation method thereof |
| CN110283590A (en) * | 2019-06-30 | 2019-09-27 | 齐齐哈尔大学 | Lithium phosphate barium blue-green fluorescent powder and preparation method thereof |
| CN112300798A (en) * | 2020-10-30 | 2021-02-02 | 东台市天源光电科技有限公司 | High-color-rendering environment-friendly red fluorescent powder and preparation method thereof |
| CN114231283A (en) * | 2022-01-24 | 2022-03-25 | 西安建筑科技大学 | Phosphate blue fluorescent powder excited by near ultraviolet light, preparation method thereof and white light LED light-emitting device |
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| CN102911663A (en) * | 2012-09-29 | 2013-02-06 | 浙江工业大学 | White light phosphor powder using calcium carbonate as only substrate and preparation method thereof |
| CN102911663B (en) * | 2012-09-29 | 2014-09-10 | 浙江工业大学 | White light phosphor powder using calcium carbonate as only substrate and preparation method thereof |
| CN102863958B (en) * | 2012-10-22 | 2014-07-30 | 中国科学院新疆理化技术研究所 | Lithium phosphate magnesium photoexitation luminescent material doped with rare earth and preparation method thereof |
| CN102863958A (en) * | 2012-10-22 | 2013-01-09 | 中国科学院新疆理化技术研究所 | Lithium phosphate magnesium photoexitation luminescent material doped with rare earth and preparation method thereof |
| CN103087712A (en) * | 2013-01-23 | 2013-05-08 | 重庆大学 | Single matrix white phosphor and preparation method thereof |
| CN103087714A (en) * | 2013-01-23 | 2013-05-08 | 重庆大学 | Single matrix white phosphor for LED (light emitting diode) and preparation method thereof |
| CN103087714B (en) * | 2013-01-23 | 2014-12-17 | 重庆大学 | Single matrix white phosphor for LED (light emitting diode) and preparation method thereof |
| CN103194230A (en) * | 2013-04-23 | 2013-07-10 | 中国科学院新疆理化技术研究所 | Europium and samarium-doped lithium magnesium phosphate photostimulated luminescent material and preparation method thereof |
| CN103194230B (en) * | 2013-04-23 | 2014-09-10 | 中国科学院新疆理化技术研究所 | Europium and samarium-doped lithium magnesium phosphate photostimulated luminescent material and preparation method thereof |
| CN103666468A (en) * | 2014-01-08 | 2014-03-26 | 轻工业部南京电光源材料科学研究所 | Purple light LED (Light-emitting Diode) excited broadband spectrum fluorescent powder and preparation method thereof |
| CN110229669A (en) * | 2019-06-30 | 2019-09-13 | 齐齐哈尔大学 | Lithium phosphate barium red fluorescence powder and preparation method thereof |
| CN110283590A (en) * | 2019-06-30 | 2019-09-27 | 齐齐哈尔大学 | Lithium phosphate barium blue-green fluorescent powder and preparation method thereof |
| CN110283590B (en) * | 2019-06-30 | 2022-04-26 | 齐齐哈尔大学 | Lithium barium phosphate blue-green fluorescent powder and preparation method thereof |
| CN112300798A (en) * | 2020-10-30 | 2021-02-02 | 东台市天源光电科技有限公司 | High-color-rendering environment-friendly red fluorescent powder and preparation method thereof |
| CN114231283A (en) * | 2022-01-24 | 2022-03-25 | 西安建筑科技大学 | Phosphate blue fluorescent powder excited by near ultraviolet light, preparation method thereof and white light LED light-emitting device |
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Application publication date: 20120822 |