CN102161890B - Single-phase white light fluorescent powder based on ultraviolet light-emitting diode (LED) excitation and production method thereof as well as luminescent device - Google Patents
Single-phase white light fluorescent powder based on ultraviolet light-emitting diode (LED) excitation and production method thereof as well as luminescent device Download PDFInfo
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Abstract
The invention relates to a single-phase white light fluorescent powder based on ultraviolet light-emitting diode (LED) excitation and a production method thereof as well as a luminescent device. The chemical formula of the fluorescent powder is Ba (2-x-y-z-a-b) CaxSryMgzLu2-m-n-pYmLanGdSi2O9: aEu<2+>, bMn<2+>, wherein x is large than or equal to 0 and less than or equal to 0.3, y is large than or equal to 0 and less than or equal to 0.1, z is large than or equal to 0 and less than or equal to 0.2, m is large than or equal to 0 and less than or equal to 0.2, n is large than or equal to 0 and less than or equal to 0.2, p is large than or equal to 0 and less than or equal to 0.2, a is large than 0 and less than or equal to 0.14, and b is large than or equal to 0 and less than or equal to 0.05. The preparation method comprises the following steps: grinding and mixing the raw materials; and roasting at high temperature at the reduction atmosphere; and then processing so as to obtain the fluorescent powder. The fluorescent powder has the characteristics of good chemical stability, wide excitation wave band, high luminous intensity, simple production method, no pollution, low cost and the like; and the emission wave length can be regulated according to requirement. A white light LED can be prepared by using an ultraviolet LED chip and the fluorescent powder provided by the invention, and a warm-toned light-regulating source can be produced.
Description
Technical field
The present invention relates to a kind of single-phase white-emitting phosphor and manufacture method and luminescent device that excites based on ultraviolet LED.
Technical background
In recent years, global energy shortage and problem of environmental pollution become increasingly conspicuous, and people urgently wish the new technology of applicating energy-saving environmental protection, and semiconductor lighting is exactly the new technology that possesses this glamour.White light LEDs promptly is basis and the industry development emphasis that semiconductor lighting is used, as a kind of novel illuminating device, have energy-efficient (the equal illumination effect is more energy-conservation more than 80% than conventional light source), life-span long (reality can reach 20,000 hours) but, the unrivaled advantage of many other light sources such as no mercury pollution planar package, be widely used in fields such as pilot lamp, signal lamp, mobile communication equipments, and be expected to replace incandescent light, luminescent lamp and enter lighting field.
White light LEDs can be divided into three types according to the mode of generating white light: the fluorescent material conversion hysteria; The multicore sheet is combined; Single-chip Multiple Quantum Well type.The main path of the white light of the actual generation of fluorescent material conversion hysteria white light LEDs at present, this scheme can be divided into three kinds again: (1) blue-ray LED+yellow fluorescent powder is realized white light; (2) blue-ray LED+red green fluorescence powder constitutes white light; (3) come synthesize white light with ultraviolet LED+redgreenblue fluorescent material.Apply yellow fluorescent powder (Re on the InGaN blue chip at present
1-r, Sm
r)
3(Al
1-s, Ga
s)
5O
12: Ce(is called for short YAG:Ce, sees U.S. Pat 5998925) realized commercialization, but this combination exist glow color with driving voltage and fluorescent coating variation in thickness change, shortcomings such as colour temperature is higher, colour rendering index is low, high temperature cancellation.Excite three primary colors fluorescent powder to realize that the production program of white light can overcome the shortcoming of above-mentioned " champac " combined white light LEDs with the ultraviolet chip.But the coated technique of heterogeneous phosphor combination can be because the problem of certain monochromatic fluorescent material cause whole white light LEDs luminous efficiency decline, even the generation look drifts about.Ultraviolet LED light excitated single phase white fluorescent material has overcome the problems referred to above, has also avoided the regulation and control of red, green, blue three primary colours proportioning and has absorbed problem again.Because vision is to the insensitivity of UV-light, only by a kind of fluorescent material decision, therefore, colour stable, color reducibility and colour rendering index height have important application prospects to the color of this class white light LEDs in White-light LED illumination of new generation.
Reported single-phase white-emitting phosphor mainly contains: 2004, Kim etc. successively developed Ba
3MgSi
2O
8: Eu
2+, Mn
2+, Sr
3MgSi
2O
8: Eu
2+And Sr
3MgSi
2O
8: Eu
2+, Mn
2+Three kinds of single-phase white-emitting phosphors [J.S.Kim, P.E. Jeon etc., Appl. Phys. Lett., 2004,85 (15): 2931; Appl. Phys. Lett., 2004,85 (17): 3696].2005, Setlur etc. reported a kind of single-phase white-emitting phosphor that is suitable for ultraviolet excitation, and its composition is Ca
2NaMg
2V
3O
12: Eu
3+, maximum excitation wavelength is [A.A. Setlur, H.A. Comanzo etc., J. Electrochem. Soc. 2005,152 (12): H205] about 330nm; Zhang Jiahua etc. have developed and have consisted of Eu
XySr
Y-xySi
zO
2z+y+1Single-phase white-emitting phosphor [patent of invention, contriver Zhang Jiahua, Sun Xiaoyuan, Wang Xiaojun, Zhang Xia, the patent No. 200510016743.9, Granted publication CN100404639C].2006, Yang Zhi equality was reported Sr
2MgSiO
5: (Eu
2+, Mn
2+) and Ca
2SiO
3Cl
2: Eu
2+The luminosity of single-matrix white fluorescent powder [Yang Zhiping, Liu Yufeng etc., silicate journal, 2006,34 (10): 1195; Luminous journal, 2006,27 (4): 629.]; Tian Yiguang etc. have invented a kind of with MOaAl
2O
3BSiO
2CL:dX is the fluorescent material [patent of invention, contriver Tian Yiguang, Gong Bingyong, patent No. application number 200610167935.4, Granted publication CN100554373C] of main component.2007, Kim etc. reported X
3MgSi
2O
8: Eu
2+, Mn
2+(X=Ba, Sr, Ca) white fluorescent powder [J.S. Kim, A.K. Kwon, Y.H. Park etc., J. Lumin., 2007,122-123:583]; Sun etc. discover 2SrOMgOxSiO
2: Eu
2+In, adjust sample SiO
2Content can modulated luminescence [X.Y. Sun, J.H. Zhang, X. Zhang etc., J. Lumin., 2007,122-123:955].2008, He etc. reported LED white fluorescent powder Mg
0.1Sr
1.9SiO
4: Eu
2+[H. He, R.L. Fu, X.F. Song etc., J. Lumin., 2008,128 (3): 489]; Zhang etc. have reported Li
2SrSiO
4: 0.01Eu, xCe white emitting fluorescent powder [X.L. Zhang, H. He, Z.S. Li etc., J. Lumin., 2008,128 (12): 1876]; Shen etc. have reported Ba
2MgSi
2-xAl
xO
7: 0.1Eu
2+, 0.1Mn
2+White emitting fluorescent powder [C.Y. Shen, Y. Yang, S.Z. Jin, etc., Opt. Int. J. Light Electron. Opt. 2008, doi:10.1016/j.ijleo.2008.05.009].2009, Zhang Xia etc. developed and have consisted of Sr
5-m-nSi
zO
n(SiO
4)
2Cl
2: Eu
2+ mNear ultraviolet excitation under single-phase white-emitting phosphor [patent of invention, contriver Zhang Xia, Zhang Jiahua, number of patent application 200910067076.5, publication number CN101565620A]; Yang Zhi equality has been studied Ca
10(Si
2O
7)
3Cl
2: Eu
2+, Mn
2+White luminescent material characteristic [Yang Zhiping, Lee expects, Wang Zhijun etc., Science Bulletin, 2009,54 (13): 1855.].Employing high temperature solid-state methods such as tight Xiao Song had synthesized a kind of single phase LiCa in 2010
3MgV
3O
12: Eu
3+White-light emitting powder [Yan Xiaosong, Li Wanwan, Liu Ji, Sun Kang, luminous journal, 2010,31 (1): 39].
As can be seen, alkaline earth metal silicate or Chlorosilicate matrix are the first-selected systems of single-phase white-emitting phosphor.Yet from such fluorescent material of having released at present, the system kind is less, is difficult to obtain low colour temperature, and luminous intensity also has the space of further raising.
Summary of the invention
The object of the present invention is to provide a kind of single-phase white-emitting phosphor and manufacture method and luminescent device that excites based on ultraviolet LED, with the new single phase silicate substrate that contains rare earth element, by singly mixing or codope, obtain white emitting fluorescent powder with modes such as changing the matrix composition, greatly improved its luminous efficiency, improved the matching of it and ultraviolet LED chip, therefore can make white luminous device, and can be made into the warm tones light source with the ultraviolet LED chip portfolio.
Technical scheme of the present invention is:
The chemical formula of the single-phase white-emitting phosphor that excites based on ultraviolet LED is:
Ba
(2-x-y-z-a-b)Ca
xSr
yMg
zLu
2-m-n-pY
mLa
nGd
pSi
2O
9:?aEu
2+,bMn
2+
0≤x≤0.3 wherein; 0≤y≤0.1; 0≤z≤0.2; 0≤m≤0.2; 0≤n≤0.2; 0≤p≤0.2; 0＜a≤0.14; 0≤b≤0.05.
The manufacture method of making the above-mentioned single-phase white-emitting phosphor that excites based on ultraviolet LED mainly comprises the steps:
(1) simple substance, oxide compound, halogenide or the corresponding salt with Mg, Ca, Sr, Ba, Y, La, Lu, Gd, Eu, Mn is raw material, and takes by weighing corresponding described raw material by the chemical formula composition and the stoichiometry of above-mentioned materials;
(2) the said mixture material is at high temperature carried out reducing roasting;
(3), promptly make the LED silicate fluorescent powder that the present invention relates to again through last handling process.
In described step (2), the reducing roasting number of times can be once, or repeatedly.
In described step (2), the reducing roasting temperature is 1100-1500 ℃.
In described step (2), the single reducing roasting time is 0.5-20 hours.
In described step (3), last handling process is a conventional process, after the reducing roasting product fragmentation soon, after fully grinding, and can use deionization washing 3～20 times, filters the process of oven dry.
A kind of luminescent device, the single-phase white-emitting phosphor Ba that contains the ultraviolet leds chip at least and excite based on ultraviolet LED
(2-x-y-z-a-b)Ca
xSr
yMg
zLu
2-m-n-pY
mLa
nGd
pSi
2O
9: aEu
2+, bMn
2+Manufacturing
Wherein, 0≤x≤0.3; 0≤y≤0.1; 0≤z≤0.2; 0≤m≤0.2; 0≤n≤0.2; 0≤p≤0.2; 0＜a≤0.14; 0≤b≤0.05.
Described luminescent device contains one or more different described fluorescent material Ba that form
(2-x-y-z-a-b)Ca
xSr
yMg
zLu
2-m-n-pY
mLa
nGd
pSi
2O
9: aEu
2+, bMn
2+
Its glow color of described luminescent device is a white.
Described luminescent device also can be made into low colour temperature, warm tones light source.
Adopt the beneficial effect of method of the present invention to be: the fluorescent material that 1, the present invention relates to not sulfur-bearing, rare earth participates in single phase composition, has bigger composition and selects and adjust leeway, stable performance.The excitation spectrum broad of the fluorescent material that 2, the present invention relates to, all very good from the stimulation effect of 250nm-410nm scope, therefore be fit to very much ultraviolet LED and excite (see figure 1).3, the fluorescent material that the present invention relates to emissive porwer under above-mentioned condition excites is very high, helps improving the luminous efficiency of LED; This is singly to mix or the method for codope and the matrix components that special rare earth participates in because the present invention has adopted; 4, the fluorescent material manufacture method simple possible that the present invention relates to is convenient to large-scale production; 5, the present invention provides a kind of simple pathway that adopts conventional led chip to realize the high-level efficiency white-light illuminating, and can be made into the warm tones light source according to the characteristic of the fluorescent material of being invented.
Description of drawings
Fig. 1 is Ba
1.925Lu
2Si
2O
9: 0.06Eu
2+, 0.015Mn
2+The exciting light spectrogram.
Fig. 2 is Ba
1.925Lu
2Si
2O
9: 0.06Eu
2+, 0.015Mn
2+Emmission spectrum figure.
Embodiment
Below in conjunction with drawings and Examples the present invention is done and to describe in further detail.
Embodiment 1:
Embodiment 1: take by weighing BaCO
31.3025g, SiO
20.4006g, Lu
2O
31.3266g, Eu
2O
30.0117g, BaCO
3, SiO
2Be analytical pure, Lu
2O
3, Eu
2O
3Purity be 4N and more than, with above raw material mix grinding evenly after, at 1100～1500 ℃ under carbon reduction atmosphere or H
2Or N
2/ H
2Under the reducing atmosphere, roasting 3～5 hours is ground behind the naturally cooling, with product washing 3 times, filters, and dries under 120 ℃ of conditions, promptly gets and consists of Ba
1.98Lu
2Si
2O
9: 0.12Eu
2+(be a=0.12, b=0).Its excitation spectrum excitation peak broad, the stimulation effect of the light of 250nm-410nm range of wavelength is better, therefore is applicable to ultraviolet leds chip etc.Its chromaticity coordinates is (0.2331,0.2440), and it is luminous to be pearl opal.
Embodiment 2-embodiment 6
Except that forming by the chemical formula of each embodiment in the table 1 and stoichiometry takes by weighing the raw material, remaining manufacturing step is all identical with embodiment 1, obtains chemical constitution, chromaticity coordinates, relative brightness and sees Table 1.
The chemical formula of table 1 embodiment 1-14 and chromaticity coordinates thereof and relative brightness
| Embodiment | Chemical formula | Chromaticity coordinates (x, y) | Relative brightness |
| 1 | Ba 1.98Lu 2Si 2O 9: 0.02Eu 2+ | 0.2331,0.2440 | 1.009 |
| 2 | Ba 1.96Lu 2Si 2O 9: 0.04Eu 2+ | 0.2233,0.2214 | 1.124 |
| 3 | Ba 1.94Lu 2Si 2O 9: 0.06Eu 2+ | 0.2149,0.2118 | 1.279 |
| 4 | Ba 1.92Lu 2Si 2O 9: 0.08Eu 2+ | 0.2226,0.2229 | 1.109 |
| 5 | Ba 1.9Lu 2Si 2O 9: 0.10Eu 2+ | 0.2352,0.2298 | 1.108 |
| 6 | Ba 1.88Lu 2Si 2O 9: 0.12Eu 2+ | 0.2411,0.2592 | 0.980 |
Embodiment 7:BaCO
31.2663g, SiO
20.4006g, Lu
2O
31.3266g, Eu
2O
30.0352g, MnCO
30.0057 g, MnCO
3Be analytical pure.At 1100～1500 ℃ under carbon reduction atmosphere or H
2Or N
2/ H
2Under the reducing atmosphere, roasting 3～5 hours is ground behind the naturally cooling, with product washing 3 times, filters, and dries under 120 ℃ of conditions, and obtaining chemical formula is Ba
1.925Lu
2Si
2O
9: 0.06Eu
2+, 0.015Mn
2+(be a=0.06, fluorescent material b=0.015).Its excitation spectrum excitation peak broad, the stimulation effect of the light of 250nm-410nm range of wavelength is better, therefore is applicable to ultraviolet leds chip etc.Its chromaticity coordinates x=0.2598, y=0.2297; Excite with emmission spectrum and see Fig. 1 and Fig. 2.
Embodiment 16-embodiment 23
Except that chemical formula composition and stoichiometry by each embodiment in the table 2 take by weighing the raw material, remaining manufacturing step is all identical with embodiment 15, obtains chemical constitution, chromaticity coordinates, relative brightness, colour temperature and colour rendering index and sees Table 2.
The chemical formula of table 2 embodiment 7-16 and chromaticity coordinates thereof and relative brightness
Embodiment 8-embodiment 16
Except that forming by the chemical formula of each embodiment in the table 1 and stoichiometry takes by weighing the raw material, remaining manufacturing step is all identical with embodiment 7, obtains chemical constitution, chromaticity coordinates, relative brightness and sees Table 2.
Embodiment 17 adopts the fluorescent material of embodiment 1 gained to be coated on the ultraviolet LED chip, has welded circuit, uses the resin sealed knot, can obtain white light emitting device of the present invention.
Embodiment 18 adopts the fluorescent material of embodiment 16 gained to be coated on the ultraviolet LED chip, has welded circuit, uses the resin sealed knot, can obtain white light emitting device of the present invention.The device that this device obtains with respect to embodiment 1 has lower colour temperature.
Embodiment 19 adopts the fluorescent material of embodiment 14 gained to be coated on the ultraviolet LED chip, has welded circuit, uses the resin sealed knot, can obtain white light emitting device of the present invention.The device that this device obtains with respect to embodiment 18 has lower colour temperature.
Embodiment 20 adopts the fluorescent material of embodiment 12 gained to be coated on the ultraviolet LED chip, has welded circuit, uses the resin sealed knot, can obtain white light emitting device of the present invention.The device that this device obtains with respect to embodiment 12 has lower colour temperature, is warm tones.
Embodiment 21 adopts the fluorescent material and the red fluorescence powder of embodiment 7 gained to be coated in together on the ultraviolet LED chip, has welded circuit, uses the resin sealed knot, can obtain white light emitting device of the present invention.The device that this device obtains with respect to embodiment 17 has lower colour temperature, is the warm tones light source.
Claims (2)
1. single-phase white-emitting phosphor that excites based on ultraviolet LED, it is characterized in that: the chemical formula of this material is:
Ba
(2-x-y-z-a-b)Ca
xSr
yMg
zLu
2-m-n-pY
mLa
nGd
pSi
2O
9:?aEu
2+,bMn
2+
0≤x≤0.3 wherein; 0≤y≤0.1; 0≤z≤0.2; 0≤m≤0.2; 0≤n≤0.2; 0≤p≤0.2; 0＜a≤0.14; 0≤b≤0.05.
2. manufacture method of making the described single-phase white-emitting phosphor that excites based on ultraviolet LED of claim 1 is characterized in that:
(1) with simple substance, oxide compound or the corresponding salt of Mg, Ca, Sr, Ba, Y, La, Lu, Gd, Eu, Mn, and SiO
2Be raw material, and take by weighing corresponding described raw material by the chemical formula composition and the stoichiometry of above-mentioned materials;
(2) the said mixture material is at high temperature carried out reducing roasting, the reducing roasting number of times is an one or many, and the single time of reducing roasting is 0.5-20 hours, and the temperature of reducing roasting is 1100-1500 ℃;
(3) again through last handling process, after the reducing roasting product fragmentation soon, after fully grinding, and use deionization washing 3～20 times, to filter, the process of oven dry is made the single-phase white-emitting phosphor that excites based on ultraviolet LED.
3
.A kind of luminescent device is characterized in that: contain the described single-phase white-emitting phosphor Ba that excites based on ultraviolet LED of ultraviolet leds chip and claim 1 at least
(2-x-y-z-a-b)Ca
xSr
yMg
zLu
2-m-n-pY
mLa
nGd
pSi
2O
9: aEu
2+, bMn
2+
Wherein, 0≤x≤0.3; 0≤y≤0.1; 0≤z≤0.2; 0≤m≤0.2; 0≤n≤0.2; 0≤p≤0.2; 0＜a≤0.14; 0≤b≤0.05.
4
.Luminescent device according to claim 3 is characterized in that: contain one or more different described fluorescent material Ba that form
(2-x-y-z-a-b)Ca
xSr
yMg
zLu
2-m-n-pY
mLa
nGd
pSi
2O
9: aEu
2+, bMn
2+
5
.Luminescent device according to claim 3 is characterized in that: its glow color is white.
6
.Luminescent device according to claim 3 is characterized in that: also can be made into low colour temperature, warm tones light source.
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|---|---|---|---|
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