CN101565620B - Single-phase white light phosphor excited by near-ultraviolet light and preparation method thereof - Google Patents
Single-phase white light phosphor excited by near-ultraviolet light and preparation method thereof Download PDFInfo
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- CN101565620B CN101565620B CN2009100670765A CN200910067076A CN101565620B CN 101565620 B CN101565620 B CN 101565620B CN 2009100670765 A CN2009100670765 A CN 2009100670765A CN 200910067076 A CN200910067076 A CN 200910067076A CN 101565620 B CN101565620 B CN 101565620B
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910004283 SiO 4 Inorganic materials 0.000 claims abstract description 25
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 13
- 230000005284 excitation Effects 0.000 claims abstract description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 20
- 238000005303 weighing Methods 0.000 claims description 9
- 229910052593 corundum Inorganic materials 0.000 claims description 8
- 239000010431 corundum Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 3
- 230000007547 defect Effects 0.000 abstract 1
- 230000009103 reabsorption Effects 0.000 abstract 1
- 238000009877 rendering Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 239000003086 colorant Substances 0.000 description 5
- 229910017639 MgSi Inorganic materials 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000000695 excitation spectrum Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 208000011038 Cold agglutinin disease Diseases 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 208000020345 childhood apraxia of speech Diseases 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 208000014155 speech-language disorder-1 Diseases 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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Abstract
本发明涉及适用于制备白光LED的荧光粉，特别是一种基于近紫外光激发的单一相白光荧光粉及其制备方法，其化学式为：Sr5-m-nZnn(SiO4)2Cl2:Eu2+ m，其中，0.10≤m≤0.15；0≤n≤0.20，在360-410nm近紫外光激发下发射出单一相白光。是以SiO2，Eu2O3，SrCO3，ZnO，SrCl2.6H2O作原料，混合研磨后在1000℃-1200℃温度下培烧3-5小时，自然冷却后研磨，即得本发明单一相白光荧光粉。可与近紫外光管芯组合制备白光LED，以克服目前红、绿、蓝三基色混合荧光粉因存在的再吸收和配比调控问题而影响流明效率和色彩还原性能的缺陷。The present invention relates to a phosphor suitable for preparing white light LEDs, in particular to a single-phase white light phosphor excited by near-ultraviolet light and a preparation method thereof, the chemical formula of which is: Sr 5-mn Zn n (SiO 4 ) 2 Cl 2 : Eu 2+ m , wherein, 0.10≤m≤0.15; 0≤n≤0.20, emits single-phase white light under the excitation of 360-410nm near-ultraviolet light. SiO 2 , Eu 2 O 3 , SrCO 3 , ZnO, SrCl 2 .6H 2 O are used as raw materials, mixed and ground, then fired at 1000°C-1200°C for 3-5 hours, cooled naturally and then ground to obtain this product Invention of single-phase white light phosphor. It can be combined with near-ultraviolet tube cores to prepare white LEDs to overcome the defects of the current red, green and blue primary color mixed phosphors that affect lumen efficiency and color reproduction performance due to the problems of reabsorption and ratio control.
Description
Technical field
The present invention relates to be applicable to the fluorescent material of preparation white light LEDs, particularly relate to a kind of under near ultraviolet excitation and launch fluorescent material of single-phase white and preparation method thereof.
Background technology
The successful research and development of high brightness GaN blue LED and the white light LEDs of realizing thus are described as the Edison that continues and have invented maximum light source revolution since the incandescent light.Compare with traditional incandescent light, luminescent lamp, White-light LED illumination is energy-efficient owing to having, the life-span long, do not have advantages such as (Hg, Pb) pollutes, WV is low, not fragile receives much concern.The LED industry increases progressively with the speed more than 20% every year in recent years.
Blue (purple) light LED phosphor combination is the important channel of realizing white light LEDs.At present; White light LEDs practical on the market is the rear-earth-doped YAG:Ce gold-tinted fluorescent material of blue light tube core excitation, because the blue light of LED is participated in the synthetic of white light directly, so the glow color of device changes with the coat-thickness and the driving voltage of fluorescent material; Color rendition power is relatively poor, and colour rendering index is on the low side.For addressing the above problem, adopt near-ultraviolet light (370-410nm) tube core to excite three primary colors fluorescent powder to realize that white light LEDs becomes the focus of research and development.Because human eye is insensitive to near-ultraviolet light, this method realizes the color of white light LEDs only by the three primary colors fluorescent powder decision, so color stable, and reproduction power is strong, and colour rendering index is high, is the direction of white light LEDs development.
Reported single-phase white-emitting phosphor has: 2004, its composition of Korean's development was respectively Sr
3MgSi
2O
8: Eu
2+And Sr
3MgSi
2O
8: Eu
2+, Mn
2+Two kinds of single-phase white-emitting phosphors (JongSu Kim, Pyung Eun Jeon, Yun Hyung Park, Jun chul Choi; And Hong LeeParka, Gwang Chul Kim, Tae Whan Kim, Appl.Phys.Lett. Applied Physics wall bulletin; 85 volume (17) phases, 3696 pages, 2004).2006, Changchun Institute of Optics, Fine Mechanics and Physics, CAS development consist of Eu
XySr
Y-xyMgSi
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, publication number CN1850940A).
Summary of the invention
The objective of the invention is to propose a kind of single-phase white-emitting phosphor based near ultraviolet excitation; This fluorescent material sends single-phase white under near ultraviolet excitation; Can with near-ultraviolet light tube core combined preparation white light LEDs, regulate and control the defective that problem influences luminous efficiency and color rendition performance to overcome present red, green, blue three primary colours mixed fluorescent powder because of absorbing again of existing with proportioning.
The present invention is based on the single-phase white-emitting phosphor of near ultraviolet excitation, is the compound with following chemical formula: Sr
5-m-nZn
n(SiO
4)
2Cl
2: Eu
2+ m, wherein, 0.10≤m≤0.15; 0≤n≤0.20.
Said x, y preferred value are: m=0.12, n=0.10; M=0.15, n=0.10.
Because rare earth ion Eu
2+The d electronic energy level structure receive matrix and lattice site environmental influence very big, just can regulate and control different cases through the adjustment matrix components than, activator concentration, regulate and control different luminescent spectrum distributions.Fluorescent material of the present invention is launched single-phase white under the 360-410nm near ultraviolet excitation.
The preparation method of fluorescent material of the present invention may further comprise the steps:
A. with SiO
2, Eu
2O
3, SrCO
3, ZnO, 8rCl
2.6H
2O makes raw material, takes by weighing above-mentioned each raw material by the stoichiometric ratio of each material in the above-mentioned chemical formula, carries out ground and mixed;
B. above-mentioned compound is inserted in the corundum crucible, at CO or H
2Roast under the reducing atmosphere, roast temperature are that the roast time is 3 one 5 hours in 1000 ℃ one 1200 ℃, grind behind the naturally cooling and promptly get said single-phase white-emitting phosphor.
Because SrCl
2.6H
2The fusing point of O lower (873 ℃) is prone to scaling loss when roast, so SrCl in the said mixing raw material of step a
2.6H
2The proportional quantity of O is for the 110%-120% by the stoichiometric ratio calculated amount, to compensate its scaling loss in roast.
Single-phase white-emitting phosphor of the present invention; Under the 360-410nm near ultraviolet excitation, launch single-phase white; With near-ultraviolet light tube core combined preparation white light LEDs; Overcome three primary colors fluorescent powder and weakened problem, also avoided the red, green, blue three primary colours to absorb problem again because of irregular colour weighing apparatus, the luminous intensity that heterogeneous mixing produces.
Description of drawings
Fig. 1 is single-phase white-emitting phosphor Sr of the present invention
4.75Zn
0.10(SiO
4)
2Cl
2: Eu
2+ 0.15Emmission spectrum (λ
Ex=400nm) with the exciting light spectrogram;
Fig. 2 is single-phase white-emitting phosphor Sr of the present invention
4.78Zn
0.10(SiO
4)
2Cl
2: Eu
2+ 0.12Emmission spectrum (λ
Ex=400nm) with the exciting light spectrogram.
Embodiment
Through following examples the present invention is done further explain.
Use spectroscopically pure SiO
2, the pure Eu of top grade
2O
3, analytical pure SrCO
3, ZnO, SrCl
2.6H
2O makes raw material, prepares fluorescent material of the present invention.
Embodiment 1
Preparation Sr
4.90(SiO
4)
2Cl
2.0: Eu
2+ 0.10(promptly work as Sr
5-m-nZn
n(SiO
4)
2Cl
2: Eu
2+ mMiddle m=0.10 is during n=0.00) fluorescent material.
Take by weighing SrCO by stoichiometric ratio
32.8782 gram, SrCl
2.6H
2O1.5972 gram (because SrCl
2.6H
2O fusing point lower (873 ℃) is by calculated amount excessive 20%), SiO
20.6008 gram, Eu
2O
30.0880 gram is put into the agate mortar mixed grinding; Put into corundum crucible, add a cover, place in the High Temperature Furnaces Heating Apparatus, at CO or H
2Under the reducing atmosphere, under 1100-1200 ℃ of temperature roast 3-5 hour; Grind behind the naturally cooling, promptly obtaining chemical formula is Sr
4.90(SiO
4)
2Cl
2.0: Eu
0.10Single-phase white-emitting phosphor.Its chromaticity coordinates is x=0.3262, y=0.4386; Colour temperature is T
C=5710K; Colour rendering index is Ra=56.0.
Preparation Sr
4.70Zn
0.20(SiO
4)
2Cl
2: Eu
0.10 2+(promptly work as Sr
5-m-nZn
n(SiO
4)
2Cl
2: Eu
2+ mMiddle m=0.10 is during n=0.20) fluorescent material.
Take by weighing SrCO by stoichiometric ratio
32.7306 gram, SrCl
2.6H
2O1.4641 gram (by calculated amount excessive 10%), ZnO0.0814, SiO
20.6008 gram, Eu
2O
30.0880 gram is put into the agate mortar mixed grinding; Put into corundum crucible, add a cover, place in the High Temperature Furnaces Heating Apparatus, at CO or H
2Under the reducing atmosphere, under 1100-1200 ℃ of temperature roast 3-5 hour; Grind behind the naturally cooling, promptly obtaining chemical formula is Sr
4.70Zn
0.20(SiO
4)
2Cl
2: Eu
0.10 2+Single-phase white-emitting phosphor.Its chromaticity coordinates is x=0.3293, y=0.4061; Colour temperature is T
C=5829K; Colour rendering index is Ra=64.0.。
Embodiment 3
Preparation Sr
4.88(SiO
4)
2Cl
2.:Eu
2+ 0.12(promptly work as Sr
5-m-nZn
n(SiO
4)
2Cl
2: Eu
2+ mMiddle m=0.12 is during n=0.00) fluorescent material.
Take by weighing SrCO by stoichiometric ratio
32.8634 gram, SrCl
2.6H
2O1.5972 gram (by calculated amount excessive 20%), SiO
20.6008 gram, Eu
2O
30.1056 gram is put into the agate mortar mixed grinding; Put into corundum crucible, add a cover, place in the High Temperature Furnaces Heating Apparatus, at CO or H
2Under the reducing atmosphere, under 1100-1200 ℃ of temperature roast 3-5 hour; Grind behind the naturally cooling, promptly obtaining chemical formula is Sr
4.88(SiO
4)
2Cl
2.:Eu
2+ 0.12Single-phase white-emitting phosphor.Its chromaticity coordinates is x=0.3370, y=0.4074; Colour temperature is T
C=6067K; Colour rendering index is Ra=61.7.
Embodiment 4
Preparation Sr
4.78Zn
0.10(SiO
4)
2Cl
2: Eu
2+ 0.12(promptly work as Sr
5-m-nZn
n(SiO
4)
2Cl
2: Eu
2+ mMiddle m=0.12 is during n=0.10) fluorescent material.
Take by weighing SrCO by stoichiometric ratio
32.7896, SrCl
2.6H
2O1.4641 gram (by calculated amount excessive 10%), SiO
20.6008 gram, ZnO0.0407, Eu
2O
30.1056 gram is put into the agate mortar thorough mixing and is ground; Put into corundum crucible, add a cover, place in the High Temperature Furnaces Heating Apparatus, at CO or H
2Under the reducing atmosphere, under 1000-1200 ℃ of temperature roast 3-5 hour; Naturally grind cold back, and promptly obtaining chemical formula is Sr
4.78Zn
0.10(SiO
4)
2Cl
2: Eu
2+ 0.12Single-phase white-emitting phosphor.
As shown in Figure 2, be this Sr
4.78Zn
0.12(SiO
4)
2Cl
2: Eu
0.10 2+Emmission spectrum (the λ of fluorescent material
Ex=400nm) and excitation spectrum (λ
Em=445nm; λ
Em=548nm).Its chromaticity coordinates is x=0.3268, y=0.3866; Colour temperature is T
C=5837K; Colour rendering index is Ra=66.6
Embodiment 5
Preparation Sr
4.85(SiO
4)
2Cl
2: Eu
2+ 0.15(promptly work as Sr
5-m-nZn
n(SiO
4)
2Cl
2: Eu
2+ mMiddle m=0.15 is during n=0.00) fluorescent material.
Take by weighing SrCO by stoichiometric ratio
32.8413 gram, SrCl
2.6H
2O1.5972 gram (by calculated amount excessive 20%), SiO
20.6008 gram, Eu
2O
30.1320 gram is put into the agate mortar mixed grinding; Put into corundum crucible, add a cover, place in the High Temperature Furnaces Heating Apparatus, at CO or H
2Under the reducing atmosphere, under 1000-1200 ℃ of temperature roast 3-5 hour; Grind behind the naturally cooling, promptly obtaining chemical formula is Sr
4.85(SiO
4)
2Cl
2.0: Eu
2+ 0.15Single-phase white-emitting phosphor.Its chromaticity coordinates is x=0.3101, y=0.4041; Colour temperature is T
C=6315K; Colour rendering index is Ra=60.0.
Embodiment 6
Preparation Sr
4.75Zn
0.10(SiO
4)
2Cl
2: Eu
2+ 0.15(promptly work as Sr
5-m-nZn
n(SiO
4)
2Cl
2: Eu
2+ mMiddle m=0.15 is during n=0.10) fluorescent material.
Take by weighing SrCO by stoichiometric ratio
32.7675 gram, SrCl
2.6H
2O1.4641 gram (by calculated amount excessive 10%), SiO
20.6008 gram, ZnO0.0407, Eu
2O
30.1320 gram is put into the agate mortar mixed grinding; Put into corundum crucible, add a cover. place in the High Temperature Furnaces Heating Apparatus, at CO or H
2Under the reducing atmosphere, under 1000-1200 ℃ of temperature roast 3-5 hour; Grind behind the naturally cooling, promptly obtaining chemical formula is Sr
4.75Zn
0.10(SiO
4)
2Cl
2: Eu
2+ 0.15Single-phase white-emitting phosphor.
As shown in Figure 1, be this Sr
4.75Zn
0.10(SiO
4)
2Cl
2: Eu
2+ 0.15Emmission spectrum (the λ of fluorescent material
Ex=400nm) and excitation spectrum (λ
Em=445nm; λ
Em=546nm), its chromaticity coordinates is x=0.3146, y=0.3747; Colour temperature is T
C=6265K; Colour rendering index is Ra=69.6.
More than the excitation spectrum of the prepared fluorescent material of each embodiment show, be effectively in the 360-410nm ultraviolet region and excite; Emmission spectrum shows that blue-light-emitting band and yellow-green colour luminous zone can synthesize white lights.
Claims (4)
1. the single-phase white-emitting phosphor based near ultraviolet excitation is characterized in that the chemical formula of said fluorescent material is: Sr
5-m-nZn
n(SiO
4)
2Cl
2: Eu
2+M, wherein, 0.10≤m≤0.15; 0≤n≤0.20.
2. the single-phase white-emitting phosphor based near ultraviolet excitation according to claim 1 is characterized in that mole number m, the n in the said chemical formula is: m=0.12, n=0.10.
3. the single-phase white-emitting phosphor based near ultraviolet excitation according to claim 1 is characterized in that mole number m, the n in the said chemical formula is: m=0.15, n=0.10.
4. the preparation method of the said white emitting fluorescent powder of claim 1 is characterized in that may further comprise the steps:
A. with SiO
2, Eu
2O
3, SrCO
3, ZnO, SrCl
2.6H
2O makes raw material, takes by weighing above-mentioned each raw material, wherein said SrCl by the stoichiometric ratio of each material in the said chemical formula of claim 1
2.6H
2The proportional quantity of O to compensate its scaling loss in roasting, carries out ground and mixed for the 110%-120% by the stoichiometric ratio calculated amount;
B. above-mentioned compound is inserted in the corundum crucible, at CO or H
2Roasting under the reducing atmosphere, maturing temperature are 1000 ℃-1200 ℃, and roasting time is 3-5 hour, grind behind the naturally cooling and promptly get said single-phase white-emitting phosphor.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1539919A (en) * | 2003-06-18 | 2004-10-27 | 北京有色金属研究总院 | Luminscent-powder in use for LED of white light, preparing method and electric light source produced |
| CN1850940A (en) * | 2005-04-22 | 2006-10-25 | 中国科学院长春光学精密机械与物理研究所 | Single-phase whitelight fluorescent powder for ultraviolet light excitation |
| CN1995277A (en) * | 2006-12-21 | 2007-07-11 | 温州大学 | Single component white light fluorescent powder for LED lamp and its preparation method |
| CN101173171A (en) * | 2007-11-15 | 2008-05-07 | 上海交通大学 | Preparation method of single-phase white light phosphor excited by ultraviolet light |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1539919A (en) * | 2003-06-18 | 2004-10-27 | 北京有色金属研究总院 | Luminscent-powder in use for LED of white light, preparing method and electric light source produced |
| CN1850940A (en) * | 2005-04-22 | 2006-10-25 | 中国科学院长春光学精密机械与物理研究所 | Single-phase whitelight fluorescent powder for ultraviolet light excitation |
| CN1995277A (en) * | 2006-12-21 | 2007-07-11 | 温州大学 | Single component white light fluorescent powder for LED lamp and its preparation method |
| CN101173171A (en) * | 2007-11-15 | 2008-05-07 | 上海交通大学 | Preparation method of single-phase white light phosphor excited by ultraviolet light |
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