CN100404639C - Single-phase whitelight fluorescent powder for ultraviolet light excitation - Google Patents

Single-phase whitelight fluorescent powder for ultraviolet light excitation Download PDF

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CN100404639C
CN100404639C CNB2005100167439A CN200510016743A CN100404639C CN 100404639 C CN100404639 C CN 100404639C CN B2005100167439 A CNB2005100167439 A CN B2005100167439A CN 200510016743 A CN200510016743 A CN 200510016743A CN 100404639 C CN100404639 C CN 100404639C
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fluorescent powder
phase white
white light
mgsi
single phase
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CN1850940A (en
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张家骅
孙晓园
王笑军
张霞
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Changchun Institute of Optics Fine Mechanics and Physics of CAS
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Changchun Institute of Optics Fine Mechanics and Physics of CAS
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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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Abstract

The present invention relates to the technical field of light emission, particularly to a single phase white light fluorescent powder suitable for ultraviolet light excitation and a manufacture method. The expression formula of the single phase white light fluorescent powder is Eu<xy>Sr<y-xy>MgSizO<2z+y+1>, wherein x is more than zero and is no more than 0.1; y is no less than two and is less than three; z is more than zero and is less than two. Raw material is fully and evenly ground and mixed, is arranged in a high purity corundum crucible or a platinum crucible and is arranged in a high-temperature furnace. Then, after heated within temperature of 1100 to 1400 DEG C and under the condition of carbon or hydrogen gas deoxidization for three to five hours, the single phase white light fluorescent powder is taken out and obtained. The present invention achieves the single phase white light fluorescent powder suitable for excitation of ultraviolet light of 250 to 450 nm by utilizing the characteristic of bivalent rare earth Eu<2+> that a d electron energy level structure is greatly influenced by a matrix and a check bit environment. The present invention is used for the new generation of white light LED illumination and the existing fluorescent lamp illumination.

Description

A kind of single-phase white-emitting phosphor and preparation method who is suitable for ultraviolet excitation
Technical field
The invention belongs to the luminescence technology field, relate to the single phase emitting phosphor that is applicable to that UV-light (250-450nm) excites, specifically a kind of single-phase white-emitting phosphor and preparation method who is suitable for ultraviolet excitation.
Background technology
1993, Japanese Ri Ya chemical company acquisition of technology broke through, and successfully develops blue light GaN photodiode (LED), for the arrival in semiconductor solid lighting epoch brings dawn.Semiconductor lighting is compared with incandescent osram lamp and luminescent lamp, have nontoxic, overlong service life (100,000 hours), energy-efficient, all solid state, plurality of advantages such as operating voltage is low, shock resistance and security are good, will become the new light sources that 21 century substitutes the traditional lighting utensil.1997, Ri Ya chemical company utilized the rear-earth-doped YAG:Ce of blue light tube core pumping 3+Gold-tinted fluorescent material is developed white light LEDs and is also put goods on the market very soon.Because white light is to be formed by the yellow fluorescence of fluorescent material and the blue light of LED, the glow color of device changes with driving voltage and fluorescent coating variation in thickness, and color reducibility is poor, and colour rendering index is low.For addressing the above problem, adopt near-ultraviolet light (370-410nm) InGaN tube core to excite three primary colors fluorescent powder to realize that the research and development of white light LEDs become at present one of focus of these field research and development in the world.Because vision is to the insensitivity of near-ultraviolet light, the color of this class white light LEDs is only by the fluorescent material decision, therefore, colour stable, color reducibility and colour rendering index height are considered to the leading of White-light LED illumination of new generation.
At present, the white emitting fluorescent powder that is complementary with the near-ultraviolet light tube core lacks, and luminescent properties is undesirable, and this white emitting fluorescent powder generally adopts the way of mixing three kinds of primary colours fluorescent material of red, green, blue to make.Because exist color to absorb and proportioning regulation and control problem between the mixture, luminous efficiency and color rendition performance are a greater impact again, therefore, the development single-phase white-emitting phosphor has crucial meaning.
The end of the year 2004, the Korea S researchist has reported two kinds of single-phase white-emitting phosphor (Jong Su Kim, Pyung Eun Jeon, Yun Hyung Park of being suitable near ultraviolet excitation, Jun Chul Choi, and Hong Lee Parka, Gwang Chul Kim, Tae Whan Kim, Appl.Phys.Lett. Applied Physics wall bulletin, 85 volume (17) phases, 3696 pages, 2004.), its composition is respectively Sr 3MgSi 2O 8: Eu 2-And Sr 3MgSi 2O 8: Eu 2+, Mn 2+
Summary of the invention
The invention reside in and utilize bivalent rare earth Eu 2+The d electronic energy level structure be subjected to matrix and the big characteristics of case environmental influence, by adjusting the matrix components ratio, regulate and control the distribution of different cases, thereby the regulation and control spectrographic distributes, purpose provides a kind of single-phase white-emitting phosphor and preparation method who is suitable for ultraviolet excitation.
Key content of the present invention is, provided a kind of compositing range that is suitable for the single-phase white-emitting phosphor of ultraviolet excitation, but tabular form is: Eu XySr Y-xyMgSi zO 2z+y+1, wherein x, y, z are mole number, span: 0＜x≤0.1; 2≤y＜3; 0＜z＜2.The fluorescent material of above-mentioned composition excites down at UV-light 250-450nm, has white light emission.
In the single-phase white-emitting phosphor preparation of the present invention, used raw material is respectively Eu 2O 3, SrCO 3, MgO and SiO 2In preparation process, press tabular form Eu XySr Y-xyMgSi zO 2z+y+1Composition, calculate and to take by weighing raw material.Above-mentioned raw materials fully ground be mixed evenly, insert in high-purity corundum crucible or the platinum crucible, put into High Temperature Furnaces Heating Apparatus.In 1100 ℃ of-1400 ℃ of temperature, under carbon or hydrogen reducing condition, heat after 3-5 hour, take out and obtain single-phase white-emitting phosphor Eu XySr Y-xyMgSi zO 2z+y+1
Characteristics of the present invention are that the material that is different from international report is formed, and has provided a kind of compositing range that is suitable for the single-phase white-emitting phosphor of ultraviolet excitation, have bigger selection and adjust leeway.Choose x=0.01; Y=2; Z=1; Prepared Eu 0.02Sr 1.98MgSi 1O 5, single-phase white-emitting phosphor has obtained chromaticity coordinates and is: x=0.32; Y=0.33; Colour rendering index is greater than 85% good result.Fig. 1 has provided the emission and the excitation spectrum of single-phase white-emitting phosphor.Emmission spectrum is made up of a blue-light-emitting band and a Yellow luminous band, and they are from the Eu that is on the different cases 2+Ion is mixed into the white light that is near the mark; Excitation spectrum shows, excites in the 250-450nm scope of ultraviolet region effectively.
Description of drawings
Fig. 1 is under the 400nm ultraviolet excitation, emmission spectrum of the present invention and excitation spectrum.The strong emission at 400nm place is from excitation light source LED.Emmission spectrum shows that chromaticity coordinates (CIE) is: x=0.32; Y=0.33; Colour rendering index (CRI) is 86%, is better than the white light LEDs of present commercialization.Excitation spectrum shows, excites in the 250-450nm scope of ultraviolet region effectively.
Embodiment
Embodiment 1: preparation Eu XySr Y-xyMgSi zO 2z+y+1, x=0.01 wherein; Y=2; Z=0.5, concrete expression is: Eu 0.02Sr 1.98MgSi 0.5O 4Press x=0.01; Y=2; Z=0.5 calculates and takes by weighing raw material, takes by weighing 3.52g Eu 2O 3, 292.2g SrCO 3, 40.3g MgO and 30g SiO 2, they are mixed.With above-mentioned raw materials fully grind be mixed even after, insert in high-purity corundum crucible or the platinum crucible, put into High Temperature Furnaces Heating Apparatus; In 1100 ℃ of-1400 ℃ of temperature and under carbon or the hydrogen reducing condition, heat after 3-5 hour, take out and obtain having single-phase white-emitting phosphor: Eu 0.02Sr 1.98MgSi 0.5O 4
Embodiment 2: preparation Eu XySr Y-xyMgSi zO 2z+y+1, x=0.05 wherein, y=2, z=0.5, concrete expression is: Eu 0.1Sr 2-0.1MgSi 0.5O 4Press x=0.05, y=2, z=0.5 calculates and takes by weighing raw material, takes by weighing 17.6g Eu 2O 3, 280.44g SrCO 3, 40.3g MgO and 30g SiO 2, they are mixed.With above-mentioned raw materials fully grind be mixed even after, insert in high-purity corundum crucible or the platinum crucible, put into High Temperature Furnaces Heating Apparatus; In 1100 ℃ of-1400 ℃ of temperature and under carbon or the hydrogen reducing condition, heat after 3-5 hour, take out and obtain having single-phase white-emitting phosphor Eu 0.1Sr 2-0.1MgSi 0.5O 4
Embodiment 3: preparation Eu XySr Y-xyMgSi zO 2z+y+1, x=0.01 wherein, y=2.8, z=0.5, concrete expression is: Eu 0.028Sr 2.8-0.028MgSi 0.5O 4.8Press x=0.01, y=2.8, z=0.5 calculates and takes by weighing raw material, takes by weighing 4.928g Eu 2O 3, 409.15g SrCO 3, 40.3g MgO and 30g SiO 2, they are mixed.With above-mentioned raw materials fully grind be mixed even after, insert in high-purity corundum crucible or the platinum crucible, put into High Temperature Furnaces Heating Apparatus; In 1100 ℃ of-1400 ℃ of temperature and under carbon or the hydrogen reducing condition, heat after 3-5 hour, take out and obtain having single-phase white-emitting phosphor Eu 0.028Sr 2.8-0.028MgSi 0.5O 4.8
Embodiment 4: preparation Eu XySr Y-xyMgSi zO 2z+y+1, x=0.05 wherein, y=2.8, z=0.5, concrete expression is: Eu 0.14Sr 2.8-0.14MgSi 0.5O 4.8Press x=0.05, y=2.8, z=0.5 calculates and takes by weighing raw material, takes by weighing 24.64g Eu 2O 3, 392.6g SrCO 3, 40.3g MgO and 30g SiO 2, they are mixed.With above-mentioned raw materials fully grind be mixed even after, insert in high-purity corundum crucible or the platinum crucible, put into High Temperature Furnaces Heating Apparatus; In 1100 ℃ of-1400 ℃ of temperature and under carbon or the hydrogen reducing condition, heat after 3-5 hour, take out and obtain having single-phase white-emitting phosphor Eu 0.14Sr 2.8-0.14MgSi 0.5O 1.8
Embodiment 5: preparation Eu XySr Y-xyMgSi zO 2z+y+1, x=0.01 wherein, y=2, z=1.5, concrete expression is: Eu 0.02Sr 2-0.02MgSi 1.5O 6Press x=0.01, y=2, z=1.5 calculates and takes by weighing former section, takes by weighing 3.52g Eu 2O 3, 292.2g SrCO 3, 40.3g MgO and 90g SiO 2, they are mixed.With above-mentioned raw materials fully grind be mixed even after, insert in high-purity corundum crucible or the platinum crucible, put into High Temperature Furnaces Heating Apparatus; In 1100 ℃ of-1400 ℃ of temperature and under carbon or the hydrogen reducing condition, heat after 3-5 hour, take out and obtain having single-phase white-emitting phosphor Eu 0.02Sr 2-0.02MgSi 1.5O 6
Embodiment 6: preparation Eu XySr Y-xyMgSi zO 2z+y+1, x=0.05 wherein, y=2, z=1.5, concrete expression is: Eu 0.1Sr 2-0.1MgSi 1.5O 6Press x=0.05, y=2, z=1.5 calculates and takes by weighing raw material, takes by weighing 17.6g Eu 2O 3, 280.44g SrCO 3, 40.3g MgO and 90g SiO 2, they are mixed.With above-mentioned raw materials fully grind be mixed even after, insert in high-purity corundum crucible or the platinum crucible, put into High Temperature Furnaces Heating Apparatus; In 1100 ℃ of-1400 ℃ of temperature and under carbon or the hydrogen reducing condition, heat after 3-5 hour, take out and obtain having single-phase white-emitting phosphor: Eu 0.1Sr 2-0.1MgSi 1.5O 6
Embodiment 7: preparation Eu XySr Y-xyMgSi zO 2z+y+1, x=0.01 wherein, y=2.8, z=1.5, concrete expression is: Eu 0.028Sr 2.8-0.028MgSi 1.5O 6.8Press x=0.01, y=2.8, z=1.5 calculates and takes by weighing raw material, takes by weighing 4.928g Eu 2O 3, 409.15g SrCO 3, 40.3g MgO and 90g SiO 2, they are mixed.With above-mentioned raw materials fully grind be mixed even after, insert in high-purity corundum crucible or the platinum crucible, put into High Temperature Furnaces Heating Apparatus; In 1100 ℃ of-1400 ℃ of temperature and under carbon or the hydrogen reducing condition, heat after 3-5 hour, take out and obtain having single-phase white-emitting phosphor Eu 0.028Sr 2.8-0.028MgSi 1.5O 6.8
Embodiment 8: preparation Eu XySr Y-xyMgSi zO 2z+y+1, x=0.05 wherein, y=2.8, z=1.5, concrete expression is: Eu 0.14Sr 2.8-0.14MgSi 1.5O 6.8Press x=0.05, y=2.8, z=1.5 calculates and takes by weighing raw material, takes by weighing 24.64g Eu 2O 3, 392.6g SrCO 3, 40.3g MgO and 90g SiO 2, they are mixed.With above-mentioned raw materials fully grind be mixed even after, insert in high-purity corundum crucible or the platinum crucible, put into High Temperature Furnaces Heating Apparatus; In 1100 ℃ of-1400 ℃ of temperature and under carbon or the hydrogen reducing condition, heat after 3-5 hour, take out and obtain having single-phase white-emitting phosphor Eu 0.14Sr 2.8-0.14MgSi 1.5O 6.8

Claims (9)

1. a single-phase white-emitting phosphor that is suitable for ultraviolet excitation is characterized in that expression is: Eu XySr Y-xyMgSi zO 2z+y+1Wherein x, y, z are mole number, span: 0＜x≤0.1; 2≤y＜3; 0＜z＜2.
2. the single-phase white-emitting phosphor that is suitable for ultraviolet excitation according to claim 1 is characterized in that exciting down at UV-light 250-450nm, has white light emission.
3. the single-phase white-emitting phosphor that is suitable for ultraviolet excitation according to claim 1 is characterized in that mole number x, y, z are: x=0.01; Y=2; Z=0.5.
4. the single-phase white-emitting phosphor that is suitable for ultraviolet excitation according to claim 1 is characterized in that mole number x, y, z are: x=0.05, y=2, z=0.5.
5. the single-phase white-emitting phosphor that is suitable for ultraviolet excitation according to claim 1 is characterized in that mole number x, y, z are: x=0.01, y=2, z=1.5.
6. the single-phase white-emitting phosphor that is suitable for ultraviolet excitation according to claim 1 is characterized in that mole number x, y, z are: x=0.05, y=2.8, z=0.5.
7. the single-phase white-emitting phosphor that is suitable for ultraviolet excitation according to claim 1 is characterized in that mole number x, y, z are: x=0.01, y=2, z=1.5.
8. the single-phase white-emitting phosphor that is suitable for ultraviolet excitation according to claim 1 is characterized in that mole number x, y, z are: x=0.05, y=2, z=1.5.
9. the single-phase white-emitting phosphor that is suitable for ultraviolet excitation according to claim 1 is characterized in that mole number x, y, z are: x=0.01, y=2.8, z=1.5.
CNB2005100167439A 2005-04-22 2005-04-22 Single-phase whitelight fluorescent powder for ultraviolet light excitation Expired - Fee Related CN100404639C (en)

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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101070470B (en) * 2007-03-22 2011-04-06 罗维鸿 WLED and its inorganic fluorescent powder
CN101565620B (en) * 2009-06-05 2012-04-11 中国科学院长春光学精密机械与物理研究所 Single-phase white-emitting phosphor based on near ultraviolet excitation and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
White-light generation through ultraviolet-emitting diode andwhite-emitting phosphor. Kim JS, Jeon PE, Park YH, et al.APPLIED PHYSICS LETTERS,Vol.85 No.17. 2004
White-light generation through ultraviolet-emitting diode andwhite-emitting phosphor. Kim JS, Jeon PE, Park YH, et al.APPLIED PHYSICS LETTERS,Vol.85 No.17. 2004 *

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