CN102352248A - Fluorescent powder for white light-emitting diodes (LEDs) and backlight LEDs - Google Patents
Fluorescent powder for white light-emitting diodes (LEDs) and backlight LEDs Download PDFInfo
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- CN102352248A CN102352248A CN2011102775307A CN201110277530A CN102352248A CN 102352248 A CN102352248 A CN 102352248A CN 2011102775307 A CN2011102775307 A CN 2011102775307A CN 201110277530 A CN201110277530 A CN 201110277530A CN 102352248 A CN102352248 A CN 102352248A
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- fluorescent material
- fluorescent powder
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
The invention belongs to the technical field of light-emitting diode (LED) light source and in particular relates to fluorescent powder for white LEDs and backlight LEDs. The chemical structural formula of the fluorescent powder is RE1xCexM2AlO5, wherein M is one or more of alkaline-earth metals; RE is one or more of La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm and Lu in rare-earth elements; and x is more than or equal to 0.001 and less than 1. During preparation, nitrates of various elements serve as original reactants; NH4X, BaX2, SrX2, boric acid or borate serves as a cosolvent; a liquid phase method is adopted; the materials are burned at high temperature in air and then are reduced in reducing atmosphere; the prepared fluorescent powder has higher brightness and stability and a more complete crystal form. During preparation, oxalate and ammonia water serve as precipitating agents, so that the elements RE, Ce, Al and M in the structural formula are precipitated completely, and the phase purity of the fluorescent powder can be improved. The fluorescent powder can be used for preparing the white LEDs and the backlight LEDs.
Description
Technical field
The invention belongs to the led light source technical field, be specifically related to the fluorescent material that a kind of LED device is used.
Background technology
The LED technology is a kind of efficient light-emitting device that electric energy is converted into luminous energy.It has incandescent light and common compact type fluorescent material incomparable advantage, and nontoxic, the life-span is long, and thermal value is low.Volume is little, and operating voltage is low, plurality of advantages such as good and environmental protection of safety performance.Gram is widely used in lighting field and display backlight source.
Present LED white-light emitting technology mainly is to utilize the YAG that can absorb the blue light that LED sends and produce gold-tinted to realize.But the white light that this kind method obtains, colour temperature are too high, and color developing is low, and brightness simultaneously is also lower.Therefore seek efficient stable and the good fluorescent material of color developing has crucial meaning.
Summary of the invention
The objective of the invention is the deficiency to existing fluorescent material, provide a kind of luminous efficiency is high, color developing is good white light and backlight LED with fluorescent material and preparation method thereof.
White light provided by the invention and backlight LED fluorescent material, its chemical structural formula is: RE1
xCe
xM
2AlO
5, wherein, M is a kind of in the alkaline-earth metal or wherein several, RE is the La in the rare earth element, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, a kind of among the Lu or wherein several, 0. 001≤x＜1.
Above-mentioned white light that the present invention proposes and backlight LED be with the preparation method of fluorescent material, according to each atoms of elements ratio in the above-mentioned chemical structural formula, take by weighing each element (comprise alkaline-earth metal M, rare earth elements RE, Al, nitrate Ce) is as the primitive reaction thing, with NH
4X, BaX
2, SrX
2, in boric acid or the borate one or more are as solubility promoter, X is one or more in the halogen, the consumption of solubility promoter is 0.01-20 ﹪ of primitive reaction thing gross weight; During preparation,, be dissolved in the distilled water, mix, be heated to 50-70 degrees centigrade, stirred 50-80 minutes at first with the nitrate of the corresponding weight of each element; Add oxalic acid again, stirred 50-80 minutes; Add ammoniacal liquor again, stirred 20-40 minutes, filter; 900-1000 degrees centigrade of constant temperature calcinations 5-8 hours in box-type furnace then; Fragmentation, the crucible of packing into, constant temperature calcination 5--8 hour in 1000-1400 degrees centigrade of reducing atmospheres again, fragmentation, ball milling, washing 100-120 degrees centigrade of dryings 5-10 hours, is crossed 200 orders then and is shone net, obtains said fluorescent material.
The fluorescent material of the present invention's preparation is encapsulated among the LED, can be made into white light LEDs, or be made into backlight LED.
Advantage of the present invention:
(1) the present invention adopts liquid phase method, makes the light emitting ionic more even distribution of fluorescent material.
(2) the present invention adopts in the first air high temperature sintering reductive two-step preparation then, makes the fluorescent material that makes have higher brightness, higher stability, more complete crystal formation.
(3) the present invention uses oxalate and ammoniacal liquor to do precipitation agent, makes corresponding M and RE in the molecular formula, and Ce element deposition is more thorough, improves the phase purity of fluorescent material.
The inventive method technology is simple, and is pollution-free, and synthesis temperature is low, easy handling.
Description of drawings
Fig. 1 is the fluorescent material emmission spectrum figure of embodiment 1.
Embodiment
The invention is further illustrated by the following examples.
Embodiment 1 takes by weighing 0.90 mole of La (NO
3)
3, be dissolved in 1000 ml distilled waters, 0.1 mole Ce (NO
3)
3, 2 moles Sr (NO
3)
2, 1 mole Al (NO
3)
3, stirred 60 minutes.The oxalic acid that adds 1.0 moles stirred 60 minutes, added 100 milliliters of ammoniacal liquor, stirred 30 minutes, added 0.001 mole of BaF
2Solubility promoter filters.1000 degrees centigrade of constant temperature is 6 hours in box-type furnace, fragmentation, the crucible of packing into, and then in 1300 degree degree centigrade reducing atmospheres constant temperature 6 hours, fragmentation, ball milling, washing in 120 degrees centigrade of dry 5-10 hours, is crossed 200 orders and is shone net, obtains said fluorescent material.
Embodiment 2 takes by weighing 0.95 mole of Y (NO
3)
3, be dissolved in 1000 ml distilled waters, 0.1 mole Ce (NO
3)
3, 2 moles Ba (NO
3)
2, 1 mole Al (NO3) 3 stirred 60 minutes.The oxalic acid that adds 1.0 moles stirred 60 minutes, added 100 milliliters of ammoniacal liquor, stirred 30 minutes, added 0.001 mole of SrF
2Solubility promoter filters.1000 degrees centigrade of constant temperature is 6 hours in box-type furnace, fragmentation, the crucible of packing into, and then in 1300 degree degree centigrade reducing atmospheres constant temperature 6 hours, fragmentation, ball milling, washing, 120 degrees centigrade of dryings 10 hours are crossed 200 orders and are shone net, obtain said fluorescent material.
Embodiment 3 takes by weighing 0.95 mole of La (NO
3)
3, be dissolved in 1000 ml distilled waters, 2 moles Ca (NO
3)
2, 0.05 mole Ce (NO
3)
2, 1 mole Al (NO
3)
3, stirred 60 minutes.The oxalic acid that adds 1.0 moles stirred 60 minutes, added 100 milliliters of ammoniacal liquor, stirred 30 minutes, added 0.001 mole of NH
4The Cl solubility promoter filters.1000 degrees centigrade of constant temperature is 6 hours in box-type furnace, fragmentation, and the crucible of packing into, in 1300 degree degree centigrade reducing atmospheres, constant temperature 6 hours, fragmentation, ball milling, washing, 120 degrees centigrade of dryings 10 hours are crossed 200 orders and are shone net, obtain said fluorescent material.
Embodiment 4 takes by weighing 0.90 mole of Lu (NO
3)
3, be dissolved in 1000 ml distilled waters, 1 mole Ba (NO
3)
2, 1 mole Mg (NO
3)
2, 0.1 mole Ce (NO
3)
2, add 1 mole Al (NO3) 3, stirred 60 minutes.The oxalic acid that adds 1.0 moles stirred 60 minutes, added 100 milliliters of ammoniacal liquor, stirred 30 minutes, added 0.001 mole of NH
4The F solubility promoter filters.1000 degrees centigrade of constant temperature is 6 hours in box-type furnace, fragmentation, and the crucible of packing into, and then in 1300 degree degree centigrade reducing atmospheres, constant temperature 6 hours, fragmentation, ball milling, washing, 120 degrees centigrade of dryings 10 hours are crossed 200 orders and are shone net, obtain said fluorescent material.
Embodiment 5 takes by weighing 1 mole of La (NO
3)
3, be dissolved in 1000 ml distilled waters, 2 moles Sr (NO
3)
2, 0.05 mole Ce (NO
3)
2, add 1 mole Al (NO
3)
3, stirred 60 minutes.The oxalic acid that adds 1.0 moles stirred 60 minutes, added 100 milliliters of ammoniacal liquor, stirred 30 minutes, added 0.001 mole of H
3BO
3Solubility promoter filters.1000 degrees centigrade of constant temperature is 6 hours in box-type furnace, fragmentation, the crucible of packing into, and then in 1300 degree degree centigrade reducing atmospheres constant temperature 6 hours, fragmentation, ball milling, washing, 120 degrees centigrade of dryings 10 hours are crossed 200 orders and are shone net, obtain said fluorescent material.
Above embodiment, the present invention embodiment several more preferably just, the common variation that those skilled in the art carries out in technical scheme scope of the present invention all should be included within protection scope of the present invention.
Claims (3)
1. white light and backlight LED fluorescent material is characterized in that the chemical structural formula of this fluorescent material is: RE1
xCe
xM
2AlO
5, wherein, M is a kind of in the alkaline-earth metal or wherein several, RE is a kind of among the La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Lu in the rare earth element or wherein several, 0. 001≤x＜1.
2. white light as claimed in claim 1 and backlight LED are with the preparation method of fluorescent material; It is characterized in that according to each atoms of elements ratio in the said chemical structural formula; Take by weighing nitrate that each element comprises alkaline-earth metal M, rare earth elements RE, Al, Ce as the primitive reaction thing, with NH
4X, BaX
2, SrX
2, in boric acid or the borate one or more are as solubility promoter, X is one or more in the halogen, the consumption of solubility promoter is 0.01-20 ﹪ of primitive reaction thing gross weight; During preparation, at first the nitrate with the corresponding weight of each element is dissolved in the distilled water, mixes, and is heated to 50-70 degrees centigrade, stirs 50-80 minutes; Add oxalic acid again, stirred 50-80 minutes; Add ammoniacal liquor again, stirred 20-40 minutes, filter; 900-1000 degrees centigrade of constant temperature calcinations 5-8 hours in box-type furnace then; Fragmentation, the crucible of packing into, constant temperature calcination 5-8 hours in 1000-1400 degree centigrade of reducing atmosphere again, fragmentation, ball milling, washing 100-120 degrees centigrade of dryings 5-10 hours, is crossed 200 eye mesh screens then, obtains said fluorescent material.
3. like the application of claim 1 fluorescent material in making white light LEDs or backlight LED.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102775307A CN102352248A (en) | 2011-09-19 | 2011-09-19 | Fluorescent powder for white light-emitting diodes (LEDs) and backlight LEDs |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102775307A CN102352248A (en) | 2011-09-19 | 2011-09-19 | Fluorescent powder for white light-emitting diodes (LEDs) and backlight LEDs |
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|---|---|
| CN102352248A true CN102352248A (en) | 2012-02-15 |
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ID=45575891
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703076A (en) * | 2012-06-11 | 2012-10-03 | 中国科学院福建物质结构研究所 | Fluorescent powder for white LED (Light Emitting Diode) and preparation method thereof |
| CN102703077A (en) * | 2012-06-11 | 2012-10-03 | 中国科学院福建物质结构研究所 | Fluorescent powder, and preparation method and application thereof |
| CN102888221A (en) * | 2012-10-29 | 2013-01-23 | 江苏博睿光电有限公司 | Fluorescent powder for LED and preparation method thereof |
| CN112442369A (en) * | 2020-12-04 | 2021-03-05 | 电子科技大学 | Calcium ion doped enhanced up-conversion red light emitting material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101376522A (en) * | 2008-10-09 | 2009-03-04 | 天津大学 | Fluorescent powder for white light LED and preparation thereof |
| CN101439869A (en) * | 2008-12-18 | 2009-05-27 | 江门市科恒实业股份有限公司 | Preparation of cerium activated rare earth aluminate ultraviolet transmitting fluorescent powder |
| US20090212314A1 (en) * | 2008-02-27 | 2009-08-27 | The Regents Of The University Of California | YELLOW EMITTING PHOSPHORS BASED ON Ce3+-DOPED ALUMINATE AND VIA SOLID SOLUTION FOR SOLID-STATE LIGHTING APPLICATIONS |
-
2011
- 2011-09-19 CN CN2011102775307A patent/CN102352248A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090212314A1 (en) * | 2008-02-27 | 2009-08-27 | The Regents Of The University Of California | YELLOW EMITTING PHOSPHORS BASED ON Ce3+-DOPED ALUMINATE AND VIA SOLID SOLUTION FOR SOLID-STATE LIGHTING APPLICATIONS |
| WO2009108840A1 (en) * | 2008-02-27 | 2009-09-03 | The Regents Of The University Of California | Yellow emitting phosphors based on ce3+-doped aluminate and via solid solution for solid-state lighting applications |
| CN101376522A (en) * | 2008-10-09 | 2009-03-04 | 天津大学 | Fluorescent powder for white light LED and preparation thereof |
| CN101439869A (en) * | 2008-12-18 | 2009-05-27 | 江门市科恒实业股份有限公司 | Preparation of cerium activated rare earth aluminate ultraviolet transmitting fluorescent powder |
Non-Patent Citations (6)
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703076A (en) * | 2012-06-11 | 2012-10-03 | 中国科学院福建物质结构研究所 | Fluorescent powder for white LED (Light Emitting Diode) and preparation method thereof |
| CN102703077A (en) * | 2012-06-11 | 2012-10-03 | 中国科学院福建物质结构研究所 | Fluorescent powder, and preparation method and application thereof |
| CN102703077B (en) * | 2012-06-11 | 2016-08-10 | 中国科学院福建物质结构研究所 | A kind of fluorescent material and preparation method and application |
| CN102888221A (en) * | 2012-10-29 | 2013-01-23 | 江苏博睿光电有限公司 | Fluorescent powder for LED and preparation method thereof |
| CN102888221B (en) * | 2012-10-29 | 2014-07-23 | 江苏博睿光电有限公司 | Fluorescent powder for LED and preparation method thereof |
| CN112442369A (en) * | 2020-12-04 | 2021-03-05 | 电子科技大学 | Calcium ion doped enhanced up-conversion red light emitting material and preparation method thereof |
| CN112442369B (en) * | 2020-12-04 | 2021-12-03 | 电子科技大学 | Calcium ion doped enhanced up-conversion red light emitting material and preparation method thereof |
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Application publication date: 20120215 |