CN101368100B - Fluorescent powder transmitting yellow light and method of producing the same - Google Patents

Fluorescent powder transmitting yellow light and method of producing the same Download PDF

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Publication number
CN101368100B
CN101368100B CN2008100512165A CN200810051216A CN101368100B CN 101368100 B CN101368100 B CN 101368100B CN 2008100512165 A CN2008100512165 A CN 2008100512165A CN 200810051216 A CN200810051216 A CN 200810051216A CN 101368100 B CN101368100 B CN 101368100B
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fluorescent powder
fluorescent material
pbo
weighing
ceo
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CN101368100A (en
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张家骅
王磊
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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

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Abstract

The invention discloses fluorescent powder used in an LED, which relates to the technical field of lighting and displaying, in particular to fluorescent powder emitting yellow light used for manufacturing white light LED and a preparing method thereof. The fluorescent powder comprises the chemical compound with the following chemical formula: Y3-x-yPbxCeyAl5O12, wherein the x in the formula is equal to 0.01 to 0.10; y is equal to 0.003 to 0.2. The preparing method comprise the following steps: Y2O3, Al2O3, CeO2 and PbO are respectively weighed according to the stoichiometric amount of each material, put in a corundum crucible and in a high-temperature furnace to be heated to 1300 to 1700 DEG C for 3 to 7 hours under the reducing atmosphere after being ground and mixed together with BaF2 used as the fluxing agent, and naturally cooled to obtain the fluorescent powder. Compared with Y3Al5O12:Ce fluorescent powder, the fluorescent powder has the advantages of the enhanced luminescence and red shift of the emission peak position, and the color rendering index of the LED made of the material is enhanced.

Description

Fluorescent material of emission sodium yellow and preparation method thereof
Technical field
The present invention relates to be used for to throw light on fluorescent material with the photodiode (LED) in technique of display field, fluorescent material of particularly a kind of emission sodium yellow that is used to make white light LEDs and preparation method thereof.
Background technology
White light emitting diode (LED) is generally believed it is the new light sources that 21 century substitutes the traditional lighting device.The scheme that produces white light mainly adopts the fluorescent material of coating emission sodium yellow on the GaN blue-light LED chip.At present, yellow fluorescent powder is mainly with Y 3Al 5O 12(YAG): Ce is main, and this kind fluorescent material lacks the ruddiness composition makes that prepared LED colour rendering index is on the low side, therefore, develops the manufacturing technology level that the fluorescent material of launching sodium yellow more efficiently will effectively improve white light emitting diode (LED).
Summary of the invention
The objective of the invention is to propose a kind of fluorescent material that is used to make the emission sodium yellow of white light emitting diode (LED),, improve the quality level of white light LEDs to overcome the above-mentioned shortcoming that the yellow fluorescent material that is used to make white light LEDs at present exists.
The present invention launches the fluorescent material of sodium yellow, is to have following general formula: Y 3-x-yPb xCe yAl 5O 12, x=0.01 in the formula～0.10; Y=0.003～0.2.
The composition characteristic of this fluorescent material is to introduce Pb ionic replacement part Y ion in YAG:Ce.Because the ionic radius of Pb is greater than Y 3+, the introducing of Pb causes lattice distortion, and it is big that lattice parameter becomes, and it is big that the crystal field splitting becomes, and causes the luminous enhancing of fluorescent material, simultaneously, the emission peak positions red shift.
Pb in this compound exists with the divalence and the quadrivalent ion of equivalent, so average valence is a trivalent.When Pb content x=0.05, fluorescent material luminous the strongest, than the raising that does not add Pb about 10%, about emission peak positions red shift 3nm.With Y 3Al 5O 12(YAG): Ce fluorescent material is compared, and the advantage of luminous enhancing, emission peak positions red shift is arranged, and increases with the LED colour rendering index of this material preparation.
The preparation method that the present invention launches the fluorescent material of sodium yellow may further comprise the steps:
A. with Y 2O 3, Al 2O 3, CeO 2, PbO is raw material, presses chemical formula Y 3-x-yPb xCe yAl 5O 12In the stoichiometric ratio of each element take by weighing the powder Y of calculated amount respectively 2O 3, Al 2O 3, CeO 2, PbO;
B. will be as the BaF of fusing assistant 2The Y that takes by weighing with step a 2O 3, Al 2O 3, CeO 2, PbO together ground and mixed put into corundum crucible after evenly;
C. the described corundum crucible that compound is housed of step b is placed High Temperature Furnaces Heating Apparatus, under reducing atmosphere, be heated to 1300-1700 ℃, constant temperature 3-7 hour, naturally cooling took out the fluorescent material that promptly gets described emission sodium yellow.
Described fusing assistant BaF 2Add-on be Y 2O 3, Al 2O 3, CeO 2, the PbO quality and 3%～5%.
Description of drawings
Fig. 1 is the graphic representation of fluorescent material emissive porwer of the present invention with the Pb change in concentration.
Embodiment
By following examples the present invention is described in further detail.
Embodiment 1
The preparation chemical formula is Y 2.93Pb 0.01Ce 0.06Al 5O 12Gold-tinted fluorescent material.
Measure than taking by weighing 3.3081g Y by element chemistry in the following formula 2O 3, 2.5491g Al 2O 3, 0.1033gCeO 2, 0.0223g PbO takes by weighing 0.1794g BaF again 2Make solubility promoter; With the abundant ground and mixed of the raw material that takes by weighing evenly after, insert the high-purity corundum crucible, put into High Temperature Furnaces Heating Apparatus; At CO or H 2And N 2Under the reducing atmosphere condition, promptly obtained gold-tinted fluorescent material Y in 3 hours 1500 ℃ of heating 2.93Pb 0.01Ce 0.06Al 5O 12
Embodiment 2
The preparation chemical formula is Y 2.89Pb 0.05Ce 0.06Al 5O 12Gold-tinted fluorescent material.
Measure than taking by weighing 3.2630g Y by element chemistry in the following formula 2O 3, 2.5491g Al 2O 3, 0.1033gCeO 2, 0.1115g PbO takes by weighing 0.1808g BaF again 2Make solubility promoter; With the abundant ground and mixed of the raw material that takes by weighing evenly after, insert the high-purity corundum crucible, put into High Temperature Furnaces Heating Apparatus; At CO or H 2And N 2Under the reducing atmosphere condition, promptly obtained gold-tinted fluorescent material Y in 3 hours 1500 ℃ of heating 2.89Pb 0.05Ce 0.06Al 5O 12
Embodiment 3
The preparation chemical formula is Y 2.84Pb 0.1Ce 0.06Al 5O 12Gold-tinted fluorescent material.
Measure than taking by weighing 3.2065g Y by element chemistry in the following formula 2O 3, 2.5491g Al 2O 3, 0.1033gCeO 2, 0.2230g PbO takes by weighing 0.1825g BaF again 2Make solubility promoter; With the abundant ground and mixed of the raw material that takes by weighing evenly after, insert the high-purity corundum crucible, put into High Temperature Furnaces Heating Apparatus; At CO or H 2And N 2Under the reducing atmosphere condition, promptly obtained gold-tinted fluorescent material Y in 3 hours 1500 ℃ of heating 2.84Pb 0.1Ce 0.06Al 5O 12
Embodiment 4
The preparation chemical formula is Y 2.85Pb 0.05Ce 0.1Al 5O 12Gold-tinted fluorescent material.
Measure than taking by weighing 3.1839g Y by element chemistry in the following formula 2O 3, 2.5491g Al 2O 3, 0.1721gCeO 2, 0.3230g PbO, 0.1799g BaF 2Make solubility promoter; With the abundant ground and mixed of the raw material that takes by weighing evenly after, insert the high-purity corundum crucible, put into High Temperature Furnaces Heating Apparatus; At CO or H 2And N 2Under the reducing atmosphere condition, promptly obtained gold-tinted fluorescent material Y in 3 hours 1500 ℃ of heating 2.85Pb 0.05Ce 0.1Al 5O 12
Embodiment 5
The preparation chemical formula is Y 2.8Pb 0.05Ce 0.15Al 5O 12Gold-tinted fluorescent material.
Measure than taking by weighing 3.2178g Y by element chemistry in the following formula 2O 3, 2.5491g Al 2O 3, 0.2582gCeO 2, 0.1115g PbO, 0.1841g BaF 2Make solubility promoter; With the abundant ground and mixed of the raw material that takes by weighing evenly after, insert the high-purity corundum crucible, put into High Temperature Furnaces Heating Apparatus; At CO or H 2And N 2Under the reducing atmosphere condition, promptly obtained gold-tinted fluorescent material Y in 3 hours 1500 ℃ of heating 2.8Pb 0.05Ce 0.15Al 5O 12
Embodiment 6
The preparation chemical formula is Y 2.947Pb 0.05Ce 0.003Al 5O 12Gold-tinted fluorescent material.
Measure than taking by weighing 3.3273g Y by element chemistry in the following formula 2O 3, 2.5491g Al 2O 3, 0.0053gCeO 2, 0.1115g PbO, 0.1798g BaF 2Make solubility promoter; With the abundant ground and mixed of the raw material that takes by weighing evenly after, insert the high-purity corundum crucible, put into High Temperature Furnaces Heating Apparatus; At CO or H 2And N 2Under the reducing atmosphere condition, promptly obtained gold-tinted fluorescent material Y in 3 hours 1500 ℃ of heating 2.947Pb 0.05Ce 0.003Al 5O 12
Embodiment 7
The preparation chemical formula is Y 2.75Pb 0.05Ce 0.2Al 5O 12Gold-tinted fluorescent material.
Measure than taking by weighing 3.1420g Y by element chemistry in the following formula 2O 3, 2.5491g Al 2O 3, 0.3442gCeO 2, 0.1115g PbO, 0.1844g BaF 2Make solubility promoter; With the abundant ground and mixed of the raw material that takes by weighing evenly after, insert the high-purity corundum crucible, put into High Temperature Furnaces Heating Apparatus.At CO or H 2And N 2Under the reducing atmosphere condition, promptly obtained gold-tinted fluorescent material Y in 3 hours 1500 ℃ of heating 2.75Pb 0.05Ce 0.2Al 5O 12
The luminous intensity of fluorescent material changes along with the variation of Pb content x, and as shown in Figure 1, when Pb content x=0.05, the luminous intensity of fluorescent material is the highest.

Claims (3)

1. a fluorescent material of launching sodium yellow is characterized in that having following general formula: Y 3-x-yPb xCe yAl 5O 12, x=0.01 in the formula～0.10; Y=0.003～0.2.
2. method for preparing the described fluorescent material of claim 1 is characterized in that may further comprise the steps:
A. with Y 2O 3, Al 2O 3, CeO 2, PbO is raw material, presses chemical formula Y 3-x-yPb xCe yAl 5O 12In the stoichiometric ratio of each element take by weighing the powder Y of calculated amount respectively 2O 3, Al 2O 3, CeO 2, PbO;
B. will be as the BaF of fusing assistant 2The Y that takes by weighing with step a 2O 3, Al 2O 3, CeO 2, PbO together ground and mixed put into corundum crucible after evenly;
C. the described corundum crucible that compound is housed of step b is placed High Temperature Furnaces Heating Apparatus, under reducing atmosphere, be heated to 1300-1700 ℃, constant temperature 3-7 hour, naturally cooling took out and promptly gets the described fluorescent material of claim 1.
3. the method for preparing the described fluorescent material of claim 1 according to claim 2 is characterized in that, described fusing assistant BaF 2Add-on be Y 2O 3, Al 2O 3, CeO 2, the PbO quality and 3%～5%.
CN2008100512165A 2008-09-25 2008-09-25 Fluorescent powder transmitting yellow light and method of producing the same Expired - Fee Related CN101368100B (en)

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CN101818058B (en) * 2010-04-13 2013-07-03 中国科学院长春光学精密机械与物理研究所 Orange long-afterglow fluorescent powder and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1331272A (en) * 2000-06-26 2002-01-16 中国科学院长春光学精密机械与物理研究所 Wavelength-converting luminous material of white light for LED

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1331272A (en) * 2000-06-26 2002-01-16 中国科学院长春光学精密机械与物理研究所 Wavelength-converting luminous material of white light for LED

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
李长敏.LED暖白光照明用(Y2.95-xGdxCe0.05)Al5O12系列荧光粉的晶相与三维荧光光谱.《大连轻工业学院学报》.2007,第26卷(第2期),全文. *

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