CN1880402A - Method for preparing white light LED phosphor powder and flux therefor - Google Patents

Method for preparing white light LED phosphor powder and flux therefor Download PDF

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Publication number
CN1880402A
CN1880402A CNA2005100437438A CN200510043743A CN1880402A CN 1880402 A CN1880402 A CN 1880402A CN A2005100437438 A CNA2005100437438 A CN A2005100437438A CN 200510043743 A CN200510043743 A CN 200510043743A CN 1880402 A CN1880402 A CN 1880402A
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China
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compound
fusing assistant
white light
light led
fluorescent material
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CNA2005100437438A
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CN100482763C (en
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魏岚
韩钧祥
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Xiamen Topstar Lighting Co Ltd
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Xiamen Topstar Lighting Co Ltd
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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

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Abstract

This invention discloses a method for producing white light LED fluorescent powder and fluxing agent. The fluxing agent used in producing white light LED fluorescent powder comprises at least one compound, in which the metal ions are the same with those in the fluorescent powder. The process for producing white light LED fluorescent powder comprises: (1) charging and mixing material: weight and homogenously mix the raw material and fluxing agent to obtain the total mixing material, wherein the raw material comprises Y2O3, Al2O3, Gd2O3, Ga2O3, CeO2 or any compound that can decompose these oxide compounds, and the fluxing agent comprises at least one compound in which the metal ions are the same with those in the fluorescent powder; (2) high temperature burning; (3) post treatment. The fluxing agent and the method of this invention do not introduce other metal ions into the fluorescent powder, which further improves the brightness and usability of the fluorescent powder.

Description

The method and the fusing assistant that prepare white light LED fluorescent powder
Affiliated technical field
The present invention relates to a kind of method and fusing assistant for preparing white light LED fluorescent powder, particularly relate to a kind of method for preparing white light LED fluorescent powder and the fusing assistant that can seldom introduce external metal ion for fluorescent material.
Background technology
Along with developing rapidly of white light LEDs, to YAG:Ce 3+The requirement of fluorescent material is also more and more higher.Require YAG:Ce 3+Fluorescent material has higher brightness and good use properties.Except conditions such as purity of raw materials and calcination technology to YAG:Ce 3+Outside the brightness of fluorescent material and use properties were influential, the selection of fusing assistant was to YAG:Ce 3+The brightness of fluorescent material and use properties also have very big influence.The effect of fusing assistant is: be used to reduce calcination temperature and improve degree of crystallinity.Present fusing assistant is generally the Ba compound (as Ba (NO 3) 2, BaF 2, BaCl 22H 2O), alkali metal compound (as NaF, KF).Their use can increase YAG:Ce 3+The introducing of external metal ion in the fluorescent material, this can reduce fluorescent material brightness, and use properties is produced adverse influence.
Summary of the invention
In order to reduce the introducing of external metal ion, the invention provides a kind of method and fusing assistant for preparing white light LED fluorescent powder, this method is seldom introduced and is not even introduced the external metal ion that is not had in the fluorescent material, and this makes fluorescent material brightness and use properties all be further improved.
Present method solves the method that its technical problem adopts: the fusing assistant of preparation white light LED fluorescent powder, and it comprises at least a compound, the metal ion that is contained in this compound is identical with the metal ion that fluorescent material is had.
Described fluorescent material is YAG:Ce 3+Fluorescent material and derivative thereof, then the metal ion that is contained in the compound of fusing assistant is Ce 3+
The compound of described fusing assistant is respectively CeF 3Or and CeCl 3Or and Ce (NO 3) 36H 2O or and Ce 2(C 2O 4) 3Or and Ce 2(CO 3) 3
Fusing assistant preferably also comprises the mullite powder, and mullite powder and above-mentioned compound form composite fluxing agent.
Described composite fluxing agent weight accounts for (0.5～10) % of total compound weight.Best, the weight of composite fluxing agent accounts for (2～4) % of the gross weight of starting material and fusing assistant.
Described mullite grain weight amount accounts for (0.05-5) % of total compound weight.Best, the weight of mullite powder accounts for (0.5～2) % of the gross weight of starting material and fusing assistant.
Described fluorescent material is YAG:Ce 3+Fluorescent material and derivative thereof, then the metal ion that is contained in the compound of fusing assistant is Y 3+Or and Al 3+Or and Gd 3+Or and Ga 3+
The compound of described fusing assistant is respectively Y 3+Or and Al 3+Or and Gd 3+Or and Ga 3+Or and Ce 3+Fluorochemical or and muriate or and nitrate or and oxalate or and carbonate.
Present method solves the other method that its technical problem adopts: prepare the method for white light LED fluorescent powder, it comprises:
(1) batching and batch mixing step: be used to take by weighing that also mixing starting material and fusing assistant are to obtain total compound, starting material comprise Y 2O 3, Al 2O 3, Gd 2O 3, Ga 2O 3, CeO 2Perhaps can resolve into other compounds of this type oxide, as carbonate, oxalate, oxyhydroxide etc.; Fusing assistant comprises at least a compound, and the metal ion that is contained in this compound is identical with the metal ion that fluorescent material is had;
(2) high temperature sintering step: be used under reductive condition, total compound that high temperature sintering is above-mentioned, wherein, calcination temperature is (1300～1600) ℃, calcination time is (2～3) hour;
(3) post-processing step: after the good fluorescent material cooling of fourth calcination, broken fluorescent material, porphyrize or pulverize fluorescent material again carries out chemical treatment then, washs, sieves, centrifuging, dries fluorescent material at last.
Described fluorescent material is YAG:Ce 3+Fluorescent material and derivative thereof, then the metal ion that is contained in the compound of fusing assistant is Ce 3+
The compound of described fusing assistant is respectively CeF 3Or and CeCl 3Or and Ce (NO 3) 36H 2O or and Ce 2(C 2O 4) 3Or and Ce 2(CO 3) 3
Fusing assistant preferably also comprises the mullite powder, and mullite powder and above-mentioned compound form composite fluxing agent.
Described mullite grain weight amount accounts for (0.05-5) % of total compound weight.Best, the weight of mullite powder accounts for (0.5～2) % of the gross weight of starting material and fusing assistant.
Described fluorescent material is YAG:Ce 3+Fluorescent material and derivative thereof, then the metal ion that is contained in the compound of fusing assistant is Y 3+Or and Al 3+Or and Gd 3+Or and Ga 3+
The compound of described fusing assistant is respectively Y 3+Or and Al 3+Or and Gd 3+Or and Ga 3+Or and Ce 3+Fluorochemical or and muriate or and nitrate or and oxalate or and carbonate.
By the above-mentioned description of this invention as can be known, compare with background technology, the present invention has following advantage:
One, the metal ion that is contained in the compound of fusing assistant of the present invention is identical with the metal ion that fluorescent material is had, fusing assistant then of the present invention seldom even is not introduced the external metal ion that is not had in the fluorescent material for fluorescent material, this makes fluorescent material brightness and use properties all be further improved, experimental result shows, make φ 5mm encapsulation 20mA white light LEDs with the fluorescent material of the present invention's preparation, light efficiency can reach more than the 75lm/W;
Its two, the mullite powder is used to reduce calcination temperature, improves degree of crystallinity, makes its crystal formation more complete.
Embodiment
Embodiment one
The fusing assistant of preparation white light LED fluorescent powder, it is a composite fluxing agent.Composite fluxing agent comprises one or more compounds and mullite powder.
The fluorescent material of present embodiment is Y 3-xAl 5O 12: xCe 3+The mole ratio of each metal ion equals each metal ion mole ratio of fluorescent material in starting material and the fusing assistant.Wherein the span of x is (0.01～0.15), but its value 0.03,0.035,0.04,0.045,0.05,0.055,0.06,0.065.
The metal ion that is contained in the compound of fusing assistant is Ce 3+The compound of fusing assistant is respectively CeF 3Or and CeCl 3Or and Ce (NO 3) 36H 2O or and Ce 2(C 2O 4) 3Or and Ce 2(CO 3) 3
The weight of composite fluxing agent accounts for (0.5～10) % of the gross weight of starting material and fusing assistant.If the weight of composite fluxing agent accounts for (2～4) % of the gross weight of starting material and fusing assistant, then effect is better, but its value 2.4%, 2.6%, 2.8%, 3.0%, 3.2%, 3.4%, 3.6%, 3.8%.
The mullite powder accounts for (0.05-5) % of the gross weight of starting material and fusing assistant.If the weight of mullite powder accounts for (0.5～2) % of the gross weight of starting material and fusing assistant, then effect is better, but its value 0.6%, 0.8%, 1%, 1.2%, 1.4%, 1.6%, 1.8%.
Prepare the method for white light LED fluorescent powder, it comprises:
(1). batching and batch mixing step: be used to take by weighing that also mixing starting material and fusing assistant are to obtain total compound, starting material comprise Y 2O 3, Al 2O 3, Gd 2O 3, Ga 2O 3, CeO 2(perhaps can resolve into other compounds of these oxide compounds) as carbonate, nitrate, oxyhydroxide etc.; Fusing assistant is used to reduce calcination temperature and improves degree of crystallinity, and it comprises one or more compounds and mullite powder, and described compound is CeF 3Or and CeCl 3Or and Ce (NO 3) 36H 2O or and Ce 2(C 2O 4) 3Or and Ce 2(CO 3) 3The weight of fusing assistant accounts for total compound (2～4) %, and the weight of mullite powder accounts for (0.5～2) % of the gross weight of total compound, and the mole ratio of each metal ion is identical with the mole ratio of each metal ion in the fluorescent material in total compound; Pack in the blender total compound and mixing, its mixing time is about 8～12 hours; Behind the mixing, total compound is packed in the corundum crucible;
(2) high temperature sintering step: be used under reductive condition, total compound that high temperature sintering is above-mentioned, wherein, calcination temperature is (1300～1600) ℃, calcination time is (2～3) hour;
(3) post-processing step: after being used for the cooling of the good fluorescent material of calcination,, pulverize fluorescent material by ball mill porphyrize or micronizer mill again, carry out chemical treatment then, wash, sieve, centrifuging, dry fluorescent material at last by crusher in crushing fluorescent material.
Experimental result shows, make φ 5mm encapsulation 20mA white light LEDs with the fluorescent material of the present invention's preparation after, light efficiency can reach more than the 751m/W.
Embodiment two
Present embodiment and embodiment one difference are: the fluorescent material of present embodiment is (Y 1-x-yCe xR y) 3Al 5O 12Wherein R is Eu or and Sm or and Tb.Wherein the span of x is (0.01～0.15), but its value 0.03,0.035,0.04,0.045,0.05,0.055,0.06,0.065.The span of y is (0～0.01), but its value 0,0.001,0.005,0.01.
The metal ion that is contained in the compound of fusing assistant is Ce 3+The compound of fusing assistant is respectively CeF 3Or and CeCl 3Or and Ce (NO 3) 36H 2O or and Ce 2(C 2O 4) 3Or and Ce 2(CO 3) 3
Embodiment three
Present embodiment and embodiment one difference are: the fluorescent material of present embodiment consists of Y 3-x-yGd yAl 5-zGa zO 12: xCe 3+Wherein the span of x is (0.01～0.15), but its value 0.03,0.035,0.04,0.045,0.05,0.055,0.06,0.065.The span of y is (0～2.5), but its value 0,0.5,1,1.5,2,2.5.The span of z is (0～4), but its value 0,1,2,3,4.
The metal ion that is contained in the compound of fusing assistant is Ce 3+The compound of fusing assistant is respectively CeF 3Or and CeCl 3Or and Ce (NO 3) 36H 2O or and Ce 2(C 2O 4) 3Or and Ce 2(CO 3) 3
Embodiment four
Present embodiment and embodiment one difference are: the compound YF of fusing assistant 3Or and AlF 3Or and YCl 3Or and AlCl 3
Embodiment five
Present embodiment and embodiment three differences are: the compound YF of fusing assistant 3Or and AlF 3Or and GdF 3Or and YCl 3Or and AlCl 3Or and GdCl 3
Embodiment six
Present embodiment and embodiment one difference are: the compound of fusing assistant is respectively Y 3+Or and Al 3+Or and Ce 3+Fluorochemical or and muriate or and nitrate or and oxalate or and carbonate.
Embodiment seven
Present embodiment and embodiment three differences are: the compound of fusing assistant is respectively Y 3+Or and Al 3+Or and Gd 3+Or and Ga 3+Or and Ce 3+Fluorochemical or and muriate or and nitrate or and oxalate or and carbonate.
The above, only for preferred embodiment of the present invention, so can not limit scope of the invention process with this, i.e. the equivalence of doing according to the present patent application claim and description changes and modification, all should still belong in the scope that patent of the present invention contains.

Claims (10)

1. prepare the fusing assistant of white light LED fluorescent powder, it comprises at least a compound, and the metal ion that is contained in this compound is identical with the metal ion that fluorescent material is had.
2. the fusing assistant of preparation white light LED fluorescent powder according to claim 1 is characterized in that: described fluorescent material is YAG:Ce 3+Fluorescent material and derivative thereof, then the metal ion that is contained in the compound of fusing assistant is Ce 3+
3. the fusing assistant of preparation white light LED fluorescent powder according to claim 2 is characterized in that: the compound of described fusing assistant is respectively CeF 3Or and CeCl 3Or and Ce (NO 3) 36H 2O or and Ce 2(C 2O 4) 3Or and Ce 2(CO 3) 3
4. according to the fusing assistant of claim 1 or 2 or 3 described preparation white light LED fluorescent powders, it is characterized in that: it also comprises the mullite powder, and mullite powder and above-mentioned compound form composite fluxing agent.
5. the fusing assistant of preparation white light LED fluorescent powder according to claim 4 is characterized in that: described composite fluxing agent weight accounts for (0.5～10) % of total compound weight.
6. the fusing assistant of preparation white light LED fluorescent powder according to claim 4 is characterized in that: described mullite grain weight amount accounts for (0.05-5) % of total compound weight.
7. the fusing assistant of preparation white light LED fluorescent powder according to claim 1 is characterized in that: described fluorescent material is YAG:Ce 3+Fluorescent material and derivative thereof, then the metal ion that is contained in the compound of fusing assistant is Y 3+Or and Al 3+Or and Gd 3+Or and Ga 3+
8. according to the fusing assistant of claim 1 or 2 or 7 described preparation white light LED fluorescent powders, it is characterized in that: the compound of described fusing assistant is respectively Y 3+Or and Al 3+Or and Gd 3+Or and Ga 3+Or and Ce 3+Fluorochemical or and muriate or and nitrate or and oxalate or and carbonate.
9. prepare the method for white light LED fluorescent powder, it is characterized in that: it comprises:
(1). batching and batch mixing step: be used to take by weighing that also mixing starting material and fusing assistant are to obtain total compound, starting material comprise Y 2O 3, Al 2O 3, Gd 2O 3, Ga 2O 3, CeO 2Perhaps can resolve into any compound of these oxide compounds; Fusing assistant comprises at least a compound, and the metal ion that is contained in this compound is identical with the metal ion that fluorescent material is had;
(2) high temperature sintering step: be used under reductive condition, total compound that high temperature sintering is above-mentioned, wherein, calcination temperature is (1300～1600) ℃, calcination time is (2～3) hour;
(3) post-processing step: after being used for the cooling of the good fluorescent material of calcination, broken fluorescent material, porphyrize or pulverize fluorescent material again carries out chemical treatment then, washs, sieves, centrifuging, dries fluorescent material at last.
10. the method for preparing white light LED fluorescent powder according to claim 9 is characterized in that: described fusing assistant also comprises the mullite powder, and mullite powder and above-mentioned compound form composite fluxing agent.
CNB2005100437438A 2005-06-17 2005-06-17 Method for preparing white light LED phosphor powder and flux therefor Expired - Fee Related CN100482763C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104130779A (en) * 2014-07-01 2014-11-05 南京大学 Yellow fluorescent powder used for white light LED and preparation method thereof
US9239157B2 (en) 2010-08-26 2016-01-19 Rasit Özgüc Light-emitting means, in particular for operation in lampholders for fluorescent lamps
TWI570093B (en) * 2013-01-28 2017-02-11 Schott Ag Strong scattering ceramic converter and its preparation method
CN106549093A (en) * 2016-10-25 2017-03-29 江苏师范大学 A kind of long-range luminescent device of the LED based on fluorescent transparent ceramic material

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9239157B2 (en) 2010-08-26 2016-01-19 Rasit Özgüc Light-emitting means, in particular for operation in lampholders for fluorescent lamps
TWI570093B (en) * 2013-01-28 2017-02-11 Schott Ag Strong scattering ceramic converter and its preparation method
US11427511B2 (en) 2013-01-28 2022-08-30 Schott Ag Strongly scattering ceramic converter and method for producing same
US11623892B2 (en) 2013-01-28 2023-04-11 Schott Ag Strongly scattering ceramic converter and method for producing same
CN104130779A (en) * 2014-07-01 2014-11-05 南京大学 Yellow fluorescent powder used for white light LED and preparation method thereof
CN106549093A (en) * 2016-10-25 2017-03-29 江苏师范大学 A kind of long-range luminescent device of the LED based on fluorescent transparent ceramic material

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Assignee: Xiamen Topstar New Materials Co., Ltd.

Assignor: Xiamen Topstar Lighting Co., Ltd.

Contract record no.: 2011350000073

Denomination of invention: Method for preparing white light LED phosphor powder and flux therefor

Granted publication date: 20090429

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Termination date: 20180617