CN104031645A - Orange fluorescent powder for white-light LEDs (light-emitting diodes) and preparation method thereof - Google Patents
Orange fluorescent powder for white-light LEDs (light-emitting diodes) and preparation method thereof Download PDFInfo
- Publication number
- CN104031645A CN104031645A CN201410279997.9A CN201410279997A CN104031645A CN 104031645 A CN104031645 A CN 104031645A CN 201410279997 A CN201410279997 A CN 201410279997A CN 104031645 A CN104031645 A CN 104031645A
- Authority
- CN
- China
- Prior art keywords
- fluorescent powder
- powder
- white light
- light led
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
Landscapes
- Luminescent Compositions (AREA)
Abstract
The invention provides an orange fluorescent powder for white-light LEDs (light-emitting diodes) and a preparation method thereof. The chemical formula of the fluorescent powder is (LU[1-x]Cex)2MMg2(Si[3-y]Tiy)O12, wherein M is one or more of alkali earth metals Ca, Sr and Ba, 0<X<=0.1, and 0.05<y<=0.5. The preparation method comprises the following steps: (1) mixing Lu2O3, CeO2, MCO3, MgO, SiO2 and TiO2, carrying out ball milling uniformly, and drying to obtain a powder mixture; (2) carrying out solid-phase sintering on the powder mixture in a muffle furnace, and grinding to obtain primary powder; and (3) putting the primary powder into a pipe furnace, introducing a reducing atmosphere, calcining, and grinding to obtain the orange fluorescent powder for white-light LEDs. The orange fluorescent powder has the advantages of uniform particle size, favorable crystallinity and excellent luminescence. The method is simple to operate, low in facility requests and suitable for industrial production.
Description
Technical field
The invention belongs to fluorescent material and preparation field thereof, particularly a kind of orange yellow fluorescent powder for white light LED and preparation method thereof.
Background technology
LED illumination is with respect to conventional light source, have advantages of that volume is little, less energy-consumption, luminous efficiency are high, long lifetime, low thermal radiation, the aspect such as pollution-free, become the most promising lighting engineering of 21 century, fluorescent material is that fluorescence converts the core of realizing white light emission in white light LEDs to.At present the scheme of synthesize white light LED mainly contains two kinds of the compound yellow fluorescent powder of blue chip and the compound three primary colors fluorescent powders of near ultraviolet chip.Wherein the spectral response curve of fluorescent material is determining the quality of the white light that LED device produces, and there is following problem in current used commercial powder: the yellow fluorescent powder of coupling blue chip is the most widely used commercial YAG: Ce, yet this fluorescent material spectral distribution is single, especially lack red visible light part, colour rendering index is very low, is not suitable for the white light of interior lighting.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of white light LEDs orange fluorescent powder and preparation method thereof.The YAG using from tradition: Ce is different, and its emission wavelength is long, and colour rendering index is high, is potential LED interior lighting fluorescent material.
The invention provides a kind of orange yellow fluorescent powder for white light LED, chemical molecular formula is (LU
1-xce
x)
2mMg
2(Si
3-yti
y) O
12, M is a kind of in alkaline-earth metal Ca, Sr, Ba or their combination; 0 < X≤0.1 wherein, 0.05 < y≤0.5.
The excitation wavelength coverage of above-mentioned orange fluorescent powder is 420-520nm.
The emission wavelength coverage of above-mentioned orange fluorescent powder is 570～620nm.
The present invention also provides a kind of preparation method of orange yellow fluorescent powder for white light LED, comprises the following steps:
(1) get Lu
2o
3, CeO
2, MCO
3, MgO, SiO
2, TiO
2after mixing, ball milling is even, and wherein M is one or several in alkaline-earth metal Ca, Sr, Ba, dry, obtains powder mixture; Wherein, Lu
2o
3, CeO
2, MCO
3, MgO, SiO
2, TiO
2mol ratio be (2-2x): 2x: 1: 2: (3-y): y, 0 < X≤0.1 wherein, 0.05 < y≤0.5;
(2) solid state reaction: by powder mixture high temperature sintering, the product obtaining grinds, obtains just powder of orange-yellow fluorescence;
(3) first powder is put into tube furnace, through high-temperature calcination, the product obtaining grinds, and obtains orange yellow fluorescent powder for white light LED.
The Lu that step (1) is described
2o
3, CeO
2, MCO
3, MgO, SiO
2, TiO
2mol ratio be (2-2x): 2x: 1: 2: (3-y): y, 0 < X≤0.1 wherein, 0.05 < y≤0.5.
The processing condition of the high temperature sintering that step (2) is described are, with the speed of 0.5～5 ℃/min, are warming up to 200～300 ℃, be incubateds 0.5～3 hour, then are warming up to 1300～1400 ℃ with the speed of 2～5 ℃/min, are incubated after 2～10h cooling.
Tube furnace in step (3) passes into reducing gas, and reducing gas is H
2, H
2and N
2, H
2with Ar or H
2gas mixture with He.
The processing condition of the high temperature sintering that step (3) is described are, be warming up to 200～300 ℃, then be warming up to 1100～1300 ℃ with the speed of 2～5 ℃/min with the speed of 0.5～5 ℃/min, cooling after insulation 2～5h.
Being ground to described in step (2) and (3) is ground to D by product
50between 10～16 microns.
beneficial effect
The prepared orange fluorescent powder powder of the present invention is compared with commercial powder, and epigranular, crystal property is good, luminescent properties is excellent.Present method is simple to operate, low for equipment requirements, is applicable to suitability for industrialized production, is potential LED interior lighting fluorescent material.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of the embodiment of the present invention 1 gained fluorescent material;
Fig. 2 is the excitation spectrum of the embodiment of the present invention 1 gained fluorescent material, and monitoring wavelength is 605nm;
Fig. 3 is the utilizing emitted light spectrogram of the embodiment of the present invention 1 gained fluorescent material, and excitation wavelength is 467nm.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
According to stoichiometric ratio 1.96: 0.04: 1: 2: 2.95: 0.05, take Lu
2o
3, CeO
2, CaCO
3, MgO, SiO
2, TiO
2, above-mentioned raw materials is mixed and to be placed in the corundum ball grinder that fills dehydrated alcohol ball milling after 10 hours, be put in and dryly in the baking oven of 110 ℃ obtain dry mixed powder; Dry mixture is placed in to retort furnace, with the speed of 0.5 ℃/min, is warming up to 200 ℃, be incubated 3 hours, speed with 2 ℃/min is warming up to 1300 ℃ again, be incubated coolingly after 10 hours, the product after sintering is ground to D50 between 10～16 microns, obtain just powder; First powder is put into tube furnace, pass into 5%H2+95%N2 gas mixture, speed with 0.5 ℃/min is warming up to 200 ℃, speed with 2 ℃/min is warming up to 1100 ℃ again, cooling after insulation 5h, product after calcining is ground to D50 between 10～16 microns, obtains orange yellow fluorescent powder for white light LED (Lu
0.98ce
0.02)
2caMg
2(Si
2.95ti
0.05) O
12.
The excitation wavelength range of this fluorescent material is 420-520nm, and excitation peak is at 467nm, and emission wavelength ranges is 570-620nm, and emission peak is at 605nm.
Embodiment 2
According to stoichiometric ratio 1.8: 0.2: 1: 2: 2.2: 0.5, take Lu
2o
3, CeO
2, MgO, BaCO
3, SiO
2, TiO
2, above-mentioned raw materials is mixed and to be placed in the corundum ball grinder that fills dehydrated alcohol ball milling after 10 hours, be put in and dryly in the baking oven of 110 ℃ obtain dry mixed powder; Dry mixture is placed in to retort furnace, with the speed of 5 ℃/min, is warming up to 300 ℃, be incubated 0.5 hour, then be warming up to 1400 ℃ with the speed of 5 ℃/min, be incubated cooling after 2 hours; Product after sintering is ground to D
50between 10～16 microns, obtain just powder, first powder is put into tube furnace, pass into 5%H
2the gas mixture of+95%He, is warming up to 300 ℃ with the speed of 3 ℃/min, then is warming up to 1300 ℃ with the speed of 5 ℃/min, cooling after insulation 2h, and the product after calcining is ground to D
50between 10～16 microns, obtain orange yellow fluorescent powder for white light LED (Lu
0.9ce
0.1)
2baMg
2(Si
2.5ti
0.5) O
12.
The excitation wavelength range of this fluorescent material is 420-520nm, and excitation peak is at 463nm, and emission wavelength ranges is 570-620nm, and emission peak is at 601nm.
Embodiment 3
According to stoichiometric ratio 1.92: 0.08: 0.8: 0.2: 2: 2.8: 0.2, take Lu
2o
3, CeO
2, CaCO
3, SrCO
3, MgO, SiO
2, TiO
2, above-mentioned raw materials is mixed and to be placed in the corundum ball grinder that fills dehydrated alcohol ball milling after 10 hours, be put in and dryly in the baking oven of 110 ℃ obtain dry mixed powder; Dry mixture is placed in to retort furnace, with the speed of 5 ℃/min, is warming up to 300 ℃, be incubated 0.5 hour, then be warming up to 1400 ℃ with the speed of 5 ℃/min, be incubated cooling after 2 hours; Product after sintering is ground to D50 between 10～16 microns, obtain just powder, first powder is put into tube furnace, pass into the gas mixture of 5%H2+95%Ar, speed with 3 ℃/min is warming up to 300 ℃, then is warming up to 1300 ℃ with the speed of 5 ℃/min, cooling after insulation 5h, product after calcining is ground to D50 between 10～16 microns, obtains orange yellow fluorescent powder for white light LED (Lu
0.96ce
0.04)
2(Ca
0.8sr
0.2) Mg
2(Si
2.8ti
0.2) O
12.
The excitation wavelength range of this fluorescent material is 420-520nm, and excitation peak is at 465nm, and emission wavelength ranges is 570-620nm, and emission peak is at 603nm.
Claims (9)
1. an orange yellow fluorescent powder for white light LED, is characterized in that: the chemical formula of this fluorescent material is (LU
1-xce
x)
2mMg
2(Si
3-yti
y) O
12, M is one or several in alkaline-earth metal Ca, Sr, Ba; 0 < X≤0.1 wherein, 0.05 < y≤0.5.
2. by a kind of orange yellow fluorescent powder for white light LED claimed in claim 1, it is characterized in that: the excitation wavelength coverage of described orange fluorescent powder is 420-520nm.
3. by a kind of orange yellow fluorescent powder for white light LED claimed in claim 1, it is characterized in that: the emission wavelength coverage of described orange fluorescent powder is 570～620nm.
4. a preparation method for orange yellow fluorescent powder for white light LED, comprises the following steps:
(1) get Lu
2o
3, CeO
2, MCO
3, MgO, SiO
2, TiO
2after mixing, ball milling is even, and wherein M is one or several in alkaline-earth metal Ca, Sr, Ba, dry, obtains powder mixture; Wherein, Lu
2o
3, CeO
2, MCO
3, MgO, SiO
2, TiO
2mol ratio be (2-2x): 2x: 1: 2: (3-y): y, 0 < X≤0.1 wherein, 0.05 < y≤0.5;
(2) solid state reaction: by powder mixture high temperature sintering, the product obtaining grinds, obtains just powder of orange-yellow fluorescence;
(3) first powder is put into tube furnace, through high-temperature calcination, the product obtaining grinds, and obtains orange yellow fluorescent powder for white light LED.
5. by the preparation method of a kind of orange yellow fluorescent powder for white light LED claimed in claim 4, it is characterized in that: the processing condition of the high temperature sintering that step (2) is described are, speed with 0.5～5 ℃/min is warming up to 200～300 ℃, be incubated 0.5～3 hour, speed with 2～5 ℃/min is warming up to 1300～1400 ℃ again, cooling after insulation 2～10h.
6. by the preparation method of a kind of orange yellow fluorescent powder for white light LED claimed in claim 4, it is characterized in that: in the tube furnace described in step (3), have reducing gas.
7. by the preparation method of a kind of orange yellow fluorescent powder for white light LED claimed in claim 7, it is characterized in that: described reducing gas is H
2, H
2and N
2, H
2with Ar or H
2gas mixture with He.
8. by the preparation method of a kind of orange yellow fluorescent powder for white light LED claimed in claim 4, it is characterized in that: the processing condition of the high-temperature calcination that step (3) is described are, speed with 0.5～5 ℃/min is warming up to 200～300 ℃, speed with 2～5 ℃/min is warming up to 1100～1300 ℃ again, cooling after insulation 2～5h.
9. by the preparation method of a kind of orange yellow fluorescent powder for white light LED claimed in claim 4, it is characterized in that: being ground to described in step (2) and (3) is ground to D by product
50between 10～16 microns.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410279997.9A CN104031645B (en) | 2014-06-20 | 2014-06-20 | A kind of orange yellow fluorescent powder for white light LED and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410279997.9A CN104031645B (en) | 2014-06-20 | 2014-06-20 | A kind of orange yellow fluorescent powder for white light LED and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104031645A true CN104031645A (en) | 2014-09-10 |
| CN104031645B CN104031645B (en) | 2016-08-17 |
Family
ID=51462648
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410279997.9A Expired - Fee Related CN104031645B (en) | 2014-06-20 | 2014-06-20 | A kind of orange yellow fluorescent powder for white light LED and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104031645B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1922286A (en) * | 2003-10-29 | 2007-02-28 | 吉尔科有限公司 | Garnet phosphor materials having enhanced spectral characteristics |
| US20110227476A1 (en) * | 2010-03-19 | 2011-09-22 | Nitto Denko Corporation | Light emitting device using orange-red phosphor with co-dopants |
| CN102618274A (en) * | 2012-03-13 | 2012-08-01 | 湖南信多利新材料有限公司 | Green phosphor for LED (Light-Emitting Diode) and preparation method of green phosphor |
-
2014
- 2014-06-20 CN CN201410279997.9A patent/CN104031645B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1922286A (en) * | 2003-10-29 | 2007-02-28 | 吉尔科有限公司 | Garnet phosphor materials having enhanced spectral characteristics |
| US20110227476A1 (en) * | 2010-03-19 | 2011-09-22 | Nitto Denko Corporation | Light emitting device using orange-red phosphor with co-dopants |
| CN102618274A (en) * | 2012-03-13 | 2012-08-01 | 湖南信多利新材料有限公司 | Green phosphor for LED (Light-Emitting Diode) and preparation method of green phosphor |
Non-Patent Citations (3)
| Title |
|---|
| ANANT A. SETLUR等: "Crystal Chemistry and Luminescence of Ce3+-Doped Lu2CaMg2(Si,Ge)3O12 and Its Use in LED Based Lighting", 《CHEM. MATER.》 * |
| 李高锋 等: "铈掺杂黄色荧光粉(LuGd)2CaMg2Si3O12的发光性能研究", 《材料保护》 * |
| 王飞等: "白光LED 用Ca0.955Al2Si2-xTixO8∶Eu2 + 荧光粉的晶体结构和光谱特性研究", 《稀有金属》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104031645B (en) | 2016-08-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chen et al. | A novel double-perovskite Gd 2 ZnTiO 6: Mn 4+ red phosphor for UV-based w-LEDs: structure and luminescence properties | |
| CN105694870B (en) | A kind of Eu3+The positive sodium magnesium silicate red fluorescence powder and its preparation method and application of activation | |
| CN103725285B (en) | Single-substrate white-light fluorescent powder for white-light LEDs (light-emitting diodes) and preparation method thereof | |
| CN103242830B (en) | Fluorosilicate-based blue-green fluorescent powder as well as preparation method and applications of fluorescent powder | |
| CN104726097A (en) | Novel yellow fluorescent powder and preparation method thereof | |
| CN104130774A (en) | Chlorosilicate fluorescent powder and preparation method thereof | |
| CN104498031B (en) | A kind of phosphate yellow fluorescent powder and preparation method thereof for white light LEDs | |
| CN103740364B (en) | A kind of yellow orange-orange red orthosilicate fluorescent material and preparation method thereof | |
| CN103289698B (en) | A kind of europium ion Eu 3+the phosphate base red fluorescence powder activated, preparation method and application | |
| CN108034423B (en) | Mn (manganese)2+Ion-doped silicate red fluorescent powder, preparation method and application | |
| CN103992795B (en) | A kind of LED red fluorescence powder and preparation method thereof | |
| CN103740367B (en) | Single-matrix white fluorescent powder for warm white LED (Light Emitting Diode) and preparation method thereof | |
| CN103725284B (en) | Single-substrate white-light fluorescent powder for white light and preparation method thereof | |
| CN105062472A (en) | Preparing method and application of blue fluorescent powder for warm white light LED | |
| CN103602335B (en) | Blue fluorescent powder for white light LED and preparation method thereof | |
| WO2016065725A1 (en) | Fluorescent material and manufacturing method thereof and composition containing the same | |
| CN102531387B (en) | Borate luminescent glass for white LED (light emitting diode) and preparation method thereof | |
| CN108659837B (en) | Eu (Eu)3+Ion activated titanium aluminate luminescent material and preparation method thereof | |
| CN102899043A (en) | Rare earth ion Dy<3+> doped Bi4Si3O12 white-light LED fluorescent powder material and preparation method thereof | |
| CN104031645B (en) | A kind of orange yellow fluorescent powder for white light LED and preparation method thereof | |
| TWI383036B (en) | Phosphor composition, and white light emitting diode device employ the same | |
| CN106867524B (en) | Preparation and application of alkaline earth aluminate blue fluorescent material | |
| Cheng et al. | Effects of RE 3+(RE= La, Ce, Pr, Sm, Dy, Ho, Er, and Tm) on the luminescence of Sr 2 MgSiO 5: Eu 2+ phosphors | |
| CN105219378B (en) | Silicate blue phosphor for white-light LEDs and preparation method thereof | |
| CN102533265A (en) | Phosphate yellow fluorescent powder excited by blue light and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160817 Termination date: 20210620 |