CN108690618A - A kind of fluorescent powder and preparation method thereof and luminescent device - Google Patents
A kind of fluorescent powder and preparation method thereof and luminescent device Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 194
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000126 substance Substances 0.000 claims abstract description 26
- 238000009877 rendering Methods 0.000 claims abstract description 13
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 8
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 8
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 22
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 13
- 238000006722 reduction reaction Methods 0.000 claims description 13
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 4
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 4
- 229910001626 barium chloride Inorganic materials 0.000 claims description 4
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims description 4
- 239000011265 semifinished product Substances 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 229910001632 barium fluoride Inorganic materials 0.000 claims description 3
- 125000002091 cationic group Chemical group 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910003443 lutetium oxide Inorganic materials 0.000 claims description 3
- 238000005554 pickling Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052909 inorganic silicate Inorganic materials 0.000 claims description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 2
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- 238000001228 spectrum Methods 0.000 abstract description 18
- 230000005284 excitation Effects 0.000 description 15
- 238000000695 excitation spectrum Methods 0.000 description 9
- 230000009471 action Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000000295 emission spectrum Methods 0.000 description 5
- 108010043121 Green Fluorescent Proteins Proteins 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 238000010791 quenching Methods 0.000 description 4
- 230000000171 quenching effect Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 2
- 206010023126 Jaundice Diseases 0.000 description 1
- 241001025261 Neoraja caerulea Species 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011982 device technology Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7774—Aluminates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
- H01L33/504—Elements with two or more wavelength conversion materials
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Luminescent Compositions (AREA)
Abstract
The present invention relates to a kind of fluorescent powder and preparation method thereof and luminescent devices.A kind of fluorescent powder of the present invention, which is characterized in that its chemical general formula is:(Lu3-x-zRz)(Al5-yGay)O12:XCe, wherein one or more elements in R Y, La, Tb, Gd and Dy, and 0.01<x<0.03,2.00<y<2.50,0≤z≤1.00, after the fluorescent powder is excited, emission peak peak wavelength is 490-500nm.The present invention has filled up the gap of bluish-green spectrum, can obtain colour rendering index 95 or more superelevation colour rendering index fluorescent powder product.
Description
Technical field
The invention belongs to rare-earth luminescent material fields, and in particular to a kind of novel garnet-base efficient green fluorescent powder and its
Preparation method and luminescent device.
Background technology
As high-end lighting area is higher and higher to the color developing requirement of white light LEDs, in order to make up feux rouges in white light LEDs
It is main in the market that green light light is made up using LuAlO series or Y (AlGa) O series phosphor powders with the insufficient defect of green spectrum
Spectrum arranges in pairs or groups nitride rouge and powder to make up red-light spectrum, to obtain the white light LEDs product of different high colour developing schemes.But the program
For the white light LEDs of superelevation colour rendering index, there is larger enforcement difficulties, because of LuAlO series or Y (AlGa) O systems
Row fluorescent powder arrange in pairs or groups nitride rouge and powder composition spectrum in, lack bluish-green spectral components, for requiring colour rendering index 95 and
There are obvious shortcomings in above scheme.
In order to supplement the blue green light ingredient in white LED spectrum, Liu Dan of the China Measures Institute et al. has studied one kind
Chemical composition is SrMgAl10O17:Eu2+/Er3+Blue-emitting phosphor, which can be within the scope of 300-390nm
It is effectively excited, emission spectrum is distributed in 430-520nm, and emission peak is located at 460nm.Effective excites scope of the fluorescent powder belongs to
Near ultraviolet region, and market white light LEDs product mainly uses 440-460nm blue chips to excite at present, which greatly limits this
The market application prospect of fluorescent powder.
A kind of MSi invents in the patent of Publication No. CN103320124A in Wuhan University of Technology2O2N2:Eu2+Fluorescent powder
Preparation method, wherein M can be obtained and effectively excited within the scope of 300-450nm when being Ba, launch peak wavelength be 490 ±
The blue green light of 2nm actually makes although the fluorescent powder of the chemical composition can effectively be excited by 440-460nm blue chips
With finding in the process, not only luminous efficiency is low for the fluorescent powder, but also poor chemical stability, and the white light LEDs prepared is caused to produce
Product light efficiency is low, and stability is poor, short life.
In height develops the color white light LEDs, generally use blue-ray LED, jaundice green light fluorescent powder and red phosphor three's group
It closes and realizes, but in the combination spectrum can have bluish-green spectrum gap and be difficult to obtain colour rendering index aobvious in 95 or more superelevation
Colour index product usually can supplement bluish-green spectrum in spectrum by the blue chip of overlength wavelength or the green light fluorescent powder that turns blue
Gap.White light LEDs product on the market mainly come excitated fluorescent powder and provides blue light, overlength using 440-460nm blue chips
The blue chip of wavelength not only increases production cost, can also reduce the launching efficiency of fluorescent powder, thus the program generally not by
Using.
Therefore, develop it is a can effectively be excited efficient transmission bluish-green spectral by blue light or purple light, and chemistry is steady
The qualitative superior fluorescent powder of energy is significant.
Invention content
In view of the drawbacks of the prior art, the purpose of the present invention is to provide a kind of performance stabilization, can excitation-emission it is bluish-green
A kind of novel garnet-base high-efficiency fluorescence powder of light and preparation method thereof and luminescent device.Specifically, the solution of the present invention is as follows:
A kind of fluorescent powder, which is characterized in that its chemical general formula is:(Lu3-x-zRz)(Al5-yGay)O12:XCe, wherein R is
Y, one or more elements in La, Tb, Gd and Dy, and 0.01<x<0.03,2.00<y<2.50,0≤z≤1.00, it is described glimmering
Emission peak peak wavelength after light powder is excited is 490-500nm.
The fluorescent powder of the present invention can be excited within the scope of optical wavelength 380-480nm, preferably in 440-460nm blue lights or
It is effectively excited within the scope of 410-440nm purple lights;Further, it is preferable to effectively be excited by 440-460nm blue lights.
In the present invention, " being excited " is understood as the broadest range that fluorescent powder can be excited;" by effectively exciting "
It should be understood as that the preferred excites scope that excites scope reduces, i.e. fluorescent powder are excited in the range with best luminous effect
Rate.
Further, wherein 2.01≤y≤2.45;
Further, preferred 2.05≤y≤2.3.Using the scheme of preferred Ga contents, the present invention is in the transmitting for ensureing fluorescent powder
Peak-to-peak value wavelength also further promotes the stability of fluorescent powder within the scope of 490-500nm.
Further, wherein 0.015≤x≤0.025;Further, preferred 0.018≤x≤0.022.Using preferred side
Case, the present invention ensure phosphor emission peak-to-peak value wavelength can within the scope of 490-500nm it is adjustable, also further ensure that fluorescence
The luminous high efficiency of powder.
Further, in the fluorescent powder R be Y, La, Tb one or more elements.
Further, the z=0 of the fluorescent powder, chemical general formula are:(Lu3-x)(Al5-yGay)O12:xCe。
The present invention also proposes a kind of phosphor mixture comprising aforementioned fluorescent powder with it is other in addition to the fluorescent powder
The mixing of powder or amorphous powder is crystallized, the wherein ratio of aforementioned fluorescent powder is not less than 50wt%, preferably not less than 80wt%.Make
It can be added in fluorescent powder certain for an application of phosphor mixture in order to improve the target practice concentration degree of encapsulating products
The Nano-meter SiO_2 of ratio2Powder is as antiprecipitant;In order to further ensure that light efficiency, preferably Nano-meter SiO_22Powder additive amount accounts for fluorescence
The 10wt% of powder mixture quality.
The present invention also proposes a kind of preparation method of fluorescent powder, includes the following steps:
Step 1, with Lu2O3,Y2O3,La2O3,Tb4O7,Gd2O3,Dy2O3,Al2O3,Ga2O3And CeO2For raw material, according to change
Learn general formula (Lu3-x-zRz)(Al5-yGay)O12:Cationic stoichiometric ratio (i.e. molar percentage) weighs raw material in xCe compositions;
Wherein, one or more elements in R Y, La, Tb, Gd and Dy, 0.01<x<0.03,2.00<y<2.50,0≤z≤1.00;
Step 2, raw material step 1 weighed carries out reduction reaction after mixing, obtains the semi-finished product of fluorescent powder;
Step 3, the semi-finished product of fluorescent powder of the step 2 through reduction reaction are further processed, obtain the fluorescent powder at
Product, it is described to be further processed including broken, cleaning, stoving process.
Further, raw material described in step 1 further includes fluxing agent BaF2And/or BaCl2。
In this preparation method, the reduction reaction of step 2 is to provide activation energy needed for reduction reaction under the high temperature conditions, is promoted
Object is mutually formed and grain growth, is completed at the same time activator Ce4+To Ce3+Transformation.Therefore preferably in reducing atmosphere and 1450-1550
DEG C temperature condition under carry out reduction reaction;Reducing atmosphere can be H2, CO, NO and N2In one or more, but reducing atmosphere
In include at least H2, a kind of gas in CO, NO, further, from the aspect of security performance and reduction effect etc., this hair
Bright preferred hydrogen atmosphere is as reducing atmosphere;
Further, in order to effectively control the speed of growth of crystal grain, grain size morphology controllable is obtained, perfect fluorescence is crystallized
Powder, the present invention are warming up to 1450-1550 DEG C, and roast preferably with the heating rate of 10-20 DEG C/min from room temperature or Current Temperatures
It burns 8-12h and completes the reduction reaction.
Further, it is further processed in step 3 successively including broken, sieving, ball milling, pickling or washing, filtering and baking
Dry technique.The particle being bonded together in sintering process can be broken up by increasing ball-milling technology, obtain the powder of good dispersion.
The present invention further provides a kind of luminescent device, including luminescent diode component and the resin containing fluorescent material, institutes
It states luminescent diode component and sends out the first light, the first described light is purple light or blue light, it is characterised in that:It is described to contain phosphor
The resin of material at least contains the first fluorescent powder, the first described fluorescent powder absorbs the first a part of light and emits second
The emission peak peak wavelength of light, the first fluorescent powder is 490-500nm, and the chemical general formula of the first fluorescent powder is:
(Lu3-x-zRz)(Al5-yGay)O12:XCe, wherein one or more elements in R Y, La, Tb, Gd and Dy, and 0.01<x<
0.03,2.00<y<2.50,0≤z≤1.00.
Further, in the chemical general formula of the first fluorescent powder, wherein 2.01≤y≤2.45, preferably 2.05≤y≤
2.3;Wherein 0.015≤x≤0.025, preferably 0.018≤x≤0.022.
Further, the first described light is 440-460nm blue lights or 410-440nm purple lights.
Further, in the chemical general formula of the first fluorescent powder, R La, Tb one or two kinds of elements.
Further, the chemical general formula of the first fluorescent powder is:(Lu3-x)(Al5-yGay)O12:xCe。
Further, the resin containing fluorescent material also contains second of fluorescent powder, and second of fluorescent powder absorbs
The first a part of light and emit the third light, the emission peak peak wavelength of second of fluorescent powder is 640-660nm, described
The chemical formula general formula of second of fluorescent powder is M(1-a)AlSiN3:AEu, wherein M=Ca or Sr, 0.01≤a≤0.05;Or M(2-b)
Si5N8:BEu, wherein M=Ca or Sr, 0.005≤b≤0.05;Or M(1-c)S:CEu, wherein M=Ca or Sr, 0.01≤c≤
0.05;Or K2V(1-d)F6:dMn4+, wherein V=Si or Ge, 0.01≤d≤0.1.
Further, the resin containing fluorescent material also contains the third fluorescent powder, the third described fluorescent powder absorbs
The first a part of light and emit the 4th kind of light, the emission peak peak wavelength of the third fluorescent powder is 510-600nm, described
The chemical formula of the third fluorescent powder is Y(3-e)Al(5-f)GafO12:ECe, wherein 0.02≤e≤0.08,1.5≤f≤2.2;Or
W(2-g)SiO4:GEu, wherein W=Ba or Sr, 0.005≤g≤0.15;Or La(3-h)Si6N11:HCe, wherein h=0.005≤h
≤0.15。
Further, the first described light is the blue light of 445-455nm, the first described fluorescent powder, second of fluorescent powder
Ratio with the third fluorescent powder is:The first fluorescent powder of 40wt%~60wt%:Second of fluorescent powder of 10wt%~30wt%:
The third fluorescent powder of 20wt%~30wt%, the luminescent device are white light source, and the positive warm colour rendering index of white is more than 95.
YAG(Y3Al5O12) fluorescent powder be industrialized production white light LED major fluorescent powder, in order to make the hair of YAG fluorescent powder
It penetrates peak blue shift and obtains green spectral components, it is existing to use the parts Ga substitution Al and obtain chemical composition as Y3Al5-xGaxO12's
The scheme of yellowish green fluorescent powder, or Lu is used to replace Y completely and obtain chemical composition as Lu3Al5O12Yellowish green fluorescent powder
Scheme.In existing Y3Al5O12In scheme, no matter Al is replaced using the parts Ga or Y, constructed crystalline substance are replaced using Lu completely
Field intensity is appointed so relatively strong, it is difficult to which the emission peak of fluorescent powder is blue shifted to 510nm or shorter.
The present invention is with Ce3+For the Lu of the centre of luminescence3Al5O12In, Al ions are replaced using part Ga, due to the ion of Ga
Ionic radius bigger of the radius compared with Al, after substitution, the lattice constant of fluorescent powder increases, and reduces Ce accordingly3+The crystal of surrounding
Field intensity so that Ce3+Luminous blue shift;Control Ce simultaneously3+Concentration in relatively low range, reduce Ce3+Between ion
The problems such as wavelength caused by cross relaxation is elongated and light emission luminance reduces, maintains higher quantum efficiency.Above-mentioned two
The reason of aspect, makes the present invention while ensureing light emission luminance, and the notable basket of emission wavelength of fluorescent powder moves, most bob ejected wave
Length can reach 490nm.
In order to obtain colour rendering index in 95 or more super white-light LED with high color rendering index product, blue green light in spectrum is made up
Compose gap, the present invention proposes a kind of by blue light or after purple light excited, and emission peak peak wavelength is the optimum chemical of 490-500nm
Composition proposal.
Compared with prior art, remarkable advantage is technical scheme of the present invention:
First, the efficient transmission of specific short wavelength.The present invention improves performance by optimization formula, and obtaining one kind can be by
Blue light or purple light effectively excite, emission peak peak wavelength be 490-500nm shortwave fluorescent powder, and can High Efficiency Luminescence, fill up
The gap of existing bluish-green spectrum so that it can obtain 95 or more superelevation colour rendering index using white light product.
Second, high-temperature thermal stability performance is superior.Currently preferred formula scheme, can promote the high stable of fluorescent powder
Performance.
Third, application field are wide.Fluorescent powder of the present invention can be suitable for due to its excellent luminous efficiency and high stability
Various luminescent devices have expanded the application range of fluorescent powder.
Description of the drawings
Fig. 1:Lu of the present invention2.98(Al2.99Ga2.01)O12:0.02Ce and Lu2.98(Al2.55Ga2.45)O12:The excitation of 0.02Ce
Spectrogram.
Fig. 2:Lu of the present invention2.98(Al2.99Ga2.01)O12:0.02Ce and Lu2.98(Al2.55Ga2.45)O12:The transmitting of 0.02Ce
Spectrogram.
Fig. 3:Lu of the present invention2.98(Al2.95Ga2.05)O12:0.02Ce,Lu2.98(Al2.8Ga2.2)O12:0.02Ce and Lu2.98
(Al2.7Ga2.3)O12:The exciting light spectrogram of 0.02Ce.
Fig. 4:Lu of the present invention2.98(Al2.95Ga2.05)O12:0.02Ce,Lu2.98(Al2.8Ga2.2)O12:0.02Ce and Lu2.98
(Al2.7Ga2.3)O12:The launching light spectrogram of 0.02Ce.
Fig. 5:Lu of the present invention2.98(Al2.8Ga2.2)O12:The XRD diagram of 0.02Ce fluorescent powders.
Fig. 6:Lu of the present invention2.98(Al2.8Ga2.2)O12:0.02Ce fluorescent powders are 520nm's with certain commercially available peak wavelength
Lu3Al5O12The thermal quenching performance comparison figure of fluorescent powder.
Fig. 7:Lu of the present invention2.985(Al2.95Ga2.05)O12:0.015Ce,Lu2.98(Al2.95Ga2.05)O12:0.02Ce and
Lu2.975(Al2.95Ga2.05)O12:The exciting light spectrogram of 0.025Ce.
Fig. 8:Lu of the present invention2.985(Al2.95Ga2.05)O12:0.015Ce,Lu2.98(Al2.95Ga2.05)O12:0.02Ce and
Lu2.975(Al2.95Ga2.05)O12:The launching light spectrogram of 0.025Ce.
Fig. 9:Lu of the present invention2.982(Al2.8Ga2.2)O12:0.018Ce,Lu2.978(Al2.8Ga2.2)O12:The excitation of 0.022Ce
Spectrogram.
Figure 10:Lu of the present invention2.982(Al2.8Ga2.2)O12:0.018Ce,Lu2.978(Al2.8Ga2.2)O12:The transmitting of 0.022Ce
Spectrogram.
Figure 11:Different doping (Lu of the invention3-x-zRz)(Al5-yGay)O12:The exciting light spectrogram of xCe fluorescent powders.
Figure 12:Different doping (Lu of the invention3-x-zRz)(Al5-yGay)O12:The launching light spectrogram of xCe fluorescent powders.
Figure 13:The present invention (Lu2.488La0.5)(Al2.52Ga2.48)O12:0.012Ce,(Lu2.472La0.5)(Al2.52Ga2.48)
O12:The exciting light spectrogram of 0.028Ce.
Figure 14:The present invention (Lu2.488La0.5)(Al2.52Ga2.48)O12:0.012Ce,(Lu2.472La0.5)(Al2.52Ga2.48)
O12:The launching light spectrogram of 0.028Ce.
Figure 15:The launching light spectrogram of the luminescent device of 490-500nm fluorescent powders of the present invention.
Figure 16:The spectrum of the scheme of 490-500nm fluorescent powders cooperation 640-660nm nitride red fluorescent powders of the present invention
Figure.
Figure 17:490-500nm fluorescent powders cooperation 640-660nm nitride red fluorescent powders and 510-600nmYAG of the present invention
The spectrogram of the scheme of fluorescent powder.
Specific implementation mode
The specific implementation mode of the present invention is described in further detail with reference to the accompanying drawings and examples.
Embodiment 1:
The present embodiment 1 proposes a kind of preparation method of fluorescent powder, includes the following steps:
According to the chemical composition of fluorescent powder proposed by the present invention, including Lu2.98(Al2.99Ga2.01)O12:0.02Ce,Lu2.98
(Al2.95Ga2.05)O12:0.02Ce,Lu2.98(Al2.8Ga2.2)O12:0.02Ce,Lu2.98(Al2.7Ga2.3)O12:0.02Ce,Lu2.98
(Al2.55Ga2.45)O12:0.02Ce etc., according to stoichiometric ratio (i.e. molar percentage) cationic in corresponding chemical composition,
Lu is weighed respectively2O3,Al2O3,Ga2O3And CeO2Raw material, the raw material are powder body material, and the purity of the raw material is that chemistry is pure,
With Lu2O3(purity 99.99%), Al2O3(purity 99.99%), Ga2O3(purity 99.99%), CeO2(purity 99.99%) is
It is preferred that;Further, further include fluxing agent BaF in the raw material in the present embodiment 12And/or BaCl2, the fluxing agent is in this implementation
The BaF of raw material gross weight 5.0wt% can be selected to account in example 12With the BaCl of 5.0wt ‰2, the purity of the fluxing agent is chemistry
It is pure, with fluxing agent BaF2(analysis is pure) and/or BaCl2(analysis is pure) is preferred.
Material powder after weighing is placed in mixing tank and carries out batch mixing, specific batch mixing can be that oxygen is added in mixing tank
Change aluminium or zirconia ball, select the diameter of ball 1cm or so or be 1cm-5cm diameters ball mixture, ratio of grinding media to material 1
~1.2:1, it discharges after 1-5h is mixed, preferably incorporation time is 3h.Uniformly mixed material powder is packed into aluminium oxide ceramics
In crucible, and crucible cover is added, is placed in high-temperature hydrogen reduction stove, 1450-1550 is raised to the heating rate of 10-20 DEG C/min
It DEG C is kept the temperature, hot stage soaking time is 8-12 hours;Preferably, 1500 are warming up to 15 DEG C/min in the present embodiment 1
DEG C heat preservation 10h synthesis.
The powder agglomates obtained through high temperature reduction reaction is passed through into broken, sieving, ball milling, pickling (5% salpeter solution) or water
It washes, filters, drying, you can obtain Lu2.98(Al2.99Ga2.01)O12:0.02Ce,Lu2.98(Al2.95Ga2.05)O12:0.02Ce,
Lu2.98(Al2.8Ga2.2)O12:0.02Ce,Lu2.98(Al2.7Ga2.3)O12:0.02Ce and Lu2.98(Al2.55Ga2.45)O12:0.02Ce
Series phosphor powder.
The excitation spectrum of fluorescent powder made from the present embodiment 1 is tested, as shown in figures 1 and 3, excitation spectrum is that fluorescent powder exists
The situation of change of the fluorescence intensity at a certain wavelength measured under the excitation light action of different wave length, that is, different wave length are sharp
Luminous relative efficiency, it is seen that under the excitation light action of about 440nm wavelength, fluorescent powder made from the present embodiment 1 has strongest
Fluorescence intensity;Fig. 2 and Fig. 4 is the emission spectrum of 1 fluorescent powder obtained of this implementation, indicates the exciting light in a certain fixed wave length
Lower distribution situation of the fluorescence intensity at different wave length of effect, that is, in fluorescence the light ingredient of different wave length relative intensity.
The result shows that:Series phosphor powder excitation spectrum made from the present embodiment 1 is similar and its optimum excitation wave is about
440nm or so, emission peak peak wavelength is within the scope of 490-500nm.
To Lu made from the present embodiment 12.98(Al2.8Ga2.2)O12:0.02Ce fluorescent powders carry out XRD detections can referring to Fig. 5
To judge that its crystal structure and group become LuAG fluorescent powders.
Certainly, the series phosphor powder of the present embodiment 1 can also there are many compositions, generally speaking, Lu2.98(Al5-yGay)O12:
0.02Ce preferably satisfies 2.01≤y≤2.45, and the present embodiment 1 is compared and tested for the possibility value of y, more excellent
Selection of land, 2.05≤y≤2.3.
Fig. 6 is Lu made from the present embodiment 12.98(Al2.8Ga2.2)O12:0.02Ce fluorescent powders are with certain commercially available peak wavelength
The Lu of 520nm3Al5O12The thermal quenching performance comparison figure of fluorescent powder.The luminous intensity of fluorescent powder, generally can be with residing temperature liter
It is high and weakens, therefore the high high-temp stability of fluorescent powder is also the key index of its performance of judge.And Lu3Al5O12Yellow green is glimmering
Light powder is widely used because of its superior thermal stability in the high-end product of white light LEDs.From fig. 6 it can be seen that with
The luminous intensity of the raising of temperature, fluorescent powder is being gradually reduced, Lu made from the present embodiment 12.98(Al2.8Ga2.2)O12:
0.02Ce fluorescent powders and Lu3Al5O12Fluorescent powder thermal quenching performance is close, and under 180 DEG C of high temperature, luminous intensity stills remain in
93% or more of luminous intensity at room temperature shows the best Lu of similar hot property3Al5O12The excellent thermal quenching of fluorescent powder
Energy.
Embodiment 2:
Another fluorescent powder and preparation method thereof that the present embodiment 2 proposes, has Lu3-x(Al2.95Ga2.05)O12:XCe's
Composition, wherein it is preferred that x meets:0.015≤x≤0.025, x distinguishes value in the present embodiment 2:0.015,0.02,0.025.Root
It carries out preparing embodiment 2 according to preparation method same as Example 1, obtains Lu3-x(Al2.95Ga2.05)O12:The fluorescence of xCe series
Powder.
Similarly, the excitation spectrum for testing fluorescent powder made from the present embodiment 2, as Fig. 7 is the embodiment of the present invention 2
Lu2.985(Al2.95Ga2.05)O12:0.015Ce,Lu2.98(Al2.95Ga2.05)O12:0.02Ce and Lu2.975
(Al2.95Ga2.05)O12:The exciting light spectrogram of 0.025Ce fluorescent powders, it is seen that under the excitation light action of about 440nm wavelength,
Fluorescent powder made from the present embodiment 2 has strongest fluorescence intensity;Fig. 8 is the emission spectrum of fluorescent powder made from the present embodiment,
Its emission peak peak wavelength is in 490-500nm.
The preferred value of embodiment as a further preference, the x of the present embodiment 2 is 0.018-0.022.
Embodiment 3:
Another fluorescent powder and preparation method thereof that the present embodiment 3 proposes, has Lu3-x(Al2.8Ga2.2)O12:The group of xCe
At x distinguishes value in the present embodiment 3:0.018,0.022.Preparation implementation is carried out using preparation method same as Example 1
Example 3 obtains Lu3-x(Al2.8Ga2.2)O12:XCe fluorescent powders.
The excitation spectrum of fluorescent powder made from the present embodiment 3 is tested, is made as shown in Figure 9 in the exciting light of about 445nm wavelength
Under, fluorescent powder made from embodiment 3 has strongest fluorescence intensity;Figure 10 is the transmitting of fluorescent powder made from the present embodiment 3
Spectrum, emission peak peak wavelength is in 490-500nm.
Embodiment 4:
The invention also discloses the series phosphor powders of another kind composition, wherein using one kind or several in La, Tb, Gd, Dy
Kind element is doped, and replaces part Lu in LuAG series phosphor powders, obtains (Lu3-x-zRz)(Al5-yGay)O12:XCe fluorescent powders,
Wherein, 0≤z≤1.00.
The present embodiment 4 proposes the series phosphor powder and preparation method thereof of another chemical composition, has as shown in table 1 group
At.It is carried out preparing embodiment 4 according to preparation method same as Example 1, obtains (Lu3-x-zRz)(Al5-yGay)O12:XCe systems
The fluorescent powder of row.
Table 1:Difference doping (Lu3-x-zRz)(Al5-yGay)O12:The chemical composition of xCe fluorescent powders
Similarly, the excitation spectrum of fluorescent powder made from the present embodiment 4 is tested, as shown in figure 11, excitation spectrum is fluorescence
The situation of change for the fluorescence intensity at a certain wavelength that powder measures under the excitation light action of different wave length, that is, different wave length
Exciting light relative efficiency, it is seen that under the excitation light action of about 442nm wavelength, the present embodiment 4 be made fluorescent powder have most
Strong fluorescence intensity;Figure 12 is the emission spectrum of fluorescent powder made from the present embodiment 4, indicates the exciting light in a certain fixed wave length
Lower distribution situation of the fluorescence intensity at different wave length of effect, that is, in fluorescence the light ingredient of different wave length relative intensity.
The result shows that:Series phosphor powder excitation spectrum made from the present embodiment 4 is similar and its maximum excitation wavelength is in 442nm
Left and right, emission peak peak wavelength is in 490-500nm.
Embodiment 5:
A kind of fluorescent powder and preparation method thereof that this implementation 5 also proposes has (Lu2.5-xLa0.5)(Al2.52Ga2.48)O12:
The composition of xCe, in the present embodiment x distinguish value:0.012,0.028.Using preparation method system same as Example 1
Standby embodiment 5, can get (Lu2.5-xLa0.5)(Al2.52Ga2.48)O12:XCe fluorescent powders.
The excitation spectrum of fluorescent powder made from the present embodiment 5 is tested, is made as shown in figure 13 in the exciting light of about 439nm wavelength
Under, fluorescent powder made from embodiment 5 has strongest fluorescence intensity;Figure 14 is the transmitting of fluorescent powder made from the present embodiment 5
Spectrum, emission peak peak wavelength is in 490-500nm.
Embodiment 6
Another fluorescent powder and preparation method thereof that the present embodiment proposes, has (Lu2.78Y0.2)(Al2.52Ga2.48)O12:
The composition of 0.02Ce is prepared using preparation method same as Example 1.Fluorescent powder made from the present embodiment 6 is carried out
Test, under the excitation light action of about 445nm wavelength, fluorescent powder made from embodiment have strongest fluorescence intensity, and
Its lower emission spectrum emission peak peak wavelength of 445nm blue lights excitation is in about 498nm.
Embodiment 7:
The present embodiment 7 proposes a kind of blue green light scheme, the fluorescent powder Lu prepared using the present invention2.98(Al2.8Ga2.2)O12:
0.02Ce is synthetically formed the LED product product of glow green under the blue chip excitation of 450-452nm.It is prepared by the present embodiment 7
LED light source, X-coordinate 0.2825, Y coordinate 0.5103, spectrum is as shown in figure 15.
Embodiment 8:
The present embodiment 8 proposes a kind of blue green light scheme, the fluorescent powder Lu prepared using the present invention2.98(Al2.8Ga2.2)O12:
0.02Ce is synthetically formed the LED product of glow green under the purple light chip excitation of 425-427nm.Prepared by the present embodiment 8
LED light source, X-coordinate 0.2278, Y coordinate 0.4782.
Embodiment 9:
The present embodiment 9 proposes a kind of LED white light parts, the packaged type with common LED, including pinned, patch
The packing forms such as formula or COB.The fluorescent powder Lu prepared using the present invention2.98(Al2.8Ga2.2)O12:0.02Ce, collocation is on the market
Common red fluorescence powder (Sr, Ca) AlSiN3:Eu synthesizes colour temperature 6000K under the blue chip excitation of 450-452nm, shows
Colour index is the white light LEDs product more than 80.LED white light sources prepared by the present embodiment 9, colour temperature 6023K, X-coordinate 0.3223,
Y coordinate 0.3375, colour rendering index 82.3, spectrum is as shown in figure 16.
Embodiment 10:
The invention also discloses a kind of LED white light parts, the packaged type with common LED, including pinned, patch
The packing forms such as formula or COB.The fluorescent powder prepared using the present invention, arrange in pairs or groups common on the market red fluorescence powder and yellow green
Fluorescent powder, synthesizes colour temperature 6000K under the blue chip excitation of 450-452nm, and colour rendering index is the white light LEDs production more than 95
Product.LED white light sources prepared by the present embodiment 10, colour temperature 6008K, X-coordinate 0.3233, Y coordinate 0.3369, colour rendering index
96.9, spectrum is as shown in figure 17.
The explanation being not directed in the specific implementation mode of the present invention belongs to technology well known in the art, can refer to known technology
It is implemented.
The present invention achieves satisfied trial effect through validation trial.
The above specific implementation mode and embodiment are to a kind of fluorescent powder proposed by the present invention and preparation method thereof and to shine
The specific support of device technology design, cannot limit protection scope of the present invention with this, every according to technology proposed by the present invention
Design, any equivalent variations done on the basis of the technical program or equivalent change, still fall within technical solution of the present invention
The range of protection.
Claims (19)
1. a kind of fluorescent powder, which is characterized in that its chemical general formula is:(Lu3-x-zRz)(Al5-yGay)O12:XCe, wherein R Y,
One or more elements in La, Tb, Gd and Dy, and 0.01<x<0.03,2.00<y<2.50,0≤z≤1.00, the fluorescence
Emission peak peak wavelength after powder is excited is 490-500nm.
2. a kind of fluorescent powder according to claim 1, it is characterised in that:Wherein 2.01≤y≤2.45.
3. a kind of fluorescent powder according to claim 2, it is characterised in that:Wherein 2.05≤y≤2.3.
4. according to a kind of any fluorescent powders of claim 1-3, it is characterised in that:Wherein 0.015≤x≤0.025.
5. a kind of fluorescent powder according to claim 4, which is characterized in that wherein 0.018≤x≤0.022.
6. a kind of fluorescent powder according to claim 1, it is characterised in that:The fluorescent powder in 440-460nm blue lights or
It is effectively excited within the scope of 410-440nm purple lights.
7. according to a kind of any fluorescent powder of claim 1-3,5-6, it is characterised in that:R is the one or more of Y, La, Tb
Element.
8. according to a kind of any fluorescent powder of claim 1-3,5-6, it is characterised in that:Z=0, chemical general formula are:
(Lu3-x)(Al5-yGay)O12:xCe。
9. a kind of phosphor mixture, which is characterized in that including a kind of fluorescent powder described in claim 1 with remove the fluorescent powder
Except other crystallization powders or amorphous powder mixing, wherein the ratio of the fluorescent powder be not less than 80wt%.
10. a kind of a kind of preparation method of fluorescent powder as described in claim 1, which is characterized in that include the following steps:
Step 1, with Lu2O3,Y2O3,La2O3,Tb4O7,Gd2O3,Dy2O3,Al2O3,Ga2O3And CeO2It is logical according to chemistry for raw material
Formula (Lu3-x-zRz)(Al5-yGay)O12:Cationic stoichiometric ratio weighs raw material in xCe compositions;Wherein, R Y, La, Tb, Gd
With one or more elements in Dy, 0.01<x<0.03,2.00<y<2.50,0≤z≤1.00;
Step 2, the raw material that step 1 weighs is uniformly mixed, carries out reduction reaction, obtains the semi-finished product of fluorescent powder;
Step 3, after further treatment by the semi-finished product of fluorescent powder of the step 2 through reduction reaction, the finished product of the fluorescent powder is obtained,
It is described to be further processed including broken, cleaning, stoving process.
11. a kind of preparation method of fluorescent powder according to claim 10, it is characterised in that:Raw material described in step 1 also wraps
Include fluxing agent BaF2And/or BaCl2。
12. a kind of preparation method of fluorescent powder according to claim 10, it is characterised in that:Reduction reaction is in step 2
It completes in a reducing atmosphere.
13. a kind of preparation method of fluorescent powder according to claim 12, it is characterised in that:In step 2 with 10-20 DEG C/
The heating rate of min completes reduction reaction under conditions of being warming up to 1450-1550 DEG C of roasting 8-12h.
14. a kind of preparation method of fluorescent powder according to claim 12, it is characterised in that:Wherein, into one described in step 2
Step processing includes broken, sieving, ball milling, pickling or washing, filtering and stoving process.
15. a kind of luminescent device, including luminescent diode component and the resin containing fluorescent material, the luminescent diode component hair
Go out the first light, the first described light is purple light or blue light, it is characterised in that:The resin containing fluorescent material at least contains
A kind of fluorescent powder, the first described fluorescent powder absorb the first a part of light and emit second of light, the first described fluorescent powder
Emission peak peak wavelength be 490-500nm, the chemical general formula of the first fluorescent powder is:(Lu3-x-zRz)(Al5-yGay)
O12:XCe, wherein one or more elements in R Y, La, Tb, Gd and Dy, and 0.01<x<0.03,2.00<y<2.50,0≤
z≤1.00。
16. a kind of luminescent device according to claim 15, it is characterised in that:The chemical general formula of the first fluorescent powder
For:(Lu3-x)(Al5-yGay)O12:XCe, wherein 0.018≤x≤0.022,2.05≤y≤2.3.
17. a kind of luminescent device according to claims 14 or 15, it is characterised in that:The resin containing fluorescent material is also
Containing second of fluorescent powder, second of fluorescent powder absorbs the first a part of light and emits the third light, described second
The emission peak peak wavelength of fluorescent powder is 640-660nm, and the chemical formula general formula of second of fluorescent powder is M(1-a)AlSiN3:
AEu, wherein M=Ca or Sr, 0.01≤a≤0.05;Or M(2-b)Si5N8:BEu, wherein M=Ca or Sr, 0.005≤b≤
0.05;Or M(1-c)S:CEu, wherein M=Ca or Sr, 0.01≤c≤0.05;Or K2V(1-d)F6:dMn4+, wherein V=Si or
Ge, 0.01≤d≤0.1.
18. a kind of luminescent device according to claim 17, it is characterised in that:The resin containing fluorescent material also contains
The third fluorescent powder, the third described fluorescent powder absorb the first a part of light and emit the 4th kind of light, the third described fluorescence
The emission peak peak wavelength of powder is 510-600nm, and the chemical general formula is Y(3-e)Al(5-f)GafO12:ECe, wherein 0.02≤e≤
0.08,1.5≤f≤2.2;Or W(2-g)SiO4:GEu, wherein W=Ba or Sr, 0.005≤g≤0.15;Or La(3-h)
Si6N11:HCe, wherein h=0.005≤h≤0.15.
19. a kind of luminescent device according to claim 18, it is characterised in that:The first described light is 445-455nm's
The ratio of blue light, first fluorescent powder, second of fluorescent powder and the third fluorescent powder is:The first fluorescence of 40wt%~60wt%
Powder:Second of fluorescent powder of 10wt%~30wt%:The third fluorescent powder of 20wt%~30wt%, the luminescent device are white light light
Source, the positive warm colour rendering index of white are more than 95.
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