CN106635016A - Phosphor, preparation method thereof and light-emitting device - Google Patents
Phosphor, preparation method thereof and light-emitting device Download PDFInfo
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- CN106635016A CN106635016A CN201611243751.1A CN201611243751A CN106635016A CN 106635016 A CN106635016 A CN 106635016A CN 201611243751 A CN201611243751 A CN 201611243751A CN 106635016 A CN106635016 A CN 106635016A
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- 238000002360 preparation method Methods 0.000 title claims description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title abstract description 15
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 18
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 17
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 9
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 9
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 9
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 9
- 229910052775 Thulium Inorganic materials 0.000 claims abstract description 9
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- 230000005855 radiation Effects 0.000 claims abstract description 9
- 229910052765 Lutetium Inorganic materials 0.000 claims abstract description 8
- 229910052796 boron Inorganic materials 0.000 claims abstract description 8
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 8
- 229910052738 indium Inorganic materials 0.000 claims abstract description 8
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 8
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 6
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 5
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 116
- 239000000203 mixture Substances 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 12
- 229910000765 intermetallic Inorganic materials 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 150000002736 metal compounds Chemical class 0.000 claims 1
- 239000000843 powder Substances 0.000 description 22
- 238000000034 method Methods 0.000 description 12
- 238000001228 spectrum Methods 0.000 description 10
- 241001025261 Neoraja caerulea Species 0.000 description 9
- 238000005245 sintering Methods 0.000 description 7
- 229910000420 cerium oxide Inorganic materials 0.000 description 6
- 238000004737 colorimetric analysis Methods 0.000 description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- 150000002910 rare earth metals Chemical class 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- -1 Carbonate compound Chemical class 0.000 description 3
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- 229910002493 Ce2(CO3)3 Inorganic materials 0.000 description 1
- 229910020187 CeF3 Inorganic materials 0.000 description 1
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 229910017569 La2(CO3)3 Inorganic materials 0.000 description 1
- 229910002226 La2O2 Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910009372 YVO4 Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- NAPFHXCBNVVCGD-UHFFFAOYSA-N carbonic acid;lutetium Chemical compound [Lu].OC(O)=O NAPFHXCBNVVCGD-UHFFFAOYSA-N 0.000 description 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium nitrate Inorganic materials [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 1
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 description 1
- 229910000333 cerium(III) sulfate Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 229910001938 gadolinium oxide Inorganic materials 0.000 description 1
- 229940075613 gadolinium oxide Drugs 0.000 description 1
- SQORATIMOBOFKR-UHFFFAOYSA-H gadolinium(3+);oxalate Chemical compound [Gd+3].[Gd+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O SQORATIMOBOFKR-UHFFFAOYSA-H 0.000 description 1
- RQXZRSYWGRRGCD-UHFFFAOYSA-H gadolinium(3+);tricarbonate Chemical compound [Gd+3].[Gd+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O RQXZRSYWGRRGCD-UHFFFAOYSA-H 0.000 description 1
- ILCLBMDYDXDUJO-UHFFFAOYSA-K gadolinium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Gd+3] ILCLBMDYDXDUJO-UHFFFAOYSA-K 0.000 description 1
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000007970 homogeneous dispersion Substances 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 description 1
- 229960001633 lanthanum carbonate Drugs 0.000 description 1
- OXHNIMPTBAKYRS-UHFFFAOYSA-H lanthanum(3+);oxalate Chemical compound [La+3].[La+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O OXHNIMPTBAKYRS-UHFFFAOYSA-H 0.000 description 1
- YXEUGTSPQFTXTR-UHFFFAOYSA-K lanthanum(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[La+3] YXEUGTSPQFTXTR-UHFFFAOYSA-K 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- YQAQUOLVUCJCHH-UHFFFAOYSA-N lutetium;oxalic acid Chemical compound [Lu].OC(=O)C(O)=O YQAQUOLVUCJCHH-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910001463 metal phosphate Inorganic materials 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- BOTHRHRVFIZTGG-UHFFFAOYSA-K praseodymium(3+);trifluoride Chemical compound F[Pr](F)F BOTHRHRVFIZTGG-UHFFFAOYSA-K 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 1
- 229910052844 willemite Inorganic materials 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
-
- 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
- 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 invention belongs to the field of phosphor and particularly relates to phosphor. The chemical formula of the phosphor is (Al-a-bGdaQb)3M5D12, wherein A is one of Lu and La or a group comprising Lu and La; Q is one of Ce, Nd, Sm, Pr, Dy, Ho, Er and Tm or a group comprising more of Ce, Nd, Sm, Pr, Dy, Ho, Er and Tm; M is one of B, Al, Ga and In or a group comprising more of B, Al, Ga and In; D is one of O, N, S, Cl and For a group comprising more of O, N, S, Cl and F; besides, a is larger than or equal to 0.4 and smaller than or equal to 0.53, and b is larger than or equal to 0.005 and smaller than or equal to 0.469; the phosphor is a crystalline phase crystal. The phosphor has large radiation peak with full width at half maximum and sufficient light-emitting intensity in an area with wavelength longer than yellow light wavelength (about 600 nm-690 nm), so that the phosphor can emit warm white light when a blue light LED is added. The phosphor has high external quantum efficiency, high internal quantum efficiency, high light-emitting efficiency and high absorptivity and can be widely applied to light-emitting devices, display devices or lighting devices.
Description
Technical field
The invention belongs to fluorescent material field, and in particular to one kind be made up of rare earth doped compound fluorescent material and its
Preparation method, and the light-emitting device using the fluorescent material, display device and lighting device.
Background technology
White light emitting diode (Light-emitting diodes, LED) is due to its energy-saving and environmental protection and life-span length etc.
Feature has become illumination of future generation.The method that specifically white light can be obtained from LED includes：(1) red light, green will respectively be launched
Three kinds of LED combinations of light and blue light simultaneously mix these LED lights, and (2) are by the LED of emitting ultraviolet light and by ultraviolet excitation point
Not Fa She red light, green light and blue light fluorescence three kinds of phosphor combinations, and mix three kinds of face of these phosphor emissions
The method of the fluorescence of color, and (3) will launch blue light blue-ray LED and radiate using blue light as exciting light with and blue light
The phosphor combination of the yellow fluorescence of complementary colours, and mix the light and the gold-tinted by phosphor emission of blue-ray LED.
The method for obtaining specific coloured light using multiple LED needs the circuit of the electric current for suitably adjusting single led to reach
The purpose of the different color of balance.Ground is compared, being with the advantage for obtaining specific coloured light with reference to LED and fluorescent material need not be such
The cost of circuit and reduction LED.Therefore, many documents have pointed out various with regard to using concrete as the fluorescent material of light source with LED
Suggestion.
The white light LEDs of commercialization at present mainly excite YAG using blue-ray LED：Ce3+Yellow fluorescent powder, what blue-ray LED sent
Blue light is mixed to form white light with the gold-tinted of phosphor emission.But YAG：Ce3+Red color light component is not enough in the emission spectrum of fluorescent material, this
Cause using single Y AG：Ce3+Fluorescent material cannot obtain low related color temperature (correlated color temperature, CCT
＜ 4500K), height drills the warm white of colour index (color rendering index, CRI ＞ 80), therefore limits it in indoor universal
Application in illumination.
In general, for a problem more than solving, red light fluorescent powder suitably must add in element, with supplement ruddiness into
Point, drill the warm white LED of colour index with height so as to prepare low colour temperature.However, the commercialization ruddiness fluorescence of current better performances
Powder transmitting frequency range is still wide, preparation must be limited in high pressure etc., causes its luminous efficiency low and expensive.
It is therefore desirable for developing a kind of fluorescent material, the fluorescent material contains and compares YAG：Ce3+The more red color light components of fluorescent material, and
There is the spectrum of giving out light that halfwidth is wider, so as to combine to prepare height with blue-ray LED under conditions of red light fluorescent powder is not used
Drill the warm white LED of colour index.
The content of the invention
The purpose of patent of the present invention is and solves the above problems and provide one kind and be made up of rare earth doped compound
Fluorescent material and preparation method, containing containing fluorescent powder composition, the light-emitting device using the fluorescent material, display device and lighting device.
One of present invention purpose ties up to a kind of fluorescent material of offer, and the chemical formula of the fluorescent material is (A1-a-bGdaQb)3M5D12, its
In
A is by one or two groups for constituting in Lu or La；
One or more groups for constituting of Q by Ce, Nd, Sm, Pr, Dy, Ho, Er or Tm；
M is by one or more groups for constituting in B, Al, Ga or In；
D is by one or more groups for constituting in O, N, S, Cl or F；
And 0.4≤a≤0.53,0.005≤b≤0.469；
The fluorescent material is crystalline phase crystal.
Preferably, one or more groups for constituting of the Q by Ce, Pr or Sm.
Preferably, the D is by one or two groups for constituting in O or N.
For example：(Lu1-a-bGdaCeb)3Al5O12、(La1-a-bGdaCeb)3Al5O12、(LukLa1-a-bGdaCeb)3Al5O12, its
In, the scope system of a, b as described above, 0≤k≤0.6.
Preferably, the Q is the group that Ce and Pr is constituted, the element number ratio of the Ce and Pr is p: q；The fluorescence
The chemical formula of powder is (A1-a-p-qGdaCepPrq)3M5D12, 0.4≤a≤0.53,0.005≤p≤0.07,0.001≤q≤0.02.
For example：(Lu1-a-bGdaCepPrq)3Al5O12、(La1-a-bGdaCepPrq)3Al5O12、(LukLa1-a-bGdaCepPrq)3Al5O12, wherein, the scope system of a, p, q as described above, 0≤k≤0.6.
Further, when being excited with the light with 430～460nm wavelength, its coloured light is in standard colorimetric for the fluorescent material
Chromaticity coordinate x and y of system (CIE), respectively 0.420≤x≤0.600,0.400≤y≤0.570.
Specifically, when being excited with the light with 430～460nm wavelength, the wavelength system for radiating peak is the fluorescent material
More than 480nm.Also, the halfwidth at the radiation peak of the fluorescent material is more than 100nm.
The fluorescent material of the present invention has a radiation peak of big halfwidth, and in the region longer than yellow wavelengths (i.e., about
600nm to 690nm) there is enough luminous intensities, thus when blue-ray LED is added, warm white can be sent.
Another object of the present invention ties up to a kind of method for manufacturing fluorescent material of offer, comprising：
It is sintered, raw material to obtain chemical formula as (A under nitrogenous hydrogen mixed atmosphere environment1-a-bGdaQb)3M5D12
Crystalline phase fluorescent material；The raw material includes metallic compound, and the metallic compound is selected from Lu comprising at least one
Or La metallic compounds；The metallic compound is comprising at least one selected from Ce, Nd, Sm, Pr, Dy, Ho, Er or Tm metallization
Compound；The metallic compound is selected from B, Al, Ga or In metallic compound comprising at least one.
Further, the raw material is mixed to form by fluorescent material presoma, the fluorescent material presoma Jing dry types
Pulverizer carries out being ground into particle diameter for 0.1 μm of -30 μm of particle.
Specifically, the metallic compound of the raw material, can include：Metal oxide, metal nitrate compound, metal
Carbonate compound, metal phosphate compounds, metallic acetate compounds, metal oxalate compound, metal fluoride or
The combination of one or more in metal chloride.
In the present invention, the concrete example in Ce sources, such as CeO2、Ce2(SO4)3、Ce2(C2O4)3、Ce2(CO3)3Hydrate,
CeCl3、CeF3、Ce(NO3)3Hydrate, CeN, Ce (OH)4Deng.Wherein it is preferably CeO2、CeN。
The concrete example in La sources, for example, nitridation lanthanum, lanthana, lanthanum nitrate, lanthanum hydroxide, lanthanum oxalate, lanthanum carbonate etc., wherein
Preferably lanthana.
The concrete example in Gd sources, for example, nitrogenize gadolinium, gadolinium oxide, gadolinium nitrate, gadolinium hydroxide, gadolinium oxalate, gadolinium carbonate etc..
The concrete example in Lu sources, for example, nitridation lutetium, luteium oxide, lutecium nitrate, oxalic acid lutetium etc., carbonic acid lutetium.
The concrete example in Al sources, such as AlN, Al2O3, Al, aluminium hydroxide, aluminum nitrate etc..
As the weight average intermediate value (weight average median diameter) of each fluorescent material presoma thing
(D50), preferably more than 0.5 μm, less than 20 μm.Therefore, it can use injecting type in advance according to the species of fluorescent material presoma
The Dry-crushers such as pulverizer are crushed.So as to reach homogeneous dispersion in the mixture that can make each fluorescent material presoma, and
Can improve by the surface area of fluorescent material presoma, therefore improve the solid phase reaction of mixture, the life of impurities phase can be suppressed
Into.Particularly, when fluorescent material precursorses are nitride, from considering for reactivity, preferably use than before other fluorescent material
Become the little nitride of particle diameter of thing.
The further object of the present invention ties up to a kind of light-emitting device of offer, including：First illuminator, the first illuminator institute
The light for sending is blue light or UV；And second illuminator, on one of first illuminator exiting surface.Wherein, described first
Fluorescent material includes at least one above-mentioned fluorescent material.
Specifically, the first illuminator LED chip, semiconductor laser diode, organic electroluminescent device or inorganic
Electroluminescent cell.
Further, the luminous colour system number Ra that drills of first illuminator is more than 80.
Preferably, in the light-emitting device, the second illuminator also includes the second fluorescent material, second fluorescent material is included
At least one fluorescent material different from the radiation spike length of first fluorescent material.
Specifically, if second fluorescent material uses red fluorescence powder, its luminous colour system number Ra that drills can be more than 90.
Specifically, if second fluorescent material is using red fluorescence powder and green emitting phosphor, it is luminous drill colour system number Ra can
More than 95.
The fluorescent material of the present invention is illustrated further, for example, the chemical formula (A of fluorescent material1-a-bGdaRb)3M5D12, when M is Al
When, wherein the Al of whole Al or a part can be replaced into B.When in BN containers add raw material and be sintered with manufacture
During the fluorescent material of the present invention, B can be mixed in resulting fluorescent material, therefore, it is possible to manufacture the fluorescent material replaced with B such as above-mentioned Al.
The fluorescent material of the present invention can send the light of yellow～orange.When being excited with the light for having 430～460nm wavelength, its
Chromaticity coordinate x and y of standard colorimetric system (CIE) is usually：By (0.420,0.400), (0.420,0.570), (0.600,
0.570) and (0.600,0.400) surround region in coordinate.Preferably, by (0.440,0.430), (0.440,
0.530), (0.580,0.530) and (0.580, the coordinate in region for 0.430) surrounding.Therefore, the present invention fluorescence
In the chromaticity coordinate of the fluorescence of powder, chromaticity coordinate x is usually more than 0.420, preferably more than 0.440, and usually 0.600 with
Under, preferably less than 0.580.On the other hand, chromaticity coordinate y is usually more than 0.400, preferably more than 0.430 and is usually
Less than 0.570, preferably less than 0.530.
Fluorescence spectrum (spectrum of the giving out light) system that sends of fluorescent material of the present invention is not particularly limited, but as yellow～orange glimmering
The purposes of body of light, when being excited with the light of 430～460nm of wavelength, the peak luminous wavelength of its spectrum of giving out light can for 480nm with
Upper, preferably more than 560nm and preferably more than 565nm, be more preferably more than 570nm and can for below 680nm, preferably
For below 650nm, more be preferably below 625nm scope.
In the present invention, the external quantum efficiency of fluorescent material can be more than 30%, be preferably more than 35%, is more preferably
More than 40%.The light-emitting component high in order to design luminous intensity, the higher the better for external quantum efficiency.In addition, the fluorescence of the present invention
The internal quantum of powder can be more than 35%, preferably more than 40%, more preferably more than 45%.Herein, Internal Quantum effect
Rate refers to, the ratio of the number of photons of the exciting light that the number of photons and fluorescent material that fluorescent material sends absorbs.Internal quantum is relatively low
When, luminous efficiency is then relatively low.In addition, the absorption efficiency of the fluorescent material of the present invention the higher the better.Its value can for more than 70%, preferably
For more than 75%, more preferably more than 80%.External quantum efficiency is obtained according to the product of internal quantum and absorption efficiency,
In order to have higher external quantum efficiency, high-selenium corn efficiency system is preferable.
In the light-emitting device of the present invention, the first illuminator can be used as the illuminator of the second illuminator for exciting aftermentioned.
Wherein, it is without spy as long as the emission wavelength of the first illuminator is Chong Die with the absorbing wavelength of the second illuminator described later
Do not limit, it is possible to use the illuminator in the emission wavelength region of wide ranges.Preferably using with from ultraviolet region to blue region
The illuminator of the emission wavelength in domain, more preferably using the luminous of the emission wavelength having from black light region to blue region
Body.As the concrete numerical value of the peak luminous wavelength of the first illuminator, it is considered to the excitation of light-emitting device, preferably 430nm～
The illuminator of the peak emission wavelength of 480nm.
As the compound of the first illuminator, preferably with GaN LED or LD of GaN compound semiconductor.It is former
Because compared with the SiC systems LED of the light for sending the region, the luminous power of GaN LED or LD, external quantum efficiency are higher,
Through with above-claimed cpd, can with low-down electrical power become clear very much it is luminous.In GaN LED or LD, preferably
It is with Alx, Gay, N luminescent layers, GaN luminescent layers or Inx, Gay, GaN LED or LD of N luminescent layers.Wherein, the value of x '+y '
It can be 0.8～1.2 scope.In GaN LED, can adulterate in these luminescent layers if the element of Zn, Si is to adjust luminous spy
Property.
Wherein, the sandwich heterojunction structure that the LED is preferably formed with luminescent layer, p layers, n-layer, electrode and substrate.This
Outer first illuminator can only use 1, it is also possible to by more than 2 in any combination with the above-mentioned illuminator of ratio.
The second illuminator in the light-emitting device of the present invention is under the irradiation of the light from above-mentioned first illuminator, can to send out
Go out the illuminator of visible ray.Second illuminator is in the fluorescent material containing above-mentioned offer of the invention as the first fluorescent material, root
According to its purposes, the second aftermentioned fluorescent material, such as orange～red fluorescence powder, green emitting phosphor, blue-fluorescence can be further included
Powder, yellow fluorescent powder etc..In addition, for example, the composition of the second illuminator can be by being scattered in encapsulation by the first and second fluorescent material
In material.
For above-mentioned second illuminator, in addition to the fluorescent material of the present invention, its composition is not particularly limited.Embodiment bag
Be incorporated to compound containing by a crystalline matrix, crystalline matrix for example, Y2O3、YVO4、Zn2SiO4、Y3Al5O12、Sr2SiO4Deng metal oxygen
Compound, Sr2Si5N8Deng metal nitride, Ca5(PO4)3The phosphate of Cl and the sulfide of ZnS, SrS, CaS, Y2O2S、La2O2S
Oxysulfide etc., add again rare earth metal, such as Ce, Pr, Nd, Pm, Sm, Eu, Tb, Dy, Ho, Er, Tm, Yb etc. ion,
And or a metal, the ion of such as Ag, Cu, Au, Al, Mn, Sb etc., to form fluorescence as active element or co-activating element
Powder.
Beneficial effects of the present invention：
(1) fluorescent material of the invention is made up of rare earth doped compound, and the chemical formula of fluorescent material is (A1-a- bGdaQb)3M5D12；The fluorescent material of the present invention has the radiation peak of big halfwidth, and in the region longer than yellow wavelengths
(that is, about 600nm to 690nm) has enough luminous intensities, when blue-ray LED is added, can send warm white.
(2) fluorescent material external quantum efficiency of the invention can be more than 30%, can be used for the high light-emitting component of luminous intensity；
The internal quantum of the fluorescent material of the present invention can be more than 35%, and luminous efficiency is high；The absorptivity of the fluorescent material of the present invention reaches
More than 70%, absorptivity is high.
(3) preparation method of fluorescent material of the invention, fluorescent material presoma Jing Dry-crushers carry out being ground into particle diameter and are
0.1 μm of -30 μm of particle, improves the solid phase reaction of mixture, can suppress the generation of impurities phase.
(4) light-emitting device of the invention, the first illuminator is used as the illuminator for exciting the second aftermentioned illuminator, so as to send out
Go out warm white.
(5) fluorescent material of the invention, can be used for light-emitting device, display device or lighting device, there is provided more ruddiness
Composition, and have the wider spectrum of giving out light of halfwidth, so as to can be under conditions of red light fluorescent powder is not used, with blue-ray LED group
Close to prepare the warm white LED that height drills colour index, therefore can improve that the luminous efficiency caused using red light fluorescent powder is low to ask
Topic, and help reduces cost.
Specific embodiment
Below by way of the method that specific embodiment is used to further illustrate present invention description, it is not intended that of the invention
It is confined to these embodiments.
Embodiment 1
Prepare fluorescent material：Will be containing luteium oxide (Lu2O3), gadolinium oxide (Gd2O3), aluminum oxide (Al2O3) and cerium oxide
(CeO2) etc. compound be well mixed by a predetermined ratio after (incorporation time about 0.5 hour to 24 hours), be filled to earthenware
High temperature sintering reaction is carried out in pot, sintering temperature is that between 1400～1700 DEG C, under nitrogen and hydrogen mixture, sintering 0.5 to 24 is little
When, sintering completed to be down to and take out after room temperature, after grinding in ball grinder, particle diameter is sorted with centrifugal atomizer, obtain
(Lu0.38Gd0.53Ce0.09)3Al5O12Powder.
Embodiment 2
Prepare fluorescent material：Will be containing luteium oxide (Lu2O3), gadolinium oxide (Gd2O3), aluminum oxide (Al2O3), cerium oxide
(CeO2) and praseodymium oxide (Pr2O3) and or (incorporation time is about after the compound such as praseodymium fluoride is well mixed by a predetermined ratio
0.5 hour to 24 hours), being filled in crucible carries out high temperature sintering reaction, and sintering temperature is between 1400～1700 DEG C, in nitrogen
Under hydrogen gaseous mixture, sinter 0.5 to 24 hour, sintering completed to be down to and take out after room temperature, after grinding in ball grinder, so that mist is centrifuged
Change machine sorts particle diameter, obtains (Lu0.38Gd0.53Ce0.07Pr0.02)3Al5O12Powder.
Embodiment 3
Fluorescent material prepared by testing example 1：
D50 particle sizes are determined as 14 μm of its (Lu with spectral fluorometer0.38Gd0.53Ce0.09)3Al5O12Powder.Make to carry out self-excitation
The light of light emitting source is the grating monochromator of 10cm by focal length, then the exciting light of wavelength 460nm is irradiated to into fluorescent material.Fluorescent material
The light Jing focal lengths produced under the irradiation of exciting light are the grating monochromator powder light of 25cm, in the wave-length coverage of 450nm～700nm
The luminous intensity of each wavelength is determined, the spectrum medium wave peak λ p=585nm that give out light of its fluorescence.
The halfwidth at peak of giving out light is calculated by the spectrum of giving out light obtained using said method.
For the measure of the chromaticity coordinate of x, y colorimetry system (the colorimetry systems of CIE 1931), by utilizing said method
The data of the wavelength region of the 450nm～700nm of the spectrum of giving out light for obtaining, in the method based on JIS Z8724, calculates JIS
Chromaticity coordinate x and y in the XYZ colorimetry systems that Z8701 specifies.Obtain its chromaticity coordinate (x, y)=(0.510,0.482).
Embodiment 4
Fluorescent material prepared by testing example 2：
D50 particle sizes are determined as 14 μm of its (Lu with spectral fluorometer0.38Gd0.53Ce0.07Pr0.02)3Al5O12Powder, remaining
Condition is identical with testing example one, and its fluorescence is given out light in spectrum, crest λ p1=585nm, λ p2=610nm, λ p3=
640nm。
The halfwidth at peak of giving out light is calculated by the spectrum of giving out light obtained using said method.
For the measure of the chromaticity coordinate of x, y colorimetry system (the colorimetry systems of CIE 1931), by utilizing said method
The data of the wavelength region of the 450nm～700nm of the spectrum of giving out light for obtaining, in the method based on JIS Z8724, calculates JIS
Chromaticity coordinate x and y in the XYZ colorimetry systems that Z8701 specifies.Obtain its chromaticity coordinate for (x, y)=(0.501,
0.488)。
Such as aforementioned embodiment, it should be appreciated that its purpose is the example present invention, and it is unrestricted.Also, by aforementioned result, because
This, the present invention provides the fluorescent material that is made up of rare earth doped compound and manufacture method, so as to solve prior art it
Problem.
Embodiment 5
A kind of fluorescent material, the chemical formula of the fluorescent material is (A1-a-bGdaQb)3M5D12, wherein A be Lu or La in one kind or
Two kinds of groups for being constituted；One or more groups for constituting of Q by Ce, Nd, Sm, Pr, Dy, Ho, Er or Tm；
M is by one or more groups for constituting in B, Al, Ga or In；
D is by one or more groups for constituting in O, N, S, Cl or F；
And 0.4≤a≤0.53,0.005≤b≤0.469；The fluorescent material is crystalline phase crystal.
Preferably, one or more groups for constituting of the Q by Ce, Pr or Sm.
Preferably, the D is by one or two groups for constituting in O or N.
Further, when being excited with the light with 430～460nm wavelength, its coloured light is in standard colorimetric for the fluorescent material
Chromaticity coordinate x and y of system (CIE), respectively 0.420≤x≤0.600,0.400≤y≤0.570.
Specifically, when being excited with the light with 430～460nm wavelength, the wavelength system for radiating peak is the fluorescent material
More than 480nm.Also, the halfwidth at the radiation peak of the fluorescent material is more than 100nm, in the present invention, the radiation peak half of fluorescent material is high
A width of more than 130nm.
The fluorescent material of the present invention has a radiation peak of big halfwidth, and in the region longer than yellow wavelengths (i.e., about
600nm to 690nm) there is enough luminous intensities, thus when blue-ray LED is added, warm white can be sent.
In the present embodiment, the chemical formula of fluorescent material can be (Lu1-a-bGdaCeb)3Al5O12、(La1-a-bGdaCeb)3Al5O12、
(LukLa1-a-b GdaCeb)3Al5O12, wherein, 0.4≤a≤0.53,0.005≤b≤0.469；0≤k≤0.6.Specific this reality
In applying example, the chemical formula of fluorescent material is (Lu0.38Gd0.53Ce0.09)3Al5O12。
Embodiment 6
A kind of fluorescent material, the chemical formula of the fluorescent material is (A1-a-bGdaQb)3M5D12, wherein A be Lu or La in one kind or
Two kinds of groups for being constituted；One or more groups for constituting of Q by Ce, Nd, Sm, Pr, Dy, Ho, Er or Tm；M is
One or more groups for being constituted in B, Al, Ga or In；
D is by one or more groups for constituting in O, N, S, Cl or F；
And 0.4≤a≤0.53,0.005≤b≤0.469；The fluorescent material is crystalline phase crystal.
Preferably, the D is by one or two groups for constituting in O or N.
Preferably, the Q is the group that Ce and Pr is constituted, the element number ratio of the Ce and Pr is p: q；The fluorescence
The chemical formula of powder is (A1-a-p-qGdaCepPrq)3M5D12, 0.4≤a≤0.53,0.005≤p≤0.07,0.001≤q≤0.02.
The chemical formula of fluorescent material can be (Lu1-a-bGdaCepPrq)3Al5O12、(La1-a-bGdaCepPrq)3Al5O12、
(LukLa1-a-bGdaCepPrq)3Al5O12, wherein, 0.4≤a≤0.53,0.005≤p≤0.07,0.001≤q≤0.02,0≤k
≤0.6.Specifically, the chemical formula of fluorescent material is (Lu in the present embodiment0.38Gd0.53Ce0.07Pr0.02)3Al5O12。
Embodiment 7
Fluorescent material prepared by embodiment 1, embodiment 2 is respectively applied to into light-emitting device.
A kind of light-emitting device, including：
First illuminator, the light that first illuminator sends is blue light or UV；
Second illuminator, on one of first illuminator exiting surface；
Wherein, second illuminator includes the first fluorescent material, and first fluorescent material is comprising at least one chemical formula
(A1-a-bGdaQb)3M5D12Fluorescent material.
Specifically, first fluorescent material be embodiment 1, the fluorescent material prepared by embodiment 2.First illuminator is
LED chip, its luminous colour system number Ra that drills is more than 80.
Specifically, the composition of the second illuminator is by the way that the first fluorescent material is scattered in encapsulating material.
The second illuminator in the light-emitting device of the present invention is under the irradiation of the light from above-mentioned first illuminator, can to send out
Go out the illuminator of visible ray.
Listed above is only the specific embodiment of the present invention, it is clear that the invention is not restricted to the embodiment of the above.This area
The those of ordinary skill's all deformations that can directly derive from present disclosure or associate, all should belong to the present invention's
Protection domain.
Claims (10)
1. a kind of fluorescent material, it is characterised in that the chemical formula of the fluorescent material is (A1-a-bGdaQb)3M5D12, wherein
A is by one or two groups for constituting in Lu or La；
The group that Q is made up of any one or more than one of Ce, Nd, Sm, Pr, Dy, Ho, Er or Tm；
M is by any one in B, Al, Ga or In or more than one groups for constituting；
D is by any one in O, N, S, Cl or F or more than one groups for constituting；
And 0.4≤a≤0.53,0.005≤b≤0.469；
The fluorescent material is crystalline phase crystal.
2. fluorescent material according to claim 1, it is characterised in that the Q for Ce, Pr or Sm any one or it is a kind of
The group that the above is constituted.
3. fluorescent material according to claim 1 and 2, it is characterised in that the D is any one in O or N or two kinds of institutes
The group of composition.
4. fluorescent material according to claim 1, it is characterised in that the Q is the group that Ce and Pr is constituted, the Ce and Pr
Element number ratio be p: q；The chemical formula of the fluorescent material is (A1-a-p-qGdaCepPrq)3M5D12, 0.4≤a≤0.53,0.005
≤ p≤0.07,0.001≤q≤0.02.
5. the preparation method of the fluorescent material described in a kind of any one of claim 1-4, it is characterised in that by raw material, nitrogenous
It is sintered under hydrogen mixed atmosphere environment, to obtain chemical formula as (A1-a-bGdaQb)3M5D12Crystalline phase fluorescent material；The original
Material includes metallic compound, and the metallic compound is selected from Lu or La metallic compounds comprising at least one；The metal
Compound is selected from Ce, Nd, Sm, Pr, Dy, Ho, Er or Tm metallic compound comprising at least one；The metallic compound is included
At least one is selected from B, Al, Ga or In metallic compound.
6. the preparation method of fluorescent material according to claim 5, it is characterised in that the raw material is by fluorescent material presoma
It is mixed to form, the fluorescent material presoma Jing Dry-crushers carry out being ground into particle diameter for 0.1 μm of -30 μm of particle.
7. a kind of light-emitting device, its feature in, including：
First illuminator, the light that first illuminator sends is blue light or UV；
Second illuminator, on one of first illuminator exiting surface；
Wherein, second illuminator includes the first fluorescent material, and first fluorescent material is appointed comprising at least one claim 1-4
Fluorescent material described in one.
8. light-emitting device according to claim 7, it is characterised in that second illuminator also includes the second fluorescent material,
Second fluorescent material includes at least one fluorescent material different from the radiation spike length of first fluorescent material.
9. the light-emitting device according to claim 7 or 8, it is characterised in that first illuminator is LED chip, partly leads
Volumetric laser diode, organic electroluminescent device or inorganic el element.
10. a kind of fluorescent material for being applied to light-emitting device, display device or lighting device, it is characterised in that comprising claim
The fluorescent material of any one of 1-4.
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