CN106554778A - A kind of single-substrate single-doping white luminescent material and preparation method and application - Google Patents
A kind of single-substrate single-doping white luminescent material and preparation method and application Download PDFInfo
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- CN106554778A CN106554778A CN201610879137.8A CN201610879137A CN106554778A CN 106554778 A CN106554778 A CN 106554778A CN 201610879137 A CN201610879137 A CN 201610879137A CN 106554778 A CN106554778 A CN 106554778A
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- 239000000463 material Substances 0.000 title claims abstract description 56
- 239000000758 substrate Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 61
- 239000000126 substance Substances 0.000 claims abstract description 24
- 229910019792 NbO4 Inorganic materials 0.000 claims abstract description 21
- 150000002500 ions Chemical class 0.000 claims abstract description 19
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 8
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 229910052593 corundum Inorganic materials 0.000 claims description 16
- 239000010431 corundum Substances 0.000 claims description 16
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 16
- GEZAXHSNIQTPMM-UHFFFAOYSA-N dysprosium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Dy+3].[Dy+3] GEZAXHSNIQTPMM-UHFFFAOYSA-N 0.000 claims description 16
- 239000004570 mortar (masonry) Substances 0.000 claims description 16
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 238000005245 sintering Methods 0.000 description 28
- 229910003443 lutetium oxide Inorganic materials 0.000 description 14
- 238000010792 warming Methods 0.000 description 14
- 238000000034 method Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 7
- 230000008901 benefit Effects 0.000 description 4
- 238000000295 emission spectrum Methods 0.000 description 4
- 230000005284 excitation Effects 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 230000009102 absorption Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 235000005811 Viola adunca Nutrition 0.000 description 2
- 240000009038 Viola odorata Species 0.000 description 2
- 235000013487 Viola odorata Nutrition 0.000 description 2
- 235000002254 Viola papilionacea Nutrition 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 244000283207 Indigofera tinctoria Species 0.000 description 1
- 244000174681 Michelia champaca Species 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 230000001795 light effect Effects 0.000 description 1
- 238000004020 luminiscence type Methods 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
- 230000008569 process Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- -1 rare earth ion Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
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- 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
- C09K11/7767—Chalcogenides
- C09K11/7769—Oxides
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- H—ELECTRICITY
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a kind of single-substrate single-doping white luminescent material and preparation method and application, its chemical composition expression formula：Lu(1‑x)DyxNbO4, in formula, x is active ions Dy3+With respect to substrate rare earth ion Lu3+The molar content for accounting for, span：0.005≤x≤0.20.The white luminescent material of the present invention belongs to niobates, has more superior physical and chemical stability compared with other compounds；Host material LuNbO4In contain rare earth ion Lu3+, be conducive to Dy3+The doping of ion；Make use of the NbO in substrate4 3‑The effective of group lights, and degree of crystallinity is high, and luminous mass is good.
Description
Technical field
The invention belongs to white light LEDs light-converting material technical field, more particularly, it relates to a kind of single-substrate single-doping is white
Color luminescent material and preparation method and application.
Background technology
White light LEDs have the remarkable advantage such as specular removal, long-life, low energy consumption, pollution-free, with other conventional illumination sources
Incomparable advantage, is applied widely in fields such as illumination, displays.At present, the implementation of white light LEDs mainly have with
Lower three kinds：One is to excite yellow fluorescent powder to form white light using blue chip；Two is to excite RGB using near ultraviolet LED chip
Three primary colours mixed fluorescent powder obtains white light；Three is to fit together red, green and blue LED chip, by the electricity for controlling three primary colours chip
Stream size realizes white light emission.The first in above-mentioned three kinds of methods has been carried out commercialization, but due to lack red fluorescence into
Part, cause color rendering index relatively low；Second method is due to proportioning between different fluorescent material and the resorbent problem of color so that color
Color reduction degree and luminous efficiency are significantly limited；The third method is due to the output voltage and light decay of different chips
Degree is different, designs complex, and such LED chip prices are costly on circuit.In order to overcome three of the above side
The shortcoming of method, searching can obtain the single-substrate single-doping fluorescent material of white light under near ultraviolet excitation becomes study hotspot.
Single-substrate single-doping white emitting fluorescent powder can directly launch white light under the exciting of black light, with other system fluorescence
Powder is compared, and has its outstanding feature：（1）Due to insensitivity of the vision to black light, the color of this kind of white light LEDs is by glimmering
Light is determined, therefore colour stable, and color reducibility is higher；（2）Can avoid causing due to various matrix compounds interphase interactions
Color imbalance, be conducive to improving color rendering propertiess；（3）Due to being single-substrate single-doping compound, resorbent problem can be avoided, is subtracted
Few energy loss, is conducive to improving luminous efficiency；（4）Reduces cost.Therefore, single-substrate single-doping white emitting fluorescent powder recent years
Increasingly paid close attention to by people, the research about this system material is also gradually goed deep into.
In recent years, about the research of single-substrate single-doping white emitting fluorescent powder, the matrix compounds scope being related to is very wide, including
Silicate, phosphate, borate, titanate, vanadate etc..Wherein, rare earth niobates（LnNbO4）Due to good thing
Physicochemical stability, high heat stability and emission conversion efficiency, self-activating centre of luminescence NbO4 3-, and it is easy to rare earth ion
The advantages of doping and be widely used in field of light emitting materials.Dy3+Ion is because of the blue light with feature and yellow emission, Chang Beizuo
For the active ions in single-substrate single-doping white emitting fluorescent powder system.
The content of the invention
The purpose of the present invention is the defect and deficiency for overcoming existing white light LED part, there is provided one kind can be had by black light
Effect is excited, and luminous mass is good, and the stable single-substrate single-doping white luminescent material of physical and chemical performance.
It is a further object to provide the preparation method of above-mentioned single-substrate single-doping white luminescent material.
A further object of the present invention is to provide above-mentioned single-substrate single-doping white luminescent material answering in white light LEDs field
With.
Above-mentioned purpose of the present invention is achieved through the following technical solutions：
A kind of single-substrate single-doping white luminescent material, its chemical composition expression formula：Lu(1-x)DyxNbO4, in formula x for activation from
Sub- Dy3+With respect to substrate rare earth ion Lu3+The molar content for accounting for, span：0.005≤x≤0.20.
Host material selected by the present invention is LuNbO4, active ions are trivalent rare earth dysprosium ion Dy3+.Swash in black light
Give, host emission blue light, Dy3+Launch weaker blue light and stronger gold-tinted in the substrate.By adjusting Dy3+Ion
Doping content, changes the transmitting ratio of blue light and gold-tinted, is capable of achieving white light emission.
Under near ultraviolet excitation of the wavelength for 240 ~ 290 nm, work as Dy3+The molar content of doping be x=
0.005, its luminous chromaticity coordinate value be x=0.251, y=0.191, positioned at blue violet light area；Work as Dy3+Moles the hundred of doping
Point content is 0.01≤x≤0.20, and its luminous chromaticity coordinate value is x=0.280 ~ 0.331, y=0.235 ~
0.302, positioned at white light area.
The preparation method of above-mentioned single-substrate single-doping white luminescent material, comprises the steps：
S1. according to the chemical composition embodied in chemical composition expression formula described in claim 1, raw material is accurately weighed, is fully ground
Mill mix homogeneously, obtains mixture；
S2. by mixture tabletting, it is then placed in reaction vessel, is placed in air atmosphere, heats up and roast in resistance furnace Program
Burn, naturally cool to room temperature；
S3. step S2 products therefrom is taken out and is ground, that is, obtain product.
Wherein, the raw material described in step S1 is：Luteium oxide, dysprosia and niobium oxide.
Preferably, the mix homogeneously that is fully ground described in step S1 is that dehydrated alcohol is added in agate mortar as medium
It is ground mix homogeneously.
Preferably, the tabletting described in step S2 is that tabletting is carried out in cold isostatic press, and mixture obtained by step S1 is existed
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure.
Furthermore it is preferred that reaction vessel described in step S2 is corundum crucible.
Preferably, heating rate described in step S2 is 3-10 DEG C/min.
It is highly preferred that heating rate described in step S2 is 5 DEG C/min.
Preferably, the temperature of roasting described in step S2 is 1150 ~ 1300 DEG C, and the time of roasting is 4-10h.
It is highly preferred that the condition of roasting described in step S2 is 1200 ~ 1250 DEG C, 5 h of roasting.
Most preferably, the condition of roasting described in step S2 is 1220 DEG C, 5 h of roasting.
Application of the above-mentioned single-substrate single-doping white luminescent material in white light LEDs.
A series of materials that said method of the present invention is prepared have similar spectral quality：Have in 240 ~ 290 nm
Very strong wide band absorption, meet near ultraviolet LED chip excite requirement；In the case where 261 nm light are excited, very strong blue light can be obtained
And yellow emission, respectively positioned at 310-550 nm (host emission and Dy3+Ion4F9/2→6H15/2Transition is launched) and 550-600
nm (Dy3+Ion4F9/2→6H13/2Transition is launched), by controlling Dy3+Doping content, it is possible to obtain colourity can in white light area
The white light of tune；It is a kind of white luminescent material that can be applicable to illumination and display white light LEDs.
Compared with prior art, the present invention has the advantages that：
1. the white luminescent material of the present invention belongs to niobates, has more superior physical and chemical stability compared with other compounds；Base
Material LuNbO4In contain rare earth ion Lu3+, be conducive to Dy3+The doping of ion；Make use of the NbO in substrate4 3-Group has
Effect is luminous, and degree of crystallinity is high, and luminous mass is good.
2. substrate can effectively absorb black light, and Dy can be effectively sensitized while its own transmission blue light3+Produce compared with
Weak blue light and stronger yellow emission.Therefore, the luminescent material has the controllability of luminescent chromaticity, controls Dy3+Doping
Concentration, it is possible to obtain colourity is in the adjustable white light in white light area.Dy can be selected according to illumination and the needs of display white light LEDs3+
Doping content, to produce chromaticity coordinates appropriate, high color purity and the suitable white light of colour temperature.
3. the process of preparing of white luminescent material of the present invention is simple, it is easy to accomplish.
Description of the drawings
In Fig. 1, a is the present invention（Embodiment 3）Luminescent material monitoring Dy3+Excitation spectrum during main 576 nm of emission peak,
B is the present invention（Embodiment 3）Emission spectrum of the luminescent material under 261 nm near ultraviolet excitations of matrix absorption peak.
Fig. 2 is the present invention（Embodiment 1,2,3,4,5,7,9,12 and 14）Luminescent material it is closely purple in 261 nm
Outer light excite under emission spectrum, in interior illustration be host emission（Blue light, 394 nm）And Dy3+Ion4F9/2→6H13/2Transition is sent out
Penetrate（Gold-tinted, 576 nm）Relative intensity with Dy3+The changing trend diagram that doping content increases.
Fig. 3 is the present invention（Embodiment 1,2,3,4,5,7,9,12 and 14）Luminescent material it is closely purple in 261 nm
Outer light excite under position view of the chromaticity coordinates in 1931 CIE chromaticity diagrams.
Specific embodiment：
The present invention is further illustrated below in conjunction with Figure of description and specific embodiment, but embodiment is not appointed to the present invention
The restriction of what form.Unless stated otherwise, the reagent for adopting of the invention, method and apparatus are for the art conventional reagent, side
Method and equipment.
Unless stated otherwise, following examples agents useful for same and material are commercial.
Embodiment 1：
Weigh luteium oxide（Lu2O3）0.5939 g, dysprosia（Dy2O3）0.0028 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.995Dy0.005NbO4。
Embodiment 2：
Weigh luteium oxide（Lu2O3）0.5909 g, dysprosia（Dy2O3）0.0056 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.99Dy0.01NbO4。
Embodiment 3：
Weigh luteium oxide（Lu2O3）0.5879 g, dysprosia（Dy2O3）0.0084 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.985Dy0.015NbO4。
Embodiment 4：
Weigh luteium oxide（Lu2O3）0.5850 g, dysprosia（Dy2O3）0.0112 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.98Dy0.02NbO4。
Embodiment 5：
Weigh luteium oxide（Lu2O3）0.5790 g, dysprosia（Dy2O3）0.0168 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.97Dy0.03NbO4。
Embodiment 6：
Weigh luteium oxide（Lu2O3）0.5730 g, dysprosia（Dy2O3）0.0224 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.96Dy0.04NbO4。
Embodiment 7：
Weigh luteium oxide（Lu2O3）0.5671 g, dysprosia（Dy2O3）0.0280 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.95Dy0.05NbO4。
Embodiment 8：
Weigh luteium oxide（Lu2O3）0.5611 g, dysprosia（Dy2O3）0.0336 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.94Dy0.06NbO4。
Embodiment 9：
Weigh luteium oxide（Lu2O3）0.5551 g, dysprosia（Dy2O3）0.0392 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.93Dy0.07NbO4。
Embodiment 10：
Weigh luteium oxide（Lu2O3）0.5491 g, dysprosia（Dy2O3）0.0448 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.92Dy0.08NbO4。
Embodiment 11：
Weigh luteium oxide（Lu2O3）0.5432 g, dysprosia（Dy2O3）0.0504 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.91Dy0.09NbO4。
Embodiment 12：
Weigh luteium oxide（Lu2O3）0.5372 g, dysprosia（Dy2O3）0.0560 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.90Dy0.10NbO4。
Embodiment 13：
Weigh luteium oxide（Lu2O3）0.5074 g, dysprosia（Dy2O3）0.0839 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.85Dy0.15NbO4。
Embodiment 14：
Weigh luteium oxide（Lu2O3）0.4775 g, dysprosia（Dy2O3）0.1119 g, niobium oxide（Nb2O5）0.3987 g, Yu Ma
In Nao mortars, add dehydrated alcohol as medium, be fully ground and mix homogeneously；Mixture is placed in cold isostatic press
The slice of cylinder of a diameter of 12.5 mm and high about 5 mm is pressed under 150 MPa pressure；Material piece is placed in corundum crucible,
In air atmosphere, in resistance furnace being warming up to 1220 DEG C with the speed of 5 DEG C/min carries out second stage sintering, and sintering time is
5h, naturally cools to room temperature；Sample is taken out and is ground, finally give product, its chemical composition expression formula is：
Lu0.8Dy0.2NbO4。
Test experiments：
For testing spectral quality of series material prepared by above-described embodiment 1-14 etc., as a result show, according to institute of the present invention
It is a series of with variable concentrations that the preparation method stated is obtained（As molar content x, span be 0.005≤x≤
0.20）Dy3+The LuNbO of doping4: xDy3+Luminescent material（Embodiment 1-14）With similar spectral quality.
And the explorative experiment of the present invention also show, in the preparation process of the series material, add during grinding anhydrous
Ethanol is conducive to raw material mix homogeneously as medium；Optimum pressure during tabletting is controlled in 150 MPa；Optimum temperature rise rate controlled
In 5 DEG C/min, optimal roasting condition is 1220 DEG C of 5 h of roasting.
By taking material prepared by embodiment 3 as an example, luminosity of the explanation according to material prepared by the method for the present invention is presented,
It is shown in Figure 1.It is observed that：In monitoring Dy3+The excitation spectrum of luminescent material is measured during main 576 nm of emission peak（A in Fig. 1）
In, Lu(1-x)DyxNbO4(0.005≤x≤0.20) serial emission material is near ultraviolet band（240 - 290 nm）There is strong broadband
Absorb, the absworption peak in the range of 300-500 nm is then derived from Dy3+The f-f transition absorptions of ion, show that the material can be expired
Sufficient near ultraviolet LED chip excites requirement.Emission spectrum under 261 nm near ultraviolet excitations（B in Fig. 1）In, there is strong indigo plant
Light and yellow emission, respectively positioned at 310-550 nm (host emission and Dy3+Ion4F9/2→6H15/2Transition is launched) and 550-
600 nm (Dy3+Ion4F9/2→6H13/2Transition is launched), champac light ratio is adjusted, after being combined, high-brightness white-light can be produced.
Lu(1-x)DyxNbO4The emission spectrum of (0.005≤x≤0.20) serial emission material with embodiment 1,2,3,4,
5,7,9,12 and 14 is shown in Figure 2 to represent.It is observed that：With Dy3+The rising of doping content, the blue light of substrate are sent out
Penetrate and gradually weaken, Dy3+Blue light and yellow emission first strengthen, doping content be x=0.015 when reach maximum, afterwards because
Give birth to concentration quenching and gradually weaken so that the transmitting ratio of blue light and gold-tinted is with Dy3+The increase of doping content changes, so as to
Realize photochromic adjustable.
Lu(1-x)PrxNbO4The chromaticity coordinates of (0.001≤x≤0.10) serial emission material is in 1931 CIE chromaticity diagrams
Position is shown in Figure 3.It is observed that：Work as Dy3+The molar content of doping be x=0.005, its luminous chromaticity coordinate value
For x=0.251, y=0.191, positioned at blue violet light area；Work as Dy3+The molar content of doping is 0.01≤x≤0.20, its
The chromaticity coordinate value of light be x=0.280 ~ 0.331, y=0.235 ~ 0.302, positioned at white light area, and with Dy3+Doping
The increase of amount gradually changes light normal complexion colour temperature, is a kind of white light phosphor of new single-substrate single-doping.
Claims (9)
1. a kind of single-substrate single-doping white luminescent material, it is characterised in that：Chemical composition expression is：Lu(1-x)DyxNbO4,
In formula, x is active ions Dy3+With respect to substrate rare earth ion Lu3+The molar content for accounting for, span：0.005≤x≤
0.20。
2. the preparation method of single-substrate single-doping white luminescent material described in claim 1, it is characterised in that comprise the steps：
S1. according to the chemical composition embodied in above-mentioned chemical composition expression formula, raw material is accurately weighed, is fully ground mixing equal
It is even, obtain mixture；
S2. by mixture tabletting, it is then placed in reaction vessel, is placed in air atmosphere, heats up and roast in resistance furnace Program
Burn, naturally cool to room temperature；
S3. step S2 products therefrom is taken out and is ground, that is, obtain product.
3. preparation method according to claim 2, it is characterised in that the raw material described in step S1 is：Luteium oxide, dysprosia
And niobium oxide.
4. preparation method according to claim 2, it is characterised in that described in step S1 be fully ground mix homogeneously be in
Dehydrated alcohol is added to be ground mix homogeneously as medium in agate mortar.
5. preparation method according to claim 2, it is characterised in that the tabletting described in step S2 is in cold isostatic press
Tabletting is carried out, mixture obtained by step S1 is pressed into into the cylinder of a diameter of 12.5 mm and high 5 mm under 150 MPa pressure
Piece.
6. preparation method according to claim 2, it is characterised in that the reaction vessel described in step S2 is corundum crucible.
7. preparation method according to claim 2, it is characterised in that the heating rate described in step S2 is 3-10 DEG C/
min。
8. preparation method according to claim 2, it is characterised in that the temperature of roasting described in step S2 is 1150 ~ 1300
DEG C, the time of roasting is 4-10h.
9. application of the single-substrate single-doping white luminescent material described in claim 1 in white light LEDs.
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