CN106905969A - In fluorescent material, the preparation method and application of near ultraviolet excitated lower transmitting gold-tinted - Google Patents
In fluorescent material, the preparation method and application of near ultraviolet excitated lower transmitting gold-tinted Download PDFInfo
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- CN106905969A CN106905969A CN201710196169.2A CN201710196169A CN106905969A CN 106905969 A CN106905969 A CN 106905969A CN 201710196169 A CN201710196169 A CN 201710196169A CN 106905969 A CN106905969 A CN 106905969A
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- 239000000463 material Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000011575 calcium Substances 0.000 claims abstract description 29
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 29
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000126 substance Substances 0.000 claims abstract description 15
- 230000005284 excitation Effects 0.000 claims abstract description 8
- 238000006467 substitution reaction Methods 0.000 claims abstract description 3
- 239000010955 niobium Substances 0.000 claims description 67
- 239000010936 titanium Substances 0.000 claims description 59
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 42
- 238000001354 calcination Methods 0.000 claims description 41
- 150000001875 compounds Chemical class 0.000 claims description 39
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 31
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 24
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 16
- 229910002651 NO3 Inorganic materials 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 235000006408 oxalic acid Nutrition 0.000 claims description 14
- 229960000583 acetic acid Drugs 0.000 claims description 12
- 239000012362 glacial acetic acid Substances 0.000 claims description 12
- 229910052758 niobium Inorganic materials 0.000 claims description 12
- -1 niobium ion Chemical class 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 11
- 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 11
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims description 11
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 claims description 10
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 10
- WPCMRGJTLPITMF-UHFFFAOYSA-I niobium(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Nb+5] WPCMRGJTLPITMF-UHFFFAOYSA-I 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- QXPQVUQBEBHHQP-UHFFFAOYSA-N 5,6,7,8-tetrahydro-[1]benzothiolo[2,3-d]pyrimidin-4-amine Chemical compound C1CCCC2=C1SC1=C2C(N)=NC=N1 QXPQVUQBEBHHQP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 239000000292 calcium oxide Substances 0.000 claims description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 6
- 239000001110 calcium chloride Substances 0.000 claims description 6
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 6
- 239000004408 titanium dioxide Substances 0.000 claims description 6
- 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 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000008139 complexing agent Substances 0.000 claims description 4
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 claims description 4
- 229910019804 NbCl5 Inorganic materials 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 238000005286 illumination Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 238000004134 energy conservation Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000009877 rendering Methods 0.000 abstract description 3
- 229910000530 Gallium indium arsenide Inorganic materials 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- 229910052761 rare earth metal Inorganic materials 0.000 abstract 1
- 150000002910 rare earth metals Chemical group 0.000 abstract 1
- 230000006641 stabilisation Effects 0.000 abstract 1
- 238000011105 stabilization Methods 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 description 10
- 230000004913 activation Effects 0.000 description 8
- 238000000695 excitation spectrum Methods 0.000 description 7
- 238000012544 monitoring process Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 2
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000001073 sample cooling Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 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
- C09K11/7701—Chalogenides
- C09K11/7703—Chalogenides with alkaline earth metals
-
- 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
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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 invention discloses a kind of fluorescent material, preparation method and application near ultraviolet excitated lower transmitting gold-tinted, materials chemistry formula is：Ca5‑5xDy5xNb4Ti3O21；Wherein x is rare earth dysprosium ion Dy3+Substitution calcium ion Ca2+Mol ratio, and 0.0001≤x≤0.20.In the near ultraviolet region that exciting light is 350 420 nanometers, emission peak is located at the gold-tinted of 574 rans to yellow fluorescent material of the present invention, and its luminous chromaticity coordinate value is x=0.490 0.505, y=0.490 0.485；The near ultraviolet semiconductor chips such as excitation wavelength and InAlGaN, InGaAs are matched very much, can be used as the yellow color component in multiple bases energy-conservation fluorescence light source LED and WLED, with modulated light source colour temperature and colour rendering index is improved, in can be also used for other the various lighting apparatus by ultraviolet excitation.Its physical and chemical performance stabilization, luminous efficiency is high, nontoxic, nuisanceless；Preparation method is simply easily operated, is directly calcined in atmosphere, low cost, without any pollution, is suitable to industrialized production.
Description
Technical field
The present invention relates to a kind of fluorescent material, preparation method and application near ultraviolet excitated lower transmitting gold-tinted, belong to hair
Luminescent material and display technology field.
Background technology
White light LEDs are emerging green lighting techniques, with powerful development potentiality.With incandescent lamp compared with fluorescent lamp,
White light LEDs have the advantages that small volume, energy-conservation, long lifespan, environmental protection, prepare it is easy.White light is mixed by multiple color
Light, the white LEDs for now using are mainly and mix red fluorescence powder with yellow fluorescent powder, and are combined with InGaN blue chips
To the required white light of people.
Although having been developed that some yellow fluorescent powders at present, major part is swashed under ultraviolet (less than 365 nanometers)
Hair, it is mismatched with blue chip (excitation area is typically at 380-470 nanometers) so answering in stably can not meeting WLEDs
With demand, therefore the yellow fluorescent powder that can be effectively excited by black light at this stage is fewer, and stability and luminous efficiency are not
Height, causes that colour rendering index is relatively low, tone is colder, and common fluorescent material can also produce sulfide etc. to have under uv irradiation in addition
Poisonous gas, cause harm to environment, and the cost that it makes trouble, producing process spends is also higher.Therefore the good Huang of performance is studied
Color fluorescent material not only has certain theory significance, with more important practical application meaning.
The content of the invention
For the problem that above-mentioned prior art is present, first purpose of the invention is to provide one kind can be by black light
Effectively excite, the fluorescent material of good stability, luminous mass transmitting gold-tinted high and free of contamination, another object of the present invention is to
There is provided the preparation method of above-mentioned fluorescent material, it is ensured that simple to operate, low cost and favorable repeatability, third object of the present invention
It is the application that above-mentioned fluorescent material is provided.
It is that to object above, the technical solution adopted by the present invention is：A kind of fluorescence near ultraviolet excitated lower transmitting gold-tinted
Material, its chemical composition formula is：Ca5-5xDy5xNb4Ti3O21, wherein x is dysprosium ion Dy3+Substitution calcium ion Ca2+Mol ratio,
And 0.0001≤x≤0.20.
Present invention also offers a kind of preparation method of the above-mentioned fluorescent material near ultraviolet excitated lower transmitting gold-tinted, including
Following steps：
(1) by formula Ca5-5xDy5xNb4Ti3O21, the stoichiometric proportion of corresponding element is weighed and contained in 0.0001≤x≤0.20
There is calcium ion Ca2+Compound, contain dysprosium ion Dy3+Compound, contain niobium ion Nb5+Compound, contain titanium ion
Ti4+Compound as the raw material for preparing, the raw material that will be weighed grinds respectively, is well mixed；
(2) mixture for obtaining step (1) is pre-sintered 1~2 time in air atmosphere, and sintering temperature is 900~1200
DEG C, sintering time is 1~10 hour；
(3) by after the mixture natural cooling of step (2), grinding is uniform, is calcined in air atmosphere, and calcining heat is
1200~1400 DEG C, calcination time is 1~15 hour, you can obtain a kind of yellow fluorescent material.
In this method, calcium ions Ca2+Compound be calcium carbonate CaCO3, calcium chloride CaCl2, calcium nitrate Ca (NO3)2、
One kind in calcium oxide CaO；Described contains dysprosium ion Dy3+Compound be dysprosia Dy2O3, dysprosium nitrate Dy (NO3)3·
6H2One kind in O；Described contains niobium ion Nb5+Compound be niobium pentaoxide Nb2O5, columbium pentachloride NbCl5In one
Kind；Described contains titanium ion Ti4+Compound be titanium dioxide TiO2。
Preferably, the calcining heat of step (3) is 1250~1350 DEG C, and calcination time is 5~8 hours.
Present invention also offers another kind the fluorescent material of near ultraviolet excitated lower transmitting gold-tinted preparation method, including such as
Lower step：
(1) by chemical formula Ca5-5xDy5xNb4Ti3O21, the stoichiometric proportion of each element in 0.0001≤x≤0.20, respectively
Weigh：Contain calcium ion Ca2+Compound, contain dysprosium ion Dy3+Compound, contain niobium ion Nb5+Compound, contain
Titanium ion Ti4+Compound be prepare raw material；
(2) step (1) is contained into calcium ion Ca2+Compound, contain dysprosium ion Dy3+Compound, contain niobium ion Nb5+
Compound be dissolved separately in deionized water or in nitric acid and with deionized water dilute, titanium ion Ti will be contained4+Chemical combination
Thing mixes and is dissolved into glacial acetic acid and then is added drop-wise in ethanol again, and between 2-4, stirring forms vitreosol to regulation pH value；
Ion mole 1.5 is separately added among various solution again to 2 times of complexing agent, described complexing agent is in citric acid, oxalic acid
One kind, respectively obtain and contain calcium ion Ca2+, dysprosium ion Dy3+, niobium ion Nb5+, titanium ion Ti4+Solution；
(3) above-mentioned solution is mixed, temperature stands, dries to be stirred 1~5 hour under conditions of 50~100 DEG C, obtains
Fluffy presoma；
(4) the presoma precalcining in air atmosphere for obtaining step (3), temperature be 400~750 DEG C, the time be 1~
10 hours；
(5) after the product natural cooling of step (4) precalcining, grind and be well mixed, calcined in air atmosphere, calcining
Temperature is 1100~1300 DEG C, and calcination time is 1~10 hour, obtains yellow fluorescent powder.
Preferably, the calcining heat of step (5) is 1150~1250 DEG C, and calcination time is 3~6 hours.
In such scheme, described calcium ions Ca2+Compound be calcium carbonate CaCO3, calcium nitrate Ca (NO3)2In one
Kind；Described contains dysprosium ion Dy3+Compound be dysprosia Dy2O3, dysprosium nitrate Dy (NO3)3·6H2One kind in O；It is described
Contain niobium ion Nb5+Compound be niobium hydroxide Nb (OH)5；The described compound containing titanium elements is butyl titanate
C16H36O4Ti, the butyl titanate is 1 with the mol ratio of ethanol, glacial acetic acid：10：1.
The present invention finally provides the application of the above-mentioned fluorescent material near ultraviolet excitated lower transmitting gold-tinted, the fluorescence
Material launches the gold-tinted of 574 rans under 350-420 nanometers of excitation, and it is sharp that can prepare with black light
The illumination of light emitting source or display device, can also mix it with red fluorescence powder, and are combined with InGaN blue chips and obtain sending out
Go out the LED of warm white.
Compared with the prior art, the advantage of technical solution of the present invention is：
(1) fluorescent material of the invention has effective light absorbs near ultraviolet region, is 350-420 nanometers in exciting light
Near ultraviolet region in, emission peak be located at 574 rans gold-tinted, its luminous chromaticity coordinate value be x=0.490-
0.505, y=0.490-0.485；The near ultraviolet semiconductor chips such as excitation wavelength and InAlGaN, InGaAs are matched very much, can be used
Make the yellow color component in multiple bases energy-conservation fluorescence light source LED and WLED, with modulated light source colour temperature and improve colour rendering index, can be with
For in other the various lighting apparatus by ultraviolet excitation.
(2) the dysprosium ion Dy of present invention application3+4f energy levels easily cleaved in crystalline field, and there is pole to crystalline field
Its big dependence, the 4f energy levels of division are influenceed by crystalline field is very big, so that different, abundant luminescent transitions are produced,
Dysprosium ion Dy3+4f energy levels resonance efficiency it is relatively low, so to realize the luminous, it is necessary to match suitable matrix material of dysprosium ion
Material, so as to realize the abundant splitting of energy level, or host material is to dysprosium ion Dy3+Energy transmission；The present invention is by dysprosium ion Dy3 +It is fused to matrix Ca5Nb4Ti3O21In, the yellow fluorescent powder crystallinity for obtaining is high, and matrix stablizes corrosion-resistant, and transmitting gold-tinted
Efficiency high, colourity is pure；The matrix of use is pollution-free, and harmful substance will not be also produced under irradiation.
(3) the yellow fluorescent material preparation process is simple that the present invention is provided is easily operated, and method safety is controllable, to production bar
Part and equipment requirement be not high, low cost, without any pollution, is suitable to industrialized production.
Brief description of the drawings
Fig. 1 prepares material C a by the present embodiment 14.25Dy0.75Nb4Ti3O21X ray diffracting spectrum；
Fig. 2 prepares sample Ca by the embodiment of the present invention 14.25Dy0.75Nb4Ti3O21Scanning electron microscopy spectrum；
Fig. 3 presses the material C a of the technical scheme of the present embodiment 1 preparation4.25Dy0.75Nb4Ti3O21In monitoring gold-tinted, 574 nanometers obtain
The excitation spectrum for arriving；
Fig. 4 presses the material C a of the technical scheme of the present embodiment 1 preparation4.25Dy0.75Nb4Ti3O21In black light, 388 nanometers are swashed
Give the luminous collection of illustrative plates for obtaining；
Fig. 5 presses the material C a of the technical scheme of the present embodiment 1 preparation4.25Dy0.75Nb4Ti3O21In black light, 388 nanometers are swashed
Give the luminescent lifetime spectrogram that 574 nano wave lengths of monitoring are obtained；
Fig. 6 prepares material C a by the present embodiment 54.75Dy0.25Nb4Ti3O21X ray diffracting spectrum；
Fig. 7 prepares sample Ca by the embodiment of the present invention 54.75Dy0.25Nb4Ti3O21Scanning electron microscopy spectrum；
Fig. 8 presses the material C a of the technical scheme of the present embodiment 5 preparation4.75Dy0.25Nb4Ti3O21In black light, 388 nanometers are swashed
Give the luminous collection of illustrative plates for obtaining；
Fig. 9 presses the material C a of the technical scheme of the present embodiment 5 preparation4.75Dy0.25Nb4Ti3O21In monitoring gold-tinted, 574 nanometers obtain
The exciting light spectrogram for arriving；
Figure 10 presses the material C a of the technical scheme of the present embodiment 5 preparation4.75Dy0.25Nb4Ti3O21In black light, 388 nanometers are swashed
Give the luminescent lifetime spectrogram that 574 nano wave lengths of monitoring are obtained.
Specific embodiment
Technical solution of the present invention is further described with reference to the accompanying drawings and examples.
Embodiment 1:
According to chemical formula Ca4.25Dy0.75Nb4Ti3O21The stoichiometric proportion of middle each element, weighs calcium carbonate CaCO respectively3:
2.1250 grams；Dysprosia Dy2O3:0.6995 gram；Niobium pentaoxide Nb2O5:2.6580 grams；Titanium dioxide TiO2:1.1981 grams are
The raw material of preparation, the raw material that will be weighed grinds respectively, is well mixed；The mixture for obtaining first time pre-burning in air atmosphere
Knot, pre-sintering temperature is 900 DEG C, and the time is 10 hours；It is pre- in air atmosphere for the second time after sample grinding uniformly after cooling
Sintering, pre-sintering temperature is 1200 DEG C, and the pre-sintered time is 1 hour；Ground and mixed is uniform after sample cooling, finally in air gas
Calcined under atmosphere, calcining heat is 1400 DEG C, and calcination time is 1 hour, obtains trivalent dysprosium ion Dy3+The yellow fluorescent powder of activation.
It is the material C a prepared by the present embodiment technical scheme referring to accompanying drawing 14.25Dy0.75Nb4Ti3O21X-ray diffraction
Collection of illustrative plates, experiment confirms that the material of gained is pure phase, the Ca with PDF card numberings 31-02915Nb4Ti3O21Correspondence, does not have impurity
Thing phase；
It is the material C a prepared by embodiment of the present invention technical scheme referring to accompanying drawing 24.25Dy0.75Nb4Ti3O21Scanning electricity
The micro- collection of illustrative plates of son, shows gained sample particle better crystallinity degree in figure；
It is the material C a prepared by the present embodiment technical scheme referring to accompanying drawing 34.25Dy0.75Nb4Ti3O21In monitoring gold-tinted
The exciting light spectrogram obtained under 574 nanometers, it can be seen that luminous excites source main at 388 nanometers, can be well matched with
The light that near ultraviolet diode chip for backlight unit sends；
It is the material C a prepared by the present embodiment technical scheme referring to accompanying drawing 44.25Dy0.75Nb4Ti3O21In black light 388
Nanometer excites down the luminous collection of illustrative plates for obtaining, it can be seen that the material mainly lights in yellow band, and the centre of luminescence is located at 574 nanometers
Left and right.
The material C a of the present embodiment technical scheme preparation is pressed referring to accompanying drawing 54.25Dy0.75Nb4Ti3O21Received in black light 388
The luminescent lifetime spectrogram that 574 nano wave lengths are obtained is monitored under meter Ji Fa, the Yellow luminous life-span is can be calculated for 0.25 millisecond.
Embodiment 2:
According to chemical formula Ca4.995Dy0.005Nb4Ti3O21The stoichiometric proportion of middle each element, weighs calcium chloride respectively
CaCl2::2.7722 grams；Dysprosium nitrate Dy (NO3)3·6H2O:0.0115 gram；Columbium pentachloride NbCl5:5.4000 grams；Titanium dioxide
TiO2:1.1981 grams is the raw material for preparing, and the raw material that will be weighed grinds respectively, is well mixed；The mixture for obtaining is in air gas
Pre-sintered under atmosphere, pre-sintering temperature is 1100 DEG C, and the pre-sintered time is 5 hours；Sintered sample grinding is uniform, in air gas
Calcined under atmosphere, calcining heat is 1200 DEG C, and calcination time is 15 hours, obtains a kind of trivalent dysprosium ion Dy3+The yellow of activation is glimmering
Light powder.
The main structural behaviour of sample, excitation spectrum, luminescent spectrum and luminescent lifetime spectrogram are similar to Example 1.
Embodiment 3:
According to chemical formula Ca4DyNb4Ti3O21The stoichiometric proportion of middle each element, weighs calcium oxide CaO respectively:1.1200
Gram；Dysprosia Dy2O3:0.9328 gram；Niobium pentaoxide Nb2O5:2.6580 grams；Titanium dioxide TiO2:1.1981 grams is preparation
Raw material, the raw material that will be weighed grinds respectively, is well mixed；The mixture for obtaining is pre-sintered in air atmosphere, pre-sintering temperature
It it is 1000 DEG C, the pre-sintered time is 8 hours；Sintered sample grinding is uniform, calcines in air atmosphere again, calcining heat
It it is 1250 DEG C, calcination time is 8 hours, obtains a kind of trivalent dysprosium ion Dy3+The yellow fluorescent powder of activation.
The main structural behaviour of sample, excitation spectrum, luminescent spectrum and luminescent lifetime spectrogram are similar to Example 1.
Embodiment 4:
According to chemical formula Ca4.5Dy0.5Nb4Ti3O21The stoichiometric proportion of middle each element, weighs calcium oxide CaO respectively:
1.2600 grams；Dysprosia Dy2O3:0.4664 gram；Niobium pentaoxide Nb2O5:2.6580 grams；Titanium dioxide TiO2:1.1981 grams；Will
The raw material for weighing grinds respectively, is well mixed；The mixture for obtaining is pre-sintered in air atmosphere, and pre-sintering temperature is 1150
DEG C, the pre-sintered time is 6 hours；The sample grinding that pre-sintering is crossed is uniform, calcines in air atmosphere, and calcining heat is 1350
DEG C, calcination time is 5 hours, obtains a kind of trivalent dysprosium ion Dy3+The yellow fluorescent powder of activation.
The main structural behaviour of sample, excitation spectrum, luminescent spectrum and luminescent lifetime spectrogram are similar to Example 1.
Embodiment 5:
According to chemical formula Ca4.75Dy0.25Nb4Ti3O21The stoichiometric proportion of middle each element, weighs calcium nitrate Ca respectively
(NO3)2:1.9487 grams；Dysprosium nitrate Dy (NO3)3·6H2O:0.2854 gram；Niobium hydroxide Nb (OH)5:1.7790 grams；The fourth of metatitanic acid four
Ester C16H36O4Ti:2.5500 grams used as raw material.By calcium nitrate Ca (NO3)2It is dissolved in deionized water, the lemon of 3.4225 grams of addition
Acid, stirring is until fully transparent；By dysprosium nitrate Dy (NO3)3·6H2O is dissolved in deionized water, adds 0.1801 gram of citric acid,
Stirring is until fully transparent；By niobium hydroxide Nb (OH)5It is placed in deionized water, the citric acid of 2.8821 grams of addition, stirring is straight
It is extremely fully transparent；By butyl titanate C16H36O4Ti and glacial acetic acid are mixed, and are then added drop-wise in ethanol again, addition 2.1616
Gram citric acid, regulation pH value is 2, and stirring forms vitreosol, butyl titanate used and ethanol, the mol ratio of glacial acetic acid
It is 1：10：1.
Above-mentioned solution is mixed, is stirred 5 hours under conditions of being 50 DEG C in temperature, stood, dry, obtain fluffy forerunner
Body；The presoma that will be obtained is calcined in air atmosphere, and calcining heat is 750 DEG C, and calcination time is 1 hour；What is obtained is pre-calcined
The product of burning, after natural cooling, grinds and is well mixed, and is calcined in air atmosphere, and calcining heat is 1300 DEG C, calcination time
It is 1 hour, obtains trivalent dysprosium ion Dy3+The yellow fluorescent powder of activation.
It is to prepare material C a by this implementation technical scheme referring to accompanying drawing 64.75Dy0.25Nb4Ti3O21X-ray diffraction
Collection of illustrative plates, experiment confirms that the material of gained is pure phase, without others impurity thing phase.
It is that present invention implementation technical scheme prepares sample Ca referring to accompanying drawing 74.75Dy0.25Nb4Ti3O21Scanning electron show
Micro- collection of illustrative plates, as a result shows gained sample particle better crystallinity degree.
It is the material C a prepared by the present embodiment technical scheme referring to accompanying drawing 84.75Dy0.25Nb4Ti3O21In black light
388 nanometers excite down the luminous collection of illustrative plates for obtaining, it can be seen that the material mainly lights in yellow band, and the centre of luminescence is located at 574
Ran；
It is the material C a prepared by the present embodiment technical scheme referring to accompanying drawing 94.75Dy0.25Nb4Ti3O21In monitoring gold-tinted
574 nanometers of exciting light spectrograms for obtaining, it can be seen that luminous excites source main at 388 nanometers, can be well matched near
The light that ultraviolet diode chip for backlight unit sends.
The material C a of the present embodiment technical scheme preparation is pressed referring to accompanying drawing 104.75Dy0.25Nb4Ti3O21In black light 388
Nanometer excites the lower monitoring luminescent lifetime spectrogram that obtains of 574 nano wave lengths, and can be calculated the Yellow luminous life-span is 0.32 milli
Second.
Embodiment 6：
According to chemical formula Ca4.9995Dy0.0005Nb4Ti3O21The stoichiometric proportion of middle each element, weighs calcium carbonate respectively
CaCO3:1.2499 grams；Dysprosia Dy2O3:0.0002 gram；Niobium hydroxide Nb (OH)5:1.7790 grams；Butyl titanate
C16H36O4Ti:2.5500 grams used as raw material.By calcium carbonate CaCO3Dust technology is dissolved in, the oxalic acid of 2.2508 grams of addition, stirring is straight
It is extremely fully transparent；By dysprosia Dy2O3Dust technology is dissolved in, the oxalic acid of 0.0002 gram of addition is stirred until fully transparent；Will
Niobium hydroxide Nb (OH)5It is placed in deionized water, the oxalic acid of 1.8008 grams of addition, stirring is until fully transparent；By the fourth of metatitanic acid four
Ester C16H36O4Ti and a small amount of glacial acetic acid are mixed, and are then added drop-wise in ethanol again, and the oxalic acid of 1.3506 grams of addition adjusts pH
It is 4 to be worth, and stirring forms vitreosol, and butyl titanate and the mol ratio of ethanol, glacial acetic acid used is 1：10：1.
By above-mentioned solution mix, temperature be 100 DEG C under conditions of stir 1 hour, stand, drying, obtain it is fluffy before
Drive body；The presoma that will be obtained precalcining in air atmosphere, calcining heat is 400 DEG C, and calcination time is 10 hours；Obtain
The product of precalcining, after natural cooling, grinds and is well mixed, and is calcined in air atmosphere, and calcining heat is 1100 DEG C, calcining
Time is 10 hours, obtains a kind of trivalent dysprosium ion Dy3+The yellow fluorescent powder of activation.
The main structural behaviour of sample, excitation spectrum, luminescent spectrum and luminescent lifetime spectrogram are similar to Example 5.
Embodiment 7:
According to chemical formula Ca4.1Dy0.9Nb4Ti3O21The stoichiometric proportion of middle each element, weighs calcium nitrate Ca (NO respectively3)2:
1.6820 grams；Dysprosium nitrate Dy (NO3)3·6H2O:1.0274 grams；Niobium hydroxide Nb (OH)5:1.7790 grams；Butyl titanate
C16H36O4Ti:2.5500 grams used as raw material.By calcium carbonate CaCO3It is dissolved in deionized water, the oxalic acid of 1.6612 grams of addition, stirring
Until fully transparent；By dysprosia Dy2O3Deionized water is dissolved in, the oxalic acid of 0.3647 gram of addition is stirred until fully transparent；
By niobium hydroxide Nb (OH)5It is placed in deionized water, the oxalic acid of 1.6207 grams of addition, stirring is until fully transparent；By metatitanic acid four
Butyl ester C16H36O4Ti and a certain amount of glacial acetic acid are mixed, and are then added drop-wise in ethanol again, and the oxalic acid of 1.2155 grams of addition is adjusted
Section pH value is 3, and stirring forms vitreosol, and butyl titanate and the mol ratio of ethanol, glacial acetic acid used is 1：10：1.
By above-mentioned solution mix, temperature be 100 DEG C under conditions of stir 1 hour, stand, drying, obtain it is fluffy before
Drive body；The presoma that will be obtained precalcining in air atmosphere, calcining heat is 550 DEG C, and calcination time is 8 hours；Obtain
The product of precalcining, after natural cooling, grinds and is well mixed, and is calcined in air atmosphere, and calcining heat is 1150 DEG C, calcining
Time is 6 hours, obtains a kind of trivalent dysprosium ion Dy3+The yellow fluorescent powder of activation.
The main structural behaviour of sample, excitation spectrum, luminescent spectrum and luminescent lifetime spectrogram are similar to Example 5.
Embodiment 8:
According to chemical formula Ca4DyNb4Ti3O21The stoichiometric proportion of middle each element, weighs calcium nitrate Ca (NO respectively3)2:
1.6410 grams；Dysprosium nitrate Dy (NO3)3·6H2O:1.1415 grams；Niobium hydroxide Nb (OH)5:1.7790 grams；Butyl titanate
C16H36O4Ti:2.5500 grams used as raw material.By calcium carbonate CaCO3It is dissolved in deionized water, the oxalic acid of 1.8008 grams of addition, stirring
Until fully transparent；By dysprosia Dy2O3Deionized water is dissolved in, the oxalic acid of 0.4502 gram of addition is stirred until fully transparent；
By niobium hydroxide Nb (OH)5It is placed in deionized water, the oxalic acid of 1.8008 grams of addition, stirring is until fully transparent；By metatitanic acid four
Butyl ester C16H36O4Ti and a certain amount of glacial acetic acid are mixed, and are then added drop-wise in ethanol again, and the oxalic acid of 1.3506 grams of addition is adjusted
Section pH value is 3.5, and stirring forms vitreosol, and butyl titanate and the mol ratio of ethanol, glacial acetic acid used is 1：10：1.
Above-mentioned solution is mixed, is stirred 4 hours under conditions of being 80 DEG C in temperature, stood, dry, obtain fluffy forerunner
Body；The presoma that will be obtained precalcining in air atmosphere, calcining heat is 650 DEG C, and calcination time is 6 hours；What is obtained is pre-
The product of calcining, after natural cooling, grinds and is well mixed, and is calcined in air atmosphere, and calcining heat is 1250 DEG C, during calcining
Between be 3 hours, obtain a kind of trivalent dysprosium ion Dy3+The yellow fluorescent powder of activation.
The main structural behaviour of sample, excitation spectrum, luminescent spectrum and luminescent lifetime spectrogram are similar to Example 5.
Claims (8)
1. a kind of in the near ultraviolet excitated lower fluorescent material for launching gold-tinted, it is characterised in that：Its chemical composition formula is：Ca5- 5xDy5xNb4Ti3O21, wherein x is dysprosium ion Dy3+Substitution calcium ion Ca2+Mol ratio, and 0.0001≤x≤0.20.
2. a kind of as claimed in claim 1 in the preparation method of the near ultraviolet excitated lower fluorescent material for launching gold-tinted, its feature
It is to comprise the following steps：
(1) by formula Ca5-5xDy5xNb4Ti3O21, the stoichiometric proportion of corresponding element is weighed and contains calcium in 0.0001≤x≤0.20
Ion Ca2+Compound, contain dysprosium ion Dy3+Compound, contain niobium ion Nb5+Compound, contain titanium ion Ti4+'s
Compound grinds respectively as the raw material for preparing, the raw material that will be weighed, and is well mixed；
(2) mixture for obtaining step (1) is pre-sintered 1~2 time in air atmosphere, and sintering temperature is 900~1200 DEG C, is burnt
The knot time is 1~10 hour；
(3) will grind uniform after the mixture natural cooling of step (2), be calcined in air atmosphere, calcining heat is 1200~
1400 DEG C, calcination time is 1~15 hour, you can obtain a kind of yellow fluorescent material.
3. the preparation method of the fluorescent material near ultraviolet excitated lower transmitting gold-tinted according to claim 2, its feature exists
In：Described calcium ions Ca2+Compound be calcium carbonate CaCO3, calcium chloride CaCl2, calcium nitrate Ca (NO3)2, calcium oxide CaO
In one kind；Described contains dysprosium ion Dy3+Compound be dysprosia Dy2O3, dysprosium nitrate Dy (NO3)3·6H2In O one
Kind；Described contains niobium ion Nb5+Compound be niobium pentaoxide Nb2O5, columbium pentachloride NbCl5In one kind；Described contains
There is titanium ion Ti4+Compound be titanium dioxide TiO2。
4. the preparation method of the fluorescent material near ultraviolet excitated lower transmitting gold-tinted according to claim 2, its feature exists
In：The calcining heat of step (3) is 1250~1350 DEG C, and calcination time is 5~8 hours.
5. a kind of as claimed in claim 1 in the preparation method of the near ultraviolet excitated lower fluorescent material for launching gold-tinted, its feature
It is to comprise the following steps：
(1) by chemical formula Ca5-5xDy5xNb4Ti3O21, the stoichiometric proportion of each element, weighs respectively in 0.0001≤x≤0.20：
Contain calcium ion Ca2+Compound, contain dysprosium ion Dy3+Compound, contain niobium ion Nb5+Compound, contain titanium ion
Ti4+Compound be prepare raw material；
(2) step (1) is contained into calcium ion Ca2+Compound, contain dysprosium ion Dy3+Compound, contain niobium ion Nb5+Change
Compound is dissolved separately in deionized water or is diluted in nitric acid and with deionized water, will contain titanium ion Ti4+Compound mix
Merging is dissolved into glacial acetic acid and then is added drop-wise in ethanol again, and between 2-4, stirring forms vitreosol to regulation pH value；It is various
Ion mole 1.5 is separately added among solution again to 2 times of complexing agent, described complexing agent is in citric acid, oxalic acid
Kind, respectively obtain and contain calcium ion Ca2+, dysprosium ion Dy3+, niobium ion Nb5+, titanium ion Ti4+Solution；
(3) above-mentioned solution is mixed, temperature stands, dries to be stirred 1~5 hour under conditions of 50~100 DEG C, obtains fluffy
Presoma；
(4) the presoma precalcining in air atmosphere for obtaining step (3), temperature is 400~750 DEG C, and the time is 1~10 small
When；
(5) after the product natural cooling of step (4) precalcining, grind and be well mixed, calcined in air atmosphere, calcining heat
It it is 1100~1300 DEG C, calcination time is 1~10 hour, obtains yellow fluorescent powder.
6. the preparation method of the fluorescent material near ultraviolet excitated lower transmitting gold-tinted according to claim 5, its feature exists
In：The calcining heat of step (5) is 1150~1250 DEG C, and calcination time is 3~6 hours.
7. the preparation method of the fluorescent material near ultraviolet excitated lower transmitting gold-tinted according to claim 5, its feature exists
In：Described calcium ions Ca2+Compound be calcium carbonate CaCO3, calcium nitrate Ca (NO3)2In one kind；Described contains dysprosium
Ion Dy3+Compound be dysprosia Dy2O3, dysprosium nitrate Dy (NO3)3·6H2One kind in O；Described contains niobium ion Nb5+
Compound be niobium hydroxide Nb (OH)5；The described compound containing titanium elements is butyl titanate C16H36O4Ti, the titanium
Sour four butyl esters are 1 with the mol ratio of ethanol, glacial acetic acid：10：1.
8. a kind of application of the fluorescent material near ultraviolet excitated lower transmitting gold-tinted as claimed in claim 1, it is characterised in that：
The fluorescent material launches the gold-tinted of 574 rans under 350-420 nanometers of excitation, can prepare near purple
Illumination or display device of the outer light for excitation source, can also mix it with red fluorescence powder, and combined with InGaN blue chips
Obtain sending the LED of warm white.
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