CN105950149B - A kind of rare earth vanadium niobates red fluorescence material and preparation method thereof - Google Patents
A kind of rare earth vanadium niobates red fluorescence material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of rare earth vanadium niobates red fluorescence material and preparation method thereof, the chemical formula of the material is A1‑x‑y‑ zV1‑nNbnO4:Eu3+ x,Sm3+ y,Bi3+ z；A represents one or both of Sc and Lu；Wherein, 0.005≤x≤0.2,0.005≤y≤0.1,0.001≤z≤0.05,0 ＜ n≤0.5, A:V:Nb:Eu:Sm:Bi=(1 x y z):(1‑n):n:x:y:z.The step of preparation method is：S1, the metallic compound for stoichiometrically weighing Sc, Lu, Eu, Sm and Bi are simultaneously dissolved in hydrochloric acid or nitric acid, form mixed solution A；S2, ammonium metavanadate, potassium niobate raw material are weighed, be dissolved in ammonia spirit, and surfactant is added and forms mixed solution B, be placed in microwave ultrasonic wave combinatorial compound instrument；S3, mixed solution A is added dropwise to by constant flow peristaltic pump in solution B, generate precipitation, then it is aged, be filtered, washed, dry, both presoma；S4, by presoma high temperature sintering, then post-processed, obtain finished product.
Description
Technical field
The present invention relates near ultraviolet LED excitation phosphor technologies fields, relate in particular to a kind of rare earth vanadium niobates
Red fluorescence material and preparation method thereof.
Background technology
White light emitting diode (Light~emiting Diodes；LED) since the advent of the world, because it has efficient, ring
The features such as guarantor, energy saving, pollution-free and long lifespan, high-tech sector is entered with the speed advanced by leaps and bounds in recent years, is known as white heat
Forth generation lighting source after lamp, fluorescent lamp, energy-saving lamp.Currently, commercialization " blue-ray LED+YAG:Ce3+" combining form generation
White light, color reducibility and colour rendering index etc. limit it because lacking red fluorescence further to be developed.With nearly purple
The gradual commercialization of outer LED, it is gradually active to " near ultraviolet LED+redgreenblue (RGB) fluorescent powder " research, but wherein apply
In the rouge and powder near ultraviolet chip (such as commercial rouge and powder：Y2O2S:Eu3+) generally existing luminous efficiency is low and thermal stability is poor etc. lacks
Point.And vanadate has cubic zircon paracrystalline organizations, is a kind of excellent host material, there is sensitization to make rare earth ion
With Ultraviolet radiation absorbing and rare earth ion capable of being passed to, there is higher luminous efficiency, be a kind of very promising luminous material
Material.Therefore, exploitation can match with existing near ultraviolet LED chip, thermal stability is good, luminous efficiency is high and colour rendering index is good
Novel rare-earth vanadate red fluorescence material is with important application prospects.
Document [G.BLASSE, J.Chem.Phys.1969,50,2974~2980] reports Sc0.97Eu0.03VO4Fluorescence
Powder, 250~270nm excitation quantums efficiency 55%, up to 75%.Document [Zuo Yinyan, Rare Metals Materials and engineering,
2007,36(3):386~389.] it also studied the Y of a small amount of Sc doping0.95-xScxEu0.05VO4The spectrum of (0.01≤x≤0.05)
Characteristic, the doping of appropriate Sc and Bi can widthization excitation spectrum, but emissive porwer also can accordingly die down.And Ye Xin spaces seminar
Around ScVO4Matrix has done numerous studies, has invented one kind with Sc1-x-y-m-nLnxVO4:Eu3+ y,Sm3+ m,Al3+ nFor principal component
[Ye Xinyu, application for a patent for invention number 201310181720.8 authorize public vanadate red phosphor material and preparation method thereof
The number of opening CN103351865A]；It also studied Bi3+、BO3 3-、PO4 3-Deng the luminescent properties to fluorescent powder influence [X.Ye,
Physica B,2016,487:8~12].[Deng Chao, shine document journal, 2015,36 (11)：1246:1251.] it also reports
Al3+Doping is to ScVO4:Eu3+,Bi3+The influence of light-emitting phosphor performance.Document [B.Yan, Opt.Mater., 2007,29 (5):
547~551.] LuVO of high temperature solid-state method synthesis is had studied4:RE3+The luminescence feature of (RE=Sm, Eu) red fluorescence powder.Text
Offer [S.Li, J.Nanosci.Nanotechno., 2014,14 (5):3631~3634.] LuVO is reported4:Eu3+,Bi3+It is red
Fluorescent powder.
As can be seen that the hot spot of research is increasingly becoming using vanadate as the fluorescent material of matrix, but at (Sc, Lu)
VO4Eu is co-doped in matrix3+, Sm3+And Bi3+, while with a certain amount of NbO4 3-To replace part VO4 3-To improve the hair of fluorescent powder
Light characteristic and thermal stability yet there are no similar report.
Invention content
It is an object of the invention in view of the above-mentioned defects in the prior art, provide a kind of rare earth vanadium niobates red fluorescence material
Material, the material is under near ultraviolet LED excitation, and luminous intensity is high, thermal stability is good；The present invention and the preparation side for providing the material
Method.Presoma is prepared using microwave/ultrasonic wave aid coprecipitation method, the particle agglomeration phenomenon of fluorescent powder can be substantially improved.
To achieve the goals above, the technical scheme is that：
The chemical formula of a kind of rare earth vanadium niobates red fluorescence material, the material is A1-x-y-zV1-nNbnO4:Eu3+ x,Sm3+ y,
Bi3+ z；A represents one or both of Sc and Lu；Wherein, 0.005≤x≤0.2,0.005≤y≤0.1,0.001≤z≤
0.05,0 ＜ n≤0.5, A:V:Nb:Eu:Sm:Bi=(1-x-y-z):(1-n):n:x:y:z.
The step of present invention and preparation method for providing above-mentioned material, preparation method is：
S1, by least one of the oxide of Eu, hydroxide, oxalates, carbonate, the oxide of Sm, hydroxide
At least one of at least one of object, oxalates, carbonate, the oxide of Sc, hydroxide, oxalates, carbonate
And/or at least one of the oxide of Lu, hydroxide, oxalates, carbonate and Bi2O3、Bi(OH)3In at least one
Kind be raw material, by above-mentioned material chemical formula composition and stoichiometric ratio weigh corresponding raw material, be mixed be dissolved in nitric acid or
In person's hydrochloric acid, mixed solution A is formed；
S2, ammonium metavanadate (NH is weighed by chemical formula composition and stoichiometric ratio4VO3), potassium niobate (K3NbO4) raw material, it will
It is dissolved in ammonia spirit, and a certain amount of surfactant is added and forms mixed solution B, the microwave being placed under certain condition
In ultrasonic wave combinatorial compound instrument；
S3, mixed solution A is added dropwise to by constant flow peristaltic pump in solution B, generates and precipitates, then aged, filtering,
Washing, drying, both obtain presoma；
S4, by presoma high temperature sintering, then post-processed, obtain finished product.
As the improvement to above-mentioned technical proposal, in the step 2 surfactant be CTAB, PEG6000, OP-10,
One or more of SDS, the quality that surfactant is added are the 0.5%~3.5% of presoma gross mass.
As the improvement to above-mentioned technical proposal, the operating condition of microwave ultrasonic wave combinatorial compound instrument is in the step 2
Microwave power is 300~900W, and ultrasonic power is 400~1000W, and microwave/ultrasonic time pattern is 1:1~3:1, reaction temperature
Degree is 20~100 DEG C.
As the improvement to above-mentioned technical proposal, in the step 3 rate of addition of constant flow peristaltic pump be 3.0~
10.0ml/min。
As the improvement to above-mentioned technical proposal, in the step 3 digestion time be 0.5~2.0h, natural filtration, go from
Son washing 2~5 times, 80~120 DEG C of drying.
As the improvement to above-mentioned technical proposal, calcination temperature is 600~1000 DEG C in the step 4, roasting time 2
~5 hours.
As the improvement to above-mentioned technical proposal, last handling process includes in the step 4：High-temperature roasting product is broken,
It fully grinds, is washed 1~3 time using ethanol solution, deionization is washed 2~5 times, is filtered, drying, and the final grain size that obtains is in 1~5 μ
The process of m fluorescent powders.
Compared with prior art, the invention has the advantages and positive effects that：
The preparation method of the rare earth vanadium niobates red fluorescence material of the present invention, the microwave of use, ultrasonic wave outfield auxiliary
Fluorescent powder prepared by coprecipitation, prepared rare earth vanadium niobates red fluorescence material have excellent luminescent properties, pattern
Rule, even particle distribution, thermal stability is good, and being one kind has high luminous intensity and meet used near ultraviolet LED novel red glimmering
Luminescent material.
1, fluorescent powder excitation wave band of the present invention meets near ultraviolet white light LEDs with newly between 200~400nm ranges
The requirement of type red illuminating material；
2, fluorescent powder of the present invention luminous intensity under above-mentioned condition excitation is very high, and the hair of LED can be greatly improved
Light efficiency reduces energy loss；This is because the Eu that the present invention uses3+、Sm3+、Bi3+The method of codope and special matrix
The coefficient result of ingredient；
3, thermal stability of the fluorescent powder of the present invention under 200 DEG C of operating condition is significantly stronger than commercial Y2O2S:Eu3 +, this is because rare earth Sc and Lu have been participated in vanadium niobates matrix components；
4, compared with conventional high-temperature solid phase method, the present invention is prepared glimmering using microwave, ultrasonic wave outfield aid coprecipitation method
Light powder pattern is more regular, even particle distribution, soilless sticking phenomenon.
Specific implementation mode
Below in conjunction with specific embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
Embodiment in invention, every other reality obtained by those of ordinary skill in the art without making creative efforts
Example is applied, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Embodiment 1：
The near ultraviolet excitated chemical formula with rare-earth vanadate red fluorescence powder product of the present embodiment is
Sc0.935V0.8Nb0.2O4:Eu3+ 0.05,Sm3+ 0.01,Bi3+ 0.005, wherein x=0.05, y=0.01, z=0.005, n=0.2, A are
Sc.Preparation method is：Weigh Sc2O38.0761g、Eu2O31.0998g、Sm2O30.2179g and Bi2O30.1456g, then its
Mixing is dissolved in 40% HNO3In, it makes it completely dissolved to form mixed solution A；Then NH is weighed4VO311.6978g and
K3NbO44.5001g is dissolved in, with ammonia spirit, and Surfactant CTAB 0.7721g being added and forms mixed solution B, after
It is placed in microwave ultrasonic wave combinatorial compound instrument, 300~900w of adjusting microwave power, 400~1000w of ultrasonic power, microwave/super
Sound temporal mode is 1:1~3:1,20~80 DEG C of reaction temperature；Mixed solution A is controlled 3~10ml/min by peristaltic pump to add
Enter into solution B, generate white precipitate, then aged 0.5~2h, natural filtration, deionized water wash 2~5 times, 80 DEG C~
120 DEG C of dryings obtain presoma；Presoma is fitted into alumina crucible to be put into high temperature furnace, 2~5 are kept the temperature in 600~1000 DEG C
Hour, it then grinds, product is cleaned 1~3 time with ethyl alcohol, then be washed with deionized water 2~5 times, mistake after cooled to room temperature
It filters, drying is to get product under the conditions of 100 DEG C.Its excitation spectrum excitation peak is wider, can be effective by 200~400nm range of wavelength light
Excitation, can be applied near ultraviolet LED chip.Its chromaticity coordinates is (0.6584,0.3295), is in pure emitting red light, relatively bright
Degree is 1.0000.
2~embodiment of embodiment 15
In addition to weighing related raw material by its chemical formula composition and stoichiometry, remaining preparation process is same as Example 1,
Chemical formula composition, chromaticity coordinates and the relative luminance of product are shown in Table 1.
1 embodiment of table, 1~15 chemical formula, chromaticity coordinates and relative luminance
Note：Data above is to test gained under near ultraviolet (397nm) excitation
Embodiment 16：
The near ultraviolet excitated chemical formula with rare-earth vanadate red fluorescence powder product of the present embodiment is
Lu0.9V0.9Nb0.1O4:Eu3+ 0.07,Sm3+ 0.02,Bi3+ 0.01, wherein x=0.07, y=0.02, z=0.01, n=0.1, A Lu.
Preparation method is：Weigh Lu (OH)313.5593g、Eu(OH)30.9473g、Sm(OH)30.2685g and Bi (OH)30.1733g, then its mixing are dissolved in 36% HCl, make it completely dissolved to form mixed solution A；Then it weighs
NH4VO37.0187g and K3NbO41.2000g is dissolved in, with ammonia spirit, and Surfactant PEG 6000 being added
0.6950g forms mixed solution B, is placed in microwave ultrasonic wave combinatorial compound instrument, adjusts 300~900w of microwave power, ultrasound
400~1000w of wave power, microwave/ultrasonic time pattern are 1:1~3:1,20~80 DEG C of reaction temperature；Mixed solution A is passed through
Peristaltic pump control 3~10ml/min be added in solution B, generate white precipitate, then aged 0.5~2h, natural filtration, go from
Sub- water washing 2~5 times, 80 DEG C~120 DEG C dryings obtain presoma；Presoma is fitted into alumina crucible to be put into high temperature furnace,
2~5 hours are kept the temperature in 600~1000 DEG C, is then ground after cooled to room temperature, product is cleaned 1~3 time with ethyl alcohol, then
It is washed with deionized water 2~5 times, filters, drying is to get product under the conditions of 100 DEG C.Its excitation spectrum excitation peak is wider, can be by 200
~400nm range of wavelength light effectively excites, and can be applied near ultraviolet LED chip.Its chromaticity coordinates is (0.6613,0.3304), is in
Pure emitting red light.
17~embodiment of embodiment 27
In addition to weighing related raw material by its chemical formula composition and stoichiometry, remaining preparation process and 16 phase of embodiment
Together, chemical formula composition, chromaticity coordinates and the relative luminance of product are shown in Table 2.
2 embodiment of table, 16~27 chemical formula, chromaticity coordinates and relative luminance
| Embodiment | Chemical formula | Chromaticity coordinates | Relative luminance |
| 16 | Lu0.9V0.9Nb0.1O4:Eu3+ 0.07,Sm3+ 0.02,Bi3+ 0.01 | (0.6613,0.3304) | 1.5480 |
| 17 | Lu0.989V0.9Nb0.1O4:Eu3+ 0.005,Sm3+ 0.005,Bi3+ 0.001 | (0.6512,0.3233) | 0.8814 |
| 18 | Lu0.964V0.9Nb0.1O4:Eu3+ 0.03,Sm3+ 0.005,Bi3+ 0.005 | (0.6588,0.3267) | 1.1034 |
| 19 | Lu0.89V0.9Nb0.1O4:Eu3+ 0.09,Sm3+ 0.015,Bi3+ 0.005 | (0.6606,0.3311) | 1.3238 |
| 20 | Lu0.84V0.9Nb0.1O4:Eu3+ 0.15,Sm3+ 0.005,Bi3+ 0.005 | (0.6592,0.3301) | 1.0276 |
| 21 | Lu0.79V0.9Nb0.1O4:Eu3+ 0.2,Sm3+ 0.005,Bi3+ 0.005 | (0.6574,0.3269) | 0.9341 |
| 22 | Lu0.85V0.9Nb0.1O4:Eu3+ 0.09,Sm3+ 0.05,Bi3+ 0.01 | (0.6534,0.3285) | 1.2323 |
| 23 | Lu0.8V0.9Nb0.1O4:Eu3+ 0.09,Sm3+ 0.1,Bi3+ 0.01 | (0.6648,0.3358) | 1.3435 |
| 24 | Lu0.875V0.9Nb0.1O4:Eu3+ 0.09,Sm3+ 0.015,Bi3+ 0.02 | (0.6663,0.3351) | 1.8216 |
| 25 | Lu0.87V0.9Nb0.1O4:Eu3+ 0.09,Sm3+ 0.015,Bi3+ 0.035 | (0.6650,0.3355) | 1.7818 |
| 26 | Lu0.845V0.9Nb0.1O4:Eu3+ 0.09,Sm3+ 0.015,Bi3+ 0.05 | (0.6671,0.3373) | 1.9064 |
| 27 | Lu0.65V0.9Nb0.1O4:Eu3+ 0.2,Sm3+ 0.1Bi3+ 0.05 | (0.6574,0.3224) | 0.8114 |
Note：Data above is to test gained under near ultraviolet (397nm) excitation
Embodiment 28：
The near ultraviolet excitated chemical formula with rare-earth vanadate red fluorescence powder product of the present embodiment is (Sc0.84Lu0.05)
V0.9Nb0.1O4:Eu3+ 0.08,Sm3+ 0.015,Bi3+ 0.015, wherein x=0.08, y=0.015, z=0.015, n=0.1, A be Sc and
Lu.Preparation method is：Weigh Sc2(CO3)316.1963g、Lu2(CO3)31.8927g、Eu2(CO3)32.7655g、Sm2(CO3)30.5051g and Bi2O30.4992g, then its mixing are dissolved in 40% HNO3In, it makes it completely dissolved to form mixed solution A；So
After weigh NH4VO315.0400g and K3NbO42.5715g, be dissolved in in ammonia spirit, and be added Surfactant OP~
10 0.6985g form mixed solution B, are placed in microwave ultrasonic wave combinatorial compound instrument, adjust 300~900w of microwave power, surpass
400~1000w of acoustic power, microwave/ultrasonic time pattern are 1:1~3:1,20~80 DEG C of reaction temperature；By mixed solution A
By peristaltic pump control 3~10ml/min be added in solution B, generate white precipitate, then aged 0.5~2h, natural filtration,
Deionized water washs 2~5 times, 80 DEG C~120 DEG C dryings, obtains presoma；Presoma loading alumina crucible is put into high temperature
In stove, 2~5 hours are kept the temperature in 600~1000 DEG C, is then ground after cooled to room temperature, product is cleaned 1~3 with ethyl alcohol
Time, then be washed with deionized water 2~5 times, it filters, drying is to get product under the conditions of 100 DEG C.Its excitation spectrum excitation peak is wider, can
It is effectively excited by 200~400nm range of wavelength light, can be applied near ultraviolet LED chip.Its chromaticity coordinates be (0.6666,
0.3358), it is in pure emitting red light.
29~embodiment of embodiment 32
In addition to weighing related raw material by its chemical formula composition and stoichiometry, remaining preparation process and 28 phase of embodiment
Together, chemical formula composition, chromaticity coordinates and the relative luminance of product are shown in Table 3.
3 embodiment of table, 28~32 chemical formula, chromaticity coordinates and relative luminance
| Embodiment | Chemical formula | Chromaticity coordinates | Relative luminance |
| 28 | (Sc0.84Lu0.05)V0.9Nb0.1O4:Eu3+ 0.08,Sm3+ 0.015,Bi3+ 0.015 | (0.6666,0.3358) | 2.2548 |
| 29 | (Sc0.74Lu0.15)V0.9Nb0.1O4:Eu3+ 0.08,Sm3+ 0.015,Bi3+ 0.015 | (0.6678,0.3373) | 2.5815 |
| 30 | (Sc0.49Lu0.4)V0.9Nb0.1O4:Eu3+ 0.08,Sm3+ 0.015,Bi3+ 0.015 | (0.6642,0.3350) | 1.9654 |
| 31 | (Sc0.29Lu0.6)V0.9Nb0.1O4:Eu3+ 0.08,Sm3+ 0.015,Bi3+ 0.015 | (0.6636,0.3341) | 1.6387 |
| 32 | (Sc0.09Lu0.8)V0.9Nb0.1O4:Eu3+ 0.08,Sm3+ 0.015,Bi3+ 0.015 | (0.6617,0.3316) | 1.1358 |
Note：Data above is to test gained under near ultraviolet (397nm) excitation
Embodiment 33：
The near ultraviolet excitated chemical formula with rare-earth vanadate red fluorescence powder product of the present embodiment is (Sc0.74Lu0.15)
V0.95Nb0.05O4:Eu3+ 0.08,Sm3+ 0.015,Bi3+ 0.015, wherein x=0.08, y=0.015, z=0.015, n=0.05, A Sc
And Lu.Preparation method is：Weigh Sc2(C2O4)318.7098g、Lu2(C2O4)36.5785g、Eu2(C2O4)33.2456g、Sm2
(C2O4)30.6051g and Bi (OH)30.5571g, then its mixing are dissolved in 36% HCl, make it completely dissolved to form mixing
Solution A；Then NH is weighed4VO315.8756g and K3NbO41.2857g, be dissolved in in ammonia spirit, and be added surface work
Property agent SDS0.8444g form mixed solution B, be placed in microwave ultrasonic wave combinatorial compound instrument, adjust microwave power 300~
900w, 400~1000w of ultrasonic power, microwave/ultrasonic time pattern are 1:1~3:1,20~80 DEG C of reaction temperature；It will mixing
Solution A controls 3~10ml/min by peristaltic pump and is added in solution B, generates white precipitate, then aged 0.5~2h, normal pressure
Filtering, deionized water wash 2~5 times, 80 DEG C~120 DEG C dryings, obtain presoma；Presoma loading alumina crucible is put into
In high temperature furnace, 2~5 hours are kept the temperature in 600~1000 DEG C, is then ground after cooled to room temperature, product is cleaned 1 with ethyl alcohol
~3 times, then be washed with deionized water 2~5 times, it filters, drying is to get product under the conditions of 100 DEG C.Its excitation spectrum excitation peak compared with
Width can effectively be excited by 200~400nm range of wavelength light, can be applied near ultraviolet LED chip.Its chromaticity coordinates be (0.6647,
0.3339), it is in pure emitting red light.
34~embodiment of embodiment 37
In addition to weighing related raw material by its chemical formula composition and stoichiometry, remaining preparation process and 33 phase of embodiment
Together, chemical formula composition, chromaticity coordinates and the relative luminance of product are shown in Table 4.
4 embodiment of table, 33~37 chemical formula, chromaticity coordinates and relative luminance
Note：Following data is to test gained under near ultraviolet (397nm) excitation.
Claims (7)
1. a kind of preparation method preparing rare earth vanadium niobates red fluorescence material, it is characterised in that：The step of preparation method
It is：
S1, by least one of the oxide of Eu, hydroxide, oxalates, carbonate, the oxide of Sm, hydroxide, grass
At least one of at least one of hydrochlorate, carbonate, the oxide of Sc, hydroxide, oxalates, carbonate and/or Lu
Oxide, hydroxide, oxalates, at least one of carbonate and Bi2O3、Bi(OH)3At least one of for original
Material weighs corresponding raw material by the chemical formula composition and stoichiometric ratio of above-mentioned material, is mixed and is dissolved in nitric acid or hydrochloric acid
In, form mixed solution A；
S2, ammonium metavanadate, potassium niobate raw material are weighed by chemical formula composition and stoichiometric ratio, be dissolved in ammonia spirit, and
A certain amount of surfactant is added and forms mixed solution B, is placed in the microwave ultrasonic wave combinatorial compound instrument under certain condition；
S3, mixed solution A is added dropwise to by constant flow peristaltic pump in solution B, generate precipitation, then it is aged, filter, wash
It washs, dry, both obtain presoma；
S4, by presoma high temperature sintering, then post-processed, obtain finished product；The chemical formula of the finished product is A1-x-y-zV1-nNbnO4:
Eu3+ x,Sm3+ y,Bi3+ z；A represents one or both of Sc and Lu；Wherein, 0.005≤x≤0.2,0.005≤y≤0.1,
0.001≤z≤0.05,0 ＜ n≤0.5, A:V:Nb:Eu:Sm:Bi=(1-x-y-z):(1-n):n:x:y:z.
2. the preparation method of rare earth vanadium niobates red fluorescence material according to claim 1, it is characterised in that：The step
Surfactant is one or more of CTAB, PEG6000, OP-10, SDS in rapid 2, and the quality that surfactant is added is
The 0.5%~3.5% of presoma gross mass.
3. the preparation method of rare earth vanadium niobates red fluorescence material according to claim 1, it is characterised in that：The step
In rapid 2 the operating condition of microwave ultrasonic wave combinatorial compound instrument be microwave power be 300~900W, ultrasonic power be 400~
1000W, microwave/ultrasonic time pattern are 1:1~3:1, reaction temperature is 20~100 DEG C.
4. the preparation method of rare earth vanadium niobates red fluorescence material according to claim 1, it is characterised in that：The step
The rate of addition of constant flow peristaltic pump is 3.0~10.0ml/min in rapid 3.
5. the preparation method of rare earth vanadium niobates red fluorescence material according to claim 1, it is characterised in that：The step
Digestion time is 0.5~2.0h, natural filtration, deionization washing 2~5 times, 80~120 DEG C of drying in rapid 3.
6. the preparation method of rare earth vanadium niobates red fluorescence material according to claim 1, it is characterised in that：The step
Calcination temperature is 600~1000 DEG C in rapid 4, and roasting time is 2~5 hours.
7. the preparation method of rare earth vanadium niobates red fluorescence material according to claim 1, it is characterised in that：The step
Last handling process includes in rapid 4：High-temperature roasting product is broken, fully grinds, is washed 1~3 time using ethanol solution, deionization washing
It 2~5 times, filters, drying, process of the final acquisition grain size in 1~5 μm of fluorescent powder.
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| Intense red-emitting multi-rare-earth doped nanoparticles of YVO4 for spectrum conversion towards improved energy harvesting by solar cells;Vineet Kumar等;《J. Phys. D: Appl. Phys.》;20131231;第46卷;365101-1—365101-9 * |
| New red Y0.85Bi0.1Eu0.05 V1-yMyO4 (M= Nb, P) phosphors for light-emitting diodes;Yuhua Wang等;《Physica B》;20081231;第403卷;2071-2075 * |
| Variable Emission Changes in Bi3+/Ln3+(Ln = Eu, Sm, Dy) Co-doped Lutetium Vanadates (LuVO4);YUHUI ZHENG等;《Journal of ELECTRONIC MATERIALS》;20160217;第45卷;2974-2980 * |
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