CN106753370A - A kind of bismuth doping Tungstoborate yellow fluorescent powder and preparation method thereof, application - Google Patents
A kind of bismuth doping Tungstoborate yellow fluorescent powder and preparation method thereof, application Download PDFInfo
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- CN106753370A CN106753370A CN201610997436.1A CN201610997436A CN106753370A CN 106753370 A CN106753370 A CN 106753370A CN 201610997436 A CN201610997436 A CN 201610997436A CN 106753370 A CN106753370 A CN 106753370A
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- tungstoborate
- fluorescent powder
- bismuth
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 34
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000000843 powder Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 239000012467 final product Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims description 34
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 9
- 239000004327 boric acid Substances 0.000 claims description 8
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 8
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims description 7
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 6
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 6
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 125000005619 boric acid group Chemical group 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 17
- 229910052593 corundum Inorganic materials 0.000 description 17
- 239000010431 corundum Substances 0.000 description 17
- 230000005284 excitation Effects 0.000 description 13
- 230000009102 absorption Effects 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 8
- KXTVFSDQZZXLDA-UHFFFAOYSA-N B([O-])([O-])[O-].[W+4].B([O-])([O-])[O-].B([O-])([O-])[O-].B([O-])([O-])[O-].[W+4].[W+4] Chemical compound B([O-])([O-])[O-].[W+4].B([O-])([O-])[O-].B([O-])([O-])[O-].B([O-])([O-])[O-].[W+4].[W+4] KXTVFSDQZZXLDA-UHFFFAOYSA-N 0.000 description 7
- 238000010183 spectrum analysis Methods 0.000 description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 230000003595 spectral effect Effects 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 238000000695 excitation spectrum Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 229910016010 BaAl2 Inorganic materials 0.000 description 1
- 241001671621 Hemarthria altissima Species 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- -1 rare earth ion Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000009103 reabsorption Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000001161 time-correlated single photon counting Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-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
- C09K11/7712—Borates
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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Abstract
The invention discloses a kind of bismuth doping Tungstoborate yellow fluorescent powder, chemical general formula is La3(1‑x)BWO9:3xBi3+, wherein x is molar fraction, and 0<x≤0.1.The invention also discloses a kind of preparation method of bismuth doping Tungstoborate yellow fluorescent powder, raw material is weighed by chemical general formula, ground and mixed is uniform；In 400 800 DEG C of 12h of pre-burning 4, room temperature is cooled to, be ground；Then 4 12h are calcined at 1,000 1300 DEG C, after cooling to room temperature with the furnace, grinding obtains final product bismuth doping Tungstoborate yellow fluorescent powder.Fluorescent material of the invention can effectively be excited by the ultraviolet light in the range of 250 410nm, be lighted within the scope of 400 800nm, be centrally located at~560nm, and excited and launched adjustable, be a kind of Yellow fluorescent powder used by white light LED.
Description
Technical field
The present invention relates to field of light emitting materials, more particularly to a kind of bismuth doping Tungstoborate yellow fluorescent powder and its preparation side
Method, application.
Background technology
In recent years, as climate change and environmental problem increasingly manifest, people are look for substitute fossil fuels and do not discharge
The energy of carbon dioxide.White light LEDs are received much concern due to the superior performance such as efficient, compact, durable and environmentally friendly.White light
Promoting the use of for LED is extremely important, can significantly decrease the use of global power demand and fossil fuel, reduces carbon dioxide
The discharge of isothermal chamber gas.At present, white light LEDs have been widely used in normal lighting, gradually replace traditional illumination light
Source --- incandescent lamp, fluorescent lamp.
The white light LEDs (abbreviation pc-WLEDs) of fluorescent material conversion are considered as novel illumination light source of future generation.At present, white light
LED component generally uses blue-light LED chip and YAG:The encapsulation of Ce phosphor combinations is formed.But, this combination is red due to lacking
Light composition, the relatively low (Ra of colour rendering index<80), the higher (Tc of colour temperature>7000K), its application in some fields is hindered, it is such as indoor
Illumination.Additionally, blue-light LED chip and YAG:The heat ageing speed of Ce fluorescent material is different, with white light LED part run time
Extension, its is luminous will to be gradually deviated from white light.
In order to solve the above problems, researcher begins attempt to new encapsulation scheme, using ultraviolet-near ultraviolet LED chip
(350-410nm) combines generation white light with red, green, blue or yellow and blue phosphor.Several fluorescent material is coated in UV LED chips
On, chip excitated fluorescent powder forms the luminous of different colours, and the light of different colours is superimposed to obtain white light.This scheme can be obtained
Colour rendering is high, aberration is small and white light of adjustable color, overcomes blue-light LED chip and YAG:What Ce phosphor combinations faced asks
Topic.New departure requirement red, green, blue or yellow and blue phosphor must have absorption in 350-410nm, in visible region without absorption, and
And in visible region High Efficiency Luminescence.In existing yellow fluorescent powder, most of is with rare earth ion (Eu2+Or Ce3+) as activation
Agent, such as BaAl2O4:Eu2+, Sr8ZnSc(PO4)7:Eu2+, LaSr2AlO5:Ce3+, in addition to having absorption in ultra-violet (UV) band, in blue light
Also there is stronger absorption in area, and lighting by yellow fluorescent powder reabsorption for part blue colour fluorescent powder causes luminous efficiency to reduce.Cause
This, exploitation has absorption at ultra-violet (UV) band (particularly 350-410nm), and the adjustable yellow fluorescent material of excitation and emission spectra is hair
Luminescent material field great Scientific And Technical Problems urgently to be resolved hurrily.
The content of the invention
In order to overcome the disadvantages mentioned above and deficiency of prior art, it is an object of the invention to provide a kind of bismuth doping tungsten boric acid
Salt yellow fluorescent powder, in blue light region without absorption, is transmitted in yellow light area, and excite and launch adjustable.
The purpose of the present invention is achieved through the following technical solutions：
A kind of bismuth doping Tungstoborate yellow fluorescent powder, chemical general formula is La3(1-x)BWO9:3xBi3+, wherein x for mole point
Number, and 0<x≤0.1.
A kind of bismuth doping Tungstoborate yellow fluorescent powder, chemical general formula is La3(1-x)BWO9:3xBi3+, wherein x for mole point
Number, and 0<x≤0.1.
A kind of preparation method of bismuth doping Tungstoborate yellow fluorescent powder, comprises the following steps：
(1) by chemical general formula La3(1-x)BWO9:3xBi3+, wherein x is molar fraction, and 0<X≤0.1, weighs element containing La
Compound, the compound containing B element, the compound containing W elements, the compound ground and mixed containing Bi elements it is uniform, mixed
Compound material；
(2) mixed material for obtaining step (1) is cooled to room temperature in 400-800 DEG C of pre-burning 4-12h, is ground；So
4-12h is calcined at 1000-1300 DEG C afterwards, after cooling to room temperature with the furnace, grinding obtains final product bismuth doping Tungstoborate yellow fluorescent powder.
The compound containing La elements is lanthanum sesquioxide or lanthanum nitrate.
The compound containing B element is boric acid or diboron trioxide.
The compound containing W elements is tungstic acid or ammonium tungstate.
The compound containing Bi elements is bismuth oxide or bismuth nitrate.
The application of described bismuth doping Tungstoborate yellow fluorescent powder, excites for preparing ultraviolet-near ultraviolet LED chip
White light LED part.
Principle of the invention is as follows：Crystallographic data shows, La3BWO9Crystal belongs to hexagonal crystal system, and P63 (No.173) is empty
Between group, cell parameterLa3BWO9La has two in crystal
Individual different crystallographic sites, are eight-coordinate.According to radius and the electric charge principle of similitude, work as Bi3+Two are formed during substitution La not
Same centre of luminescence Bi (I) and Bi (II).By changing excitation wavelength, so as to realize luminous adjustable.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) bismuth Doped Tungsten borate fluorescent powder excitation band of the invention is relatively wide, has strong suction in the range of 250-410nm
Receive.
(2) bismuth Doped Tungsten borate fluorescent powder of the invention Yellow light-emitting low temperature under ultraviolet excitation, lights in 400-800nm models
Within enclosing ,~560nm is centrally located at.
(3) bismuth Doped Tungsten borate fluorescent powder transmitting of the invention is adjustable, and by changing excitation wavelength, emission peak positions can
580nm is transferred to from 540nm.
(4) bismuth Doped Tungsten borate fluorescent powder of the invention excites adjustable, by changing monitoring wavelength, excites the peak position can
350nm is transferred to from 326nm.
(5) bismuth Doped Tungsten borate fluorescent powder Stability Analysis of Structures of the invention, synthetic method is simple, is easy to large-scale production.
(6) bismuth Doped Tungsten borate fluorescent powder of the invention can be applied to the white light that ultraviolet-near ultraviolet LED chip is excited
LED component is encapsulated.
Brief description of the drawings
Fig. 1 is the X-ray powder diffraction pattern of proportioning (1)-(6) sample of embodiment 1.
Fig. 2 is the emission spectrum of proportioning (1)-(6) sample of embodiment 1, excitation wavelength 340nm.
Fig. 3 is the excitation spectrum of proportioning (1)-(6) sample of embodiment 1, monitoring wavelength 560nm.
Fig. 4 is the monitoring wavelength dependency spectrum of proportioning (3) sample of embodiment 1.
Fig. 5 is the excitation wavelength dependence spectrum of proportioning (3) sample of embodiment 1.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Embodiment 1
Lanthanum sesquioxide, boric acid, tungstic acid, bismuth oxide are chosen as initial compounds raw material, by each element
Metering ratio is learned, four kinds of raw materials of compound are weighed respectively, totally 6 groups, matched as follows：
(1)La:B:W:Bi=2.985:1:1:0.015, correspondence x=0.5%；
(2)La:B:W:Bi=2.970:1:1:0.030, correspondence x=1.0%；
(3)La:B:W:Bi=2.955:1:1:0.045, correspondence x=1.5%；
(4)La:B:W:Bi=2.940:1:1:0.060, correspondence x=2.0%；
(5)La:B:W:Bi=2.925:1:1:0.075, correspondence x=2.5%；
(6)La:B:W:Bi=2.910:1:1:0.090, correspondence x=3.0%；
Mixture it is ground it is well mixed after, load corundum crucible；Corundum crucible is placed in corundum boat, high-temperature cabinet is put into
Formula electric furnace.Strict control heating rate, in 600 DEG C of pre-burning 4h.Room temperature is cooled to, is ground；Then in 1000 DEG C of calcinings
12h, after cooling to room temperature with the furnace, grinding obtains final product bismuth doping Tungstoborate yellow fluorescent material.
Fig. 1 is the X-ray powder diffraction pattern of proportioning (1)-(6) sample of embodiment 1.Using German Brooker company
(Bruker) D8 ADVANCE types x-ray powder diffraction instrument is determined.Radiation source is Cu target K alpha raysSurvey
Examination voltage 40kV, tests electric current 40mA, 0.02 °/step of scanning step, sweep speed：0.12s/step.XRD spectrum analytical table
It is bright to be La3BWO9Phase, belongs to monoclinic system, and dopping effect does not introduce other thing phases or impurity.
Fig. 2 is the emission spectrum of proportioning (1)-(6) sample of embodiment 1, and excitation wavelength is 340nm.Fourth is liked using Britain
Fort company (Edinburgh) FLS920 type stable states moment XRF is determined.Xenon lamp with 450W as excitation source, during outfit
Between correct single photon counting card (TCSPC), the red quick photomultiplier (PMT) of thermoelectric cold, TM300 excitation monochromators and double TM300
Transmitting monochromator.As shown in Figure 2, under 340nm ultraviolet excitations, sample can all produce be centrally located at~yellow of 560nm sends out
Light, wavelength covering 400-800nm, correspondence Bi3+'s3P1→1S0Transition.And with Bi3+Doping concentration increase, launch peak position
Put and produce slight red shift.
Fig. 3 is the excitation spectrum of proportioning (1)-(6) sample of embodiment 1, and monitoring wavelength is 560nm.Test condition and Fig. 2
It is identical.As shown in figure 3, excitation spectrum has in the range of 250-410nm absorbing, absorption edge is with Bi3+Doping concentration increase
There is red shift greatly, show that sample has strong and wide absorption in ultra-violet (UV) band, and with Bi3+Doping concentration increase and increase
By force.
Fig. 4 is the monitoring wavelength dependency spectrum of proportioning (3) sample of embodiment 1.Test condition is identical with Fig. 2.As schemed
4, as monitoring wavelength reduces, excite peak position from 350nm blue shift to 326nm.
Fig. 5 is the excitation wavelength dependence spectrum of proportioning (3) sample of embodiment 1.Test condition is identical with Fig. 2.As schemed
5, as excitation wavelength increases, emission peak positions are from 540nm red shift to 580nm.
Embodiment 2
Lanthanum sesquioxide, boric acid, tungstic acid, bismuth nitrate are chosen as initial compounds raw material, is matched somebody with somebody by each element mole
Compare La:B:W:Bi=2.955:1:1:0.045, correspondence x=1.5%；Four kinds of raw materials of compound are weighed respectively, and mixture is ground
After well mixed, load corundum crucible, crucible is placed in corundum boat, be put into high-temperature box type electric furnace.Strict control heating rate,
In 650 DEG C of pre-burning 6h.Room temperature is cooled to, is ground；Then 12h is calcined at 1100 DEG C, after cooling to room temperature with the furnace, grinding is
Obtain bismuth doping Tungstoborate yellow fluorescent material.XRD spectrum analysis shows its be La3BWO9Crystalline phase.The spectral quality of fluorescent material is same
Embodiment 1 is similar to.
Embodiment 3
Lanthanum sesquioxide, boric acid, tungstic acid, bismuth nitrate are chosen as initial compounds raw material, is matched somebody with somebody by each element mole
Compare La:B:W:Bi=2.910:1:1:0.090, correspondence x=3.0%；Four kinds of raw materials of compound are weighed respectively, and mixture is ground
After well mixed, load corundum crucible, crucible is placed in corundum boat, be put into high-temperature box type electric furnace.Strict control heating rate,
In 600 DEG C of pre-burning 8h.Room temperature is cooled to, is ground；Then 8h is calcined at 1150 DEG C, after cooling to room temperature with the furnace, grinding is
Obtain bismuth doping Tungstoborate yellow fluorescent material.XRD spectrum analysis shows its be La3BWO9Crystalline phase.The spectral quality of fluorescent material is same
Embodiment 1 is similar to.
Embodiment 4
Lanthanum sesquioxide, diboron trioxide, tungstic acid, bismuth oxide are chosen as initial compounds raw material, by each
Element mol ratio La:B:W:Bi=2.970:1:1:0.030, correspondence x=1.0%；Four kinds of raw materials of compound are weighed respectively, are mixed
Compound it is ground it is well mixed after, load corundum crucible, crucible is placed in corundum boat, be put into high-temperature box type electric furnace.Strict control
Heating rate processed, in 550 DEG C of pre-burning 12h.Room temperature is cooled to, is ground；Then 8h is calcined at 1100 DEG C, cools to room with the furnace
Wen Hou, grinding obtains final product bismuth doping Tungstoborate yellow fluorescent material.XRD spectrum analysis shows its be La3BWO9Crystalline phase.Fluorescent material
Spectral quality it is similar with embodiment 1.
Embodiment 5
Lanthanum sesquioxide, boric acid, ammonium tungstate, bismuth oxide are chosen as initial compounds raw material, by each element mole
Proportioning La:B:W:Bi=2.970:1:1:0.030, correspondence x=1.0%；Four kinds of raw materials of compound are weighed respectively, and mixture is through grinding
After mill is well mixed, load corundum crucible, crucible is placed in corundum boat, be put into high-temperature box type electric furnace.Strict control heats up fast
Rate, in 500 DEG C of pre-burning 12h.Room temperature is cooled to, is ground；Then 4h is calcined at 1150 DEG C, after cooling to room temperature with the furnace, is ground
Mill obtains final product bismuth doping Tungstoborate yellow fluorescent material.XRD spectrum analysis shows its be La3BWO9Crystalline phase.The light spectrality of fluorescent material
Matter is similar with embodiment 1.
Embodiment 6
Lanthanum nitrate, boric acid, tungstic acid, bismuth oxide are chosen as initial compounds raw material, is matched somebody with somebody by each element mole
Compare La:B:W:Bi=2.925:1:1:0.075, correspondence x=2.5%；Four kinds of raw materials of compound are weighed respectively, and mixture is ground
After well mixed, load corundum crucible, crucible is placed in corundum boat, be put into high-temperature box type electric furnace.Strict control heating rate,
In 700 DEG C of pre-burning 5h.Room temperature is cooled to, is ground；Then 6h is calcined at 1100 DEG C, after cooling to room temperature with the furnace, grinding is
Obtain bismuth doping Tungstoborate yellow fluorescent material.XRD spectrum analysis shows its be La3BWO9Crystalline phase.The spectral quality of fluorescent material is same
Embodiment 1 is similar to.
Embodiment 7
Lanthanum nitrate, boric acid, ammonium tungstate, bismuth nitrate are chosen as initial compounds raw material, by each element mol ratio La:B:
W:Bi=2.985:1:1:0.015, correspondence x=0.5%；Four kinds of raw materials of compound are weighed respectively, and the ground mixing of mixture is equal
After even, load corundum crucible, crucible is placed in corundum boat, be put into high-temperature box type electric furnace.Strict control heating rate, 400
DEG C pre-burning 8h.Room temperature is cooled to, is ground；Then 12h is calcined at 1000 DEG C, after cooling to room temperature with the furnace, grinding obtains final product bismuth
Doping Tungstoborate yellow fluorescent material.XRD spectrum analysis shows its be La3BWO9Crystalline phase.The spectral quality of fluorescent material is with implementation
Example 1 is similar to.
Embodiment 8
Lanthanum sesquioxide, diboron trioxide, ammonium tungstate, bismuth nitrate are chosen as initial compounds raw material, is rubbed by each element
You are proportioning La:B:W:Bi=2.970:1:1:0.030, correspondence x=1.0%；Four kinds of raw materials of compound, mixture warp are weighed respectively
After ground and mixed is uniform, load corundum crucible, crucible is placed in corundum boat, be put into high-temperature box type electric furnace.Strict control heats up
Speed, in 450 DEG C of pre-burning 12h.Room temperature is cooled to, is ground；Then 4h is calcined at 1150 DEG C, after cooling to room temperature with the furnace,
Grinding obtains final product bismuth doping Tungstoborate yellow fluorescent material.XRD spectrum analysis shows its be La3BWO9Crystalline phase.The spectrum of fluorescent material
Property is similar with embodiment 1.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by the embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (7)
1. a kind of bismuth doping Tungstoborate yellow fluorescent powder, it is characterised in that chemical general formula is La3(1-x)BWO9:3xBi3+, wherein
X is molar fraction, and 0<x≤0.1.
2. a kind of bismuth adulterates the preparation method of Tungstoborate yellow fluorescent powder, it is characterised in that comprise the following steps：
(1) by chemical general formula La3(1-x)BWO9:3xBi3+, wherein x is molar fraction, and 0<X≤0.1, weighs the change containing La elements
Compound, the compound containing B element, the compound containing W elements, the compound ground and mixed containing Bi elements are uniform, obtain mixture
Material；
(2) mixed material for obtaining step (1) is cooled to room temperature in 400-800 DEG C of pre-burning 4-12h, is ground；Then exist
1000-1300 DEG C of calcining 4-12h, after cooling to room temperature with the furnace, grinding obtains final product bismuth doping Tungstoborate yellow fluorescent powder.
3. bismuth according to claim 2 adulterates the preparation method of Tungstoborate yellow fluorescent powder, it is characterised in that described to contain
The compound of La elements is lanthanum sesquioxide or lanthanum nitrate.
4. bismuth according to claim 2 adulterates the preparation method of Tungstoborate yellow fluorescent powder, it is characterised in that described to contain
The compound of B element is boric acid or diboron trioxide.
5. bismuth according to claim 2 adulterates the preparation method of Tungstoborate yellow fluorescent powder, it is characterised in that described to contain
The compound of W elements is tungstic acid or ammonium tungstate.
6. bismuth according to claim 2 adulterates the preparation method of Tungstoborate yellow fluorescent powder, it is characterised in that described to contain
The compound of Bi elements is bismuth oxide or bismuth nitrate.
7. bismuth described in claim 1 adulterates the application of Tungstoborate yellow fluorescent powder, it is characterised in that for prepare it is ultraviolet-
The white light LED part that near ultraviolet LED chip is excited.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942929A (en) * | 2012-11-30 | 2013-02-27 | 苏州大学 | Ytterbium ion Yb<3+> activated borotungstate upconversion luminescent material and preparation method thereof |
| CN103289695A (en) * | 2013-05-13 | 2013-09-11 | 上海师范大学 | Efficient red fluorescent material and preparation method thereof |
| CN103497768A (en) * | 2013-09-29 | 2014-01-08 | 华南理工大学 | Near-ultraviolet excited molybdenum-tungsten borate red fluorescent powder and preparation method thereof |
-
2016
- 2016-11-14 CN CN201610997436.1A patent/CN106753370B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942929A (en) * | 2012-11-30 | 2013-02-27 | 苏州大学 | Ytterbium ion Yb<3+> activated borotungstate upconversion luminescent material and preparation method thereof |
| CN103289695A (en) * | 2013-05-13 | 2013-09-11 | 上海师范大学 | Efficient red fluorescent material and preparation method thereof |
| CN103497768A (en) * | 2013-09-29 | 2014-01-08 | 华南理工大学 | Near-ultraviolet excited molybdenum-tungsten borate red fluorescent powder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115011341A (en) * | 2022-06-06 | 2022-09-06 | 渤海大学 | Fluorescent powder emitting broadband green light and preparation method thereof |
| CN115011341B (en) * | 2022-06-06 | 2023-08-22 | 渤海大学 | Fluorescent powder capable of emitting broadband green light and preparation method thereof |
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