CN106753361A - A kind of bismuth doping tungstate red fluorescent powder and preparation method, application - Google Patents
A kind of bismuth doping tungstate red fluorescent powder and preparation method, application Download PDFInfo
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- CN106753361A CN106753361A CN201610997434.2A CN201610997434A CN106753361A CN 106753361 A CN106753361 A CN 106753361A CN 201610997434 A CN201610997434 A CN 201610997434A CN 106753361 A CN106753361 A CN 106753361A
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- bismuth
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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
- C09K11/74—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing arsenic, antimony or bismuth
- C09K11/7457—Vanadates; Chromates; Molybdates; Tungstates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
Abstract
The invention discloses a kind of bismuth doping tungstate red fluorescent powder, chemical general formula is Zn1‑xWO4:xBi3+, wherein x is molar fraction, and 0<x≤0.05.The invention also discloses the preparation method of the fluorescent material, the corresponding compound of each element is weighed by chemical composition formula；After being ground 4 12h are calcined at 800 1200 DEG C.The fluorescent material can effectively be excited by the ultraviolet light in the range of 250 410nm, be lighted within the scope of 450 850nm, be centrally located at 665nm, have absorption in ultra-violet (UV) band, in blue light and green Region without absorption, can be used to prepare the white light LED part that near ultraviolet LED chip is excited.
Description
Technical field
The present invention relates to field of light emitting materials, more particularly to a kind of bismuth doping tungstate red fluorescent powder and preparation method,
Using.
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), it is hindered to be expanded to some other application field.
Additionally, blue-light LED chip and YAG:The heat ageing speed of Ce fluorescent material is different, with the extension of white light LED part run time,
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 three primary colors fluorescent powder.Several fluorescent material is coated on UV LED chips,
Chip excitated fluorescent powder forms red, green, blue and lights, and three coloured light is superimposed to obtain white light.It is high that this scheme can obtain colour rendering,
Aberration is small and white light of adjustable color, overcomes blue-light LED chip and YAG:Ce phosphor combination problems faceds.New departure will
Seeking red, green, blue fluorescent material must have absorption in 350-410nm, in visible region without absorption, and efficiently be sent out in visible region
Light.Existing fluorescent material, especially red fluorescence powder, such as (Ba, Sr)2Si5N8:Eu2+, (Sr, Ca) AlSiN3:Eu2+, (Sr,
Ca)S:Eu2+, in addition to having absorption in ultra-violet (UV) band, also there is absorption in blue light and green Region, part is blue or green emitting phosphor
Light by red fluorescence powder reabsorption, cause luminous efficiency to reduce, it is difficult to meet new departure requirement.Therefore, exploitation is in ultra-violet (UV) band
(particularly 350-410nm) has absorption, blue light or green Region without the red fluorescence material for absorbing be field of light emitting materials urgently
The great Scientific And Technical Problems for solving.
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 tungstates
Red fluorescence powder, has absorption in ultra-violet (UV) band, in blue light and green Region without absorption, has luminous in red light district.
The purpose of the present invention is achieved through the following technical solutions：
A kind of bismuth doping tungstate red fluorescent powder, chemical general formula is Zn1-xWO4:xBi3+, wherein x is molar fraction, and 0
<x≤0.05。
A kind of preparation method of bismuth doping tungstate red fluorescent powder, comprises the following steps：
(1) it is Zn by chemical general formula1-xWO4:xBi3+, wherein x is molar fraction, and 0<X≤0.05, weighs element containing Zn
Compound, the compound containing W elements and the compound containing Bi elements, ground and mixed is uniform, obtains mixed material；
(2) mixed material for obtaining step (1) calcines 4-12h at 800-1200 DEG C, and after being cooled to room temperature, grinding is obtained final product
Bismuth doping tungstate red fluorescent powder.
The compound containing Zn elements is zinc oxide, zinc acetate or zinc nitrate.
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 tungstate red fluorescent powder, for preparing the white light LEDs that near ultraviolet LED chip is excited
Device.
Principle of the invention is as follows：Crystallographic data shows, ZnWO4Crystal belongs to monoclinic system, P2/c (No.13) space
Group, cell parameterZnWO4In crystal W and
Zn only has an independent crystallographic sites, is hexa-coordinate.According to radius and the electric charge principle of similitude, Bi3+Substitution Zn cases,
Produce emitting red light.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) bismuth doping Tungstate fluorescent powder of the invention is excited in the range of 250-410nm with wide, in blue light or green
Light area does not absorb.
(2) bismuth of the invention adulterates Tungstate fluorescent powder under ultraviolet excitation, and light covering 450-850nm, centre bit
In~665nm.
(3) bismuth doping tungstates phosphor structure stabilization of the invention, synthetic method is simple, is easy to large-scale production.
(4) bismuth doping Tungstate fluorescent powder of the invention can be applied to the white light LED part envelope that near ultraviolet LED chip is excited
Dress.
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 365nm.
Fig. 3 is the excitation spectrum of proportioning (1)-(6) sample of embodiment 1, monitoring wavelength 665nm.
Fig. 4 is the part excitation spectrum of proportioning (1)-(6) sample of embodiment 1, monitoring wavelength 665nm.
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
Zinc oxide, tungstic acid, bismuth oxide are chosen as initial compounds raw material, by each element mol ratio, point
Another name takes three kinds of raw materials of compound, totally 6 groups, matches as follows：
(1)Zn:W:Bi=0.995:1:0.005, correspondence x=0.5%；
(2)Zn:W:Bi=0.990:1:0.010, correspondence x=1.0%；
(3)Zn:W:Bi=0.985:1:0.015, correspondence x=1.5%；
(4)Zn:W:Bi=0.980:1:0.020, correspondence x=2.0%；
(5)Zn:W:Bi=0.975:1:0.025, correspondence x=2.5%；
(6)Zn:W:Bi=0.970:1:0.030, correspondence x=3.0%
After the ground mixing of mixture, load corundum crucible, crucible is placed in corundum boat, be put into high-temperature box type electric furnace.
Strict control heating rate, 4h is calcined at 900 DEG C.After being cooled to room temperature, grinding obtains final product the bismuth tungstate red fluorescent material of doping.
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, scanning step width 0.02 °/step, sweep speed 0.12s/step.XRD spectrum analysis shows
It is ZnWO4Phase, 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 365nm.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 365nm ultraviolet excitations, sample can all produce the feux rouges that peak value is located near 665nm
Transmitting, wavelength covering 450-850nm, correspondence Bi3+'s3P1→1S0Transition.
Fig. 3 is the excitation spectrum of proportioning (1)-(6) sample of embodiment 1, and monitoring wavelength is 665nm.Test condition and Fig. 2
It is identical.As shown in figure 3, the corresponding excitation spectrum of 665nm feux rouges has in the range of 250-410nm absorbing, peak value is located at 300nm
And 365nm, matrix ZnWO is come from respectively4And Bi3+Absorption.The absorption of matrix is relative to Bi3+It is relatively strong, and with Bi3+Content
Increase, Bi3+Absorption strengthened, show that sample has strong and wide absorption in ultra-violet (UV) band.
Fig. 4 is the part excitation spectrum of proportioning (1)-(6) sample of embodiment 1, and monitoring wavelength is 665nm.Test condition
It is identical with Fig. 2.As shown in figure 3, the corresponding excitation spectrum of 665nm feux rouges has in the range of 340-420nm absorbing, peak value is located at
365nm, from Bi3+'s1S0→3P1Transition.
Embodiment 2
Zinc oxide, tungstic acid, bismuth oxide are chosen as initial compounds raw material, by each element mol ratio Zn:
W:Bi=0.995:1:0.005, correspondence x=0.5%；Three kinds of raw materials of compound are weighed respectively, after the ground mixing of mixture, dress
Enter corundum crucible, crucible is placed in corundum boat, be put into high-temperature box type electric furnace.Strict control heating rate, in 800 DEG C of calcinings
12h.After being cooled to room temperature, grinding obtains final product the bismuth tungstate red fluorescent material of doping.XRD spectrum analysis shows its be ZnWO4It is brilliant
Phase.The spectral quality of fluorescent material is similar with embodiment 1.
Embodiment 3
Zinc acetate, tungstic acid, bismuth oxide are chosen as initial compounds raw material, by each element mol ratio Zn:
W:Bi=0.985:1:0.015, correspondence x=1.5%；Three kinds of raw materials of compound are weighed respectively, after the ground mixing of mixture, dress
Enter corundum crucible, crucible is placed in corundum boat, be put into high-temperature box type electric furnace.Strict control heating rate, in 1000 DEG C of calcinings
5h.After being cooled to room temperature, grinding obtains final product the bismuth tungstate red fluorescent material of doping.XRD spectrum analysis shows its be ZnWO4It is brilliant
Phase.The spectral quality of fluorescent material is similar with embodiment 1.
Embodiment 4
Zinc oxide, tungstic acid, bismuth nitrate are chosen as initial compounds raw material, by each element mol ratio Zn:W:Bi
=0.975:1:0.025, correspondence x=2.5%；Three kinds of raw materials of compound are weighed respectively, after the ground mixing of mixture, load firm
Beautiful crucible, crucible is placed in corundum boat, is put into high-temperature box type electric furnace.Strict control heating rate, 4h is calcined at 1150 DEG C.It is cold
But to after room temperature, grinding obtains final product bismuth and adulterates tungstate red fluorescent material.XRD spectrum analysis shows its be ZnWO4Crystalline phase.Fluorescence
The spectral quality of powder is similar with embodiment 1.
Embodiment 5
Zinc oxide, ammonium tungstate, bismuth oxide are chosen as initial compounds raw material, by each element mol ratio Zn:W:
Bi=0.990:1:0.010, correspondence x=1.0%；Three kinds of raw materials of compound are weighed respectively, after the ground mixing of mixture, are loaded
Corundum crucible, crucible is placed in corundum boat, is put into high-temperature box type electric furnace.Strict control heating rate, 4h is calcined at 900 DEG C.
After being cooled to room temperature, grinding obtains final product the bismuth tungstate red fluorescent material of doping.XRD spectrum analysis shows its be MWO4Crystalline phase.It is glimmering
The spectral quality of light powder is similar with embodiment 1.
Embodiment 6
Zinc acetate, ammonium tungstate, bismuth oxide are chosen as initial compounds raw material, by each element mol ratio Zn:W:
Bi=0.995:1:0.005, correspondence x=0.5%；Three kinds of raw materials of compound are weighed respectively, after the ground mixing of mixture, are loaded
Corundum crucible, crucible is placed in corundum boat, is put into high-temperature box type electric furnace.Strict control heating rate, 5h is calcined at 950 DEG C.
After being cooled to room temperature, grinding obtains final product the bismuth tungstate red fluorescent material of doping.XRD spectrum analysis shows its be ZnWO4Crystalline phase.It is glimmering
The spectral quality of light powder is similar with embodiment 1.
Embodiment 7
Choose zinc nitrate, ammonium tungstate, bismuth oxide and make initial compounds raw material, by each element mol ratio Zn:W:Bi
=0.960:1:0.040, correspondence x=4.0%；Three kinds of raw materials of compound are weighed respectively, after the ground mixing of mixture, load firm
Beautiful crucible, crucible is placed in corundum boat, is put into high-temperature box type electric furnace.Strict control heating rate, 4h is calcined at 1050 DEG C.It is cold
But to after room temperature, grinding obtains final product bismuth and adulterates tungstate red fluorescent material.XRD spectrum analysis shows its be ZnWO4Crystalline phase.Fluorescence
The spectral quality of powder is similar to in embodiment 1.
Embodiment 8
Choose zinc nitrate, ammonium tungstate, bismuth nitrate and make initial compounds raw material, by each element mol ratio M:W:Bi=
0.990:1:0.010, correspondence x=1.0%；Three kinds of raw materials of compound are weighed respectively, after the ground mixing of mixture, load corundum
Crucible, crucible is placed in corundum boat, is put into high-temperature box type electric furnace.Strict control heating rate, 6h is calcined at 1150 DEG C.Cooling
To room temperature, grinding obtains final product the bismuth tungstate red fluorescent material of doping.XRD spectrum analysis shows its be ZnWO4Crystalline phase.Fluorescent material
Spectral quality with embodiment 1 be similar to.
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 (6)
1. a kind of bismuth doping tungstate red fluorescent powder, it is characterised in that chemical general formula is Zn1-xWO4:xBi3+, wherein x is to rub
That fraction, and 0<x≤0.05.
2. a kind of bismuth adulterates the preparation method of tungstate red fluorescent powder, it is characterised in that comprise the following steps：
(1) it is Zn by chemical general formula1-xWO4:xBi3+, wherein x is molar fraction, and 0<X≤0.05, weighs the change containing Zn elements
Compound, the compound containing W elements and the compound containing Bi elements, ground and mixed are uniform, obtain mixed material；
(2) mixed material for obtaining step (1) calcines 4-12h at 800-1200 DEG C, and after being cooled to room temperature, grinding obtains final product bismuth and mixes
Miscellaneous tungstate red fluorescent powder.
3. bismuth according to claim 2 adulterates the preparation method of tungstate red fluorescent powder, it is characterised in that described containing Zn
The compound of element is zinc oxide, zinc acetate or zinc nitrate.
4. bismuth according to claim 2 adulterates the preparation method of tungstate red fluorescent powder, it is characterised in that described containing W
The compound of element is tungstic acid or ammonium tungstate.
5. bismuth according to claim 2 adulterates the preparation method of tungstate red fluorescent powder, it is characterised in that described containing Bi
The compound of element is bismuth oxide or bismuth nitrate.
6. the application of the bismuth doping tungstate red fluorescent powder described in claim 1, it is characterised in that for preparing near ultraviolet
The white light LED part that LED chip is excited.
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Cited By (2)
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| CN115011341A (en) * | 2022-06-06 | 2022-09-06 | 渤海大学 | Fluorescent powder emitting broadband green light and preparation method thereof |
| CN115724466A (en) * | 2022-10-28 | 2023-03-03 | 佛山市明事达智能材料有限公司 | Zinc oxide composite material and preparation method and application thereof |
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