CN106753361B - 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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- CN106753361B CN106753361B CN201610997434.2A CN201610997434A CN106753361B CN 106753361 B CN106753361 B CN 106753361B CN 201610997434 A CN201610997434 A CN 201610997434A CN 106753361 B CN106753361 B CN 106753361B
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- fluorescent powder
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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
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- 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 bismuths to adulterate tungstate red fluorescent powder, chemical general formula Zn1‑xWO4:xBi3+, wherein x is molar fraction, and 0 < x≤0.05.The invention also discloses the preparation methods of the fluorescent powder, by the corresponding compound of the weighed each element of chemical composition general formula；In 800-1200 DEG C of calcining 4-12h after being ground.The fluorescent powder can effectively be excited by the ultraviolet light within the scope of 250-410nm, be shone within the scope of 450-850nm, and center is located at 665nm, have absorption in ultra-violet (UV) band, in blue light and green Region without absorption, can be used for preparing the white light LED part of near ultraviolet LED chip excitation.
Description
Technical field
The present invention relates to field of light emitting materials, in particular to a kind of bismuth doping tungstate red fluorescent powder and preparation method,
Using.
Background technique
In recent years, as climate change and environmental problem increasingly show, people are look for substitute fossil fuels and do not discharge
The energy of carbon dioxide.White light LEDs are concerned due to the superior performance such as efficient, compact, durable and environmentally friendly.White light
The popularization and use of LED are extremely important, can reduce the use of global power demand and fossil fuel significantly, reduce carbon dioxide
The discharge of isothermal chamber gas.Currently, white light LEDs have been widely used in normal lighting, traditional illumination light is gradually replaced
Source --- incandescent lamp, fluorescent lamp.
The white light LEDs (abbreviation pc-WLEDs) of fluorescent powder conversion are considered as next-generation novel illumination light source.Currently, white light
LED component generallys use blue-light LED chip and YAG:Ce phosphor combination encapsulates.But it is this combination it is red due to lacking
Light ingredient, colour rendering index is relatively low (Ra<80), and colour temperature is higher (Tc>7000K), hinders it and expands to some other application field.
In addition, blue-light LED chip is different from the heat ageing rate of YAG:Ce fluorescent powder, with the extension of white light LED part runing time,
It, which shines, will be gradually deviated from white light.
To solve the above-mentioned problems, researcher begins trying new encapsulation scheme, using ultraviolet-near ultraviolet LED chip
(350-410nm) is combined with red, green, blue three primary colors fluorescent powder generates white light.Several fluorescent powder is coated in UV LED chip,
Chip excitated fluorescent powder forms red, green, blue and shines, and three coloured light is superimposed to obtain white light.This scheme can obtain colour rendering height,
Color difference is small and the white light of adjustable color, overcomes blue-light LED chip and YAG:Ce phosphor combination problems faced.New departure is wanted
It asks red, green, blue fluorescent powder that must have absorption in 350-410nm, in visible region without absorption, and is efficiently sent out in visible region
Light.Existing fluorescent powder, especially red fluorescence powder, such as (Ba, Sr)2Si5N8:Eu2+, (Sr, Ca) AlSiN3:Eu2+, (Sr,
Ca)S:Eu2+, partially blue or green emitting phosphor in addition to also having absorption in blue light and green Region other than there is absorption in ultra-violet (UV) band
It shines by red fluorescence powder reabsorption, causes luminous efficiency to reduce, it is difficult to meet new departure requirement.Therefore, exploitation is in ultra-violet (UV) band
(especially 350-410nm) has absorption, the red fluorescence material of blue light or green Region without absorption be field of light emitting materials urgently
The great Scientific And Technical Problems solved.
Summary of the invention
In order to overcome the disadvantages mentioned above and deficiency of the prior art, the purpose of the present invention is to provide a kind of bismuths to adulterate tungstates
Red fluorescence powder has absorption in ultra-violet (UV) band, in blue light and green Region without absorption, has in red light district luminous.
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 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, comprising the following steps:
It (1) 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 of the element containing W and the compound of the element containing Bi, ground and mixed is uniform, obtains mixed material；
(2) mixed material for obtaining step (1) after being cooled to room temperature, is ground in 800-1200 DEG C of calcining 4-12h to obtain the final product
Bismuth adulterates tungstate red fluorescent powder.
The compound of the element containing Zn is zinc oxide, zinc acetate or zinc nitrate.
The compound of the element containing W is tungstic acid or ammonium tungstate.
The compound of the element containing Bi is bismuth oxide or bismuth nitrate.
The application of the bismuth doping tungstate red fluorescent powder, is used to prepare the white light LEDs of near ultraviolet LED chip excitation
Device.
The principle of the present invention is as follows: crystallographic data shows, ZnWO4Crystal belongs to monoclinic system, the space P2/c (No.13)
Group, cell parameterZnWO4In crystal W and
Zn only has an independent crystallographic sites, is hexa-coordinate.According to radius and the charge principle of similitude, Bi3+Replace Zn case,
Generate emitting red light.
Compared with prior art, the present invention has the following advantages and beneficial effects:
(1) bismuth doping Tungstate fluorescent powder of the invention has wide excitation within the scope of 250-410nm, in blue light or green
Light area does not absorb.
(2) bismuth of the invention doping Tungstate fluorescent powder is under ultraviolet excitation, and shine covering 450-850nm, centre bit
In~665nm.
(3) bismuth of the invention doping tungstates phosphor structure is stablized, and synthetic method is simple, is convenient for large-scale production.
(4) bismuth of the invention doping Tungstate fluorescent powder can be applied to the white light LED part envelope of near ultraviolet LED chip excitation
Dress.
Detailed description of the invention
Fig. 1 is proportion (1)-(6) sample X-ray powder diffraction pattern of embodiment 1.
Fig. 2 is proportion (1)-(6) sample emission spectrum of embodiment 1, excitation wavelength 365nm.
Fig. 3 is proportion (1)-(6) sample excitation spectrum of embodiment 1, monitors wavelength 665nm.
Fig. 4 is proportion (1)-(6) sample part excitation spectrum of embodiment 1, monitors wavelength 665nm.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, embodiments of the present invention are not limited thereto.
Embodiment 1
Zinc oxide, tungstic acid, bismuth oxide are chosen as initial compounds raw material to divide by each element mol ratio
Three kinds of raw materials of compound also known as are taken, totally 6 groups, are matched as follows:
(1) Zn:W:Bi=0.995:1:0.005, corresponding x=0.5%；
(2) Zn:W:Bi=0.990:1:0.010, corresponding x=1.0%；
(3) Zn:W:Bi=0.985:1:0.015, corresponding x=1.5%；
(4) Zn:W:Bi=0.980:1:0.020, corresponding x=2.0%；
(5) Zn:W:Bi=0.975:1:0.025, corresponding x=2.5%；
(6) Zn:W:Bi=0.970:1:0.030, corresponding x=3.0%
After the ground mixing of mixture, it is packed into corundum crucible, crucible is placed in corundum boat, high-temperature box type electric furnace is put into.
Strict control heating rate, in 900 DEG C of calcining 4h.After being cooled to room temperature, grinds and adulterate tungstate red fluorescent material up to bismuth.
Fig. 1 is proportion (1)-(6) sample X-ray powder diffraction pattern of embodiment 1.Using German Brooker company
(Bruker) D8 ADVANCE type x-ray powder diffraction instrument measures.Radiation source is Cu target K alpha rayIt surveys
Voltage 40kV is tried, electric current 40mA is tested, scans 0.02 °/step of step width, scanning speed 0.12s/step.XRD spectrum analysis shows
It is ZnWO4Phase, belongs to monoclinic system, and dopping effect does not introduce other object phases or impurity.
Fig. 2 is proportion (1)-(6) sample emission spectrum of embodiment 1, excitation wavelength 365nm.Fourth is liked using Britain
The measurement of fort company (Edinburgh) FLS920 type stable state moment Fluorescence Spectrometer.Using the xenon lamp of 450W as excitation light source, when outfit
Between correct single photon counting card (TCSPC), the red quick photomultiplier tube (PMT) of thermoelectric cold, TM300 excitation monochromator and double TM300
Emit monochromator.As shown in Figure 2, under 365nm ultraviolet excitation, sample all can produce the feux rouges that peak value is located near 665nm
Transmitting, wavelength cover 450-850nm, corresponding Bi3+'s3P1→1S0Transition.
Fig. 3 is proportion (1)-(6) sample excitation spectrum of embodiment 1, and monitoring wavelength is 665nm.Test condition and Fig. 2
It is identical.It is absorbed as shown in figure 3, the corresponding excitation spectrum of 665nm feux rouges has within the scope of 250-410nm, peak value is located at 300nm
And 365nm, it is derived from matrix ZnWO respectively4And Bi3+Absorption.The absorption of matrix is relative to Bi3+It is relatively strong, and with Bi3+Content
Increase, Bi3+Absorption enhanced, show sample ultra-violet (UV) band have strong and wide absorption.
Fig. 4 is proportion (1)-(6) sample part excitation spectrum of embodiment 1, and monitoring wavelength is 665nm.Test condition
It is identical as Fig. 2.It is absorbed as shown in figure 3, the corresponding excitation spectrum of 665nm feux rouges has within the scope of 340-420nm, peak value is located at
365nm is derived 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, corresponding 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, high-temperature box type electric furnace is put into.Strict control heating rate is calcined at 800 DEG C
12h.After being cooled to room temperature, grinds and adulterate tungstate red fluorescent material up to bismuth.XRD spectrum is analysis shows it is ZnWO4It is brilliant
Phase.The spectral property of fluorescent powder 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, corresponding 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, high-temperature box type electric furnace is put into.Strict control heating rate is calcined at 1000 DEG C
5h.After being cooled to room temperature, grinds and adulterate tungstate red fluorescent material up to bismuth.XRD spectrum is analysis shows it is ZnWO4It is brilliant
Phase.The spectral property of fluorescent powder 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, corresponding x=2.5%；Three kinds of raw materials of compound are weighed respectively, after the ground mixing of mixture, are packed into rigid
Crucible is placed in corundum boat, is put into high-temperature box type electric furnace by beautiful crucible.Strict control heating rate, in 1150 DEG C of calcining 4h.It is cold
But tungstate red fluorescent material is adulterated up to bismuth to grinding after room temperature.XRD spectrum is analysis shows it is ZnWO4Crystal phase.Fluorescence
The spectral property 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, corresponding x=1.0%；Three kinds of raw materials of compound are weighed respectively, after the ground mixing of mixture, are packed into
Crucible is placed in corundum boat, is put into high-temperature box type electric furnace by corundum crucible.Strict control heating rate, in 900 DEG C of calcining 4h.
After being cooled to room temperature, grinds and adulterate tungstate red fluorescent material up to bismuth.XRD spectrum is analysis shows it is MWO4Crystal phase.It is glimmering
The spectral property 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, corresponding x=0.5%；Three kinds of raw materials of compound are weighed respectively, after the ground mixing of mixture, are packed into
Crucible is placed in corundum boat, is put into high-temperature box type electric furnace by corundum crucible.Strict control heating rate, in 950 DEG C of calcining 5h.
After being cooled to room temperature, grinds and adulterate tungstate red fluorescent material up to bismuth.XRD spectrum is analysis shows it is ZnWO4Crystal phase.It is glimmering
The spectral property of light powder is similar with embodiment 1.
Embodiment 7
It chooses zinc nitrate, ammonium tungstate, bismuth oxide and makees initial compounds raw material, by each element mol ratio Zn:W:Bi
=0.960:1:0.040, corresponding x=4.0%；Three kinds of raw materials of compound are weighed respectively, after the ground mixing of mixture, are packed into rigid
Crucible is placed in corundum boat, is put into high-temperature box type electric furnace by beautiful crucible.Strict control heating rate, in 1050 DEG C of calcining 4h.It is cold
But tungstate red fluorescent material is adulterated up to bismuth to grinding after room temperature.XRD spectrum is analysis shows it is ZnWO4Crystal phase.Fluorescence
The spectral property of powder is similar in embodiment 1.
Embodiment 8
It chooses zinc nitrate, ammonium tungstate, bismuth nitrate and makees initial compounds raw material, by each element mol ratio M:W:Bi=
0.990:1:0.010, corresponding x=1.0%；Three kinds of raw materials of compound are weighed respectively, after the ground mixing of mixture, are packed into corundum
Crucible is placed in corundum boat, is put into high-temperature box type electric furnace by crucible.Strict control heating rate, in 1150 DEG C of calcining 6h.It is cooling
To room temperature, grinds and adulterate tungstate red fluorescent material up to bismuth.XRD spectrum is analysis shows it is ZnWO4Crystal phase.Fluorescent powder
Spectral property it is similar in embodiment 1.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by the embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (6)
1. a kind of bismuth adulterates tungstate red fluorescent powder, which is characterized in that chemical general formula Zn1-xWO4:xBi3+, wherein x is to rub
That score, and 0 < x≤0.05.
2. a kind of preparation method of bismuth doping tungstate red fluorescent powder, which comprises the following steps:
It (1) is Zn by chemical general formula1-xWO4:xBi3+, wherein x is molar fraction, and 0 < x≤0.05 weighs the change of the element containing Zn
Object, the compound of the element containing W and the compound of the element containing Bi are closed, ground and mixed is uniform, obtains mixed material；
(2) mixed material for obtaining step (1) after being cooled to room temperature, grinds and mixes up to bismuth in 800-1200 DEG C of calcining 4-12h
Miscellaneous tungstate red fluorescent powder.
3. the preparation method of bismuth doping tungstate red fluorescent powder according to claim 2, which is characterized in that described to contain Zn
The compound of element is zinc oxide, zinc acetate or zinc nitrate.
4. the preparation method of bismuth doping tungstate red fluorescent powder according to claim 2, which is characterized in that described to contain W
The compound of element is tungstic acid or ammonium tungstate.
5. the preparation method of bismuth doping tungstate red fluorescent powder according to claim 2, which is characterized in that described to contain Bi
The compound of element is bismuth oxide or bismuth nitrate.
6. the application of bismuth doping tungstate red fluorescent powder described in claim 1, which is characterized in that be used to prepare near ultraviolet
The white light LED part of LED chip excitation.
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| CN115724466B (en) * | 2022-10-28 | 2023-07-18 | 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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