CN107245335B - A kind of wolframic acid alkali white light emitting material and its preparation method and application - Google Patents
A kind of wolframic acid alkali white light emitting material and its preparation method and application Download PDFInfo
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- CN107245335B CN107245335B CN201710401156.4A CN201710401156A CN107245335B CN 107245335 B CN107245335 B CN 107245335B CN 201710401156 A CN201710401156 A CN 201710401156A CN 107245335 B CN107245335 B CN 107245335B
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- 239000000463 material Substances 0.000 title claims abstract description 30
- 239000002253 acid Substances 0.000 title claims abstract description 10
- 239000003513 alkali Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 230000005284 excitation Effects 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 6
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims description 4
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium (III) oxide Inorganic materials [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Inorganic materials [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 3
- 238000002485 combustion reaction Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 12
- 230000003760 hair shine Effects 0.000 abstract description 6
- 150000002500 ions Chemical class 0.000 description 13
- 238000000295 emission spectrum Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910004415 SrWO4 Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- 230000005283 ground state Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 241000083879 Polyommatus icarus Species 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000005472 transition radiation Effects 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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7776—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 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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- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Luminescent Compositions (AREA)
Abstract
A kind of wolframic acid alkali white light emitting material and its preparation method and application, chemical formula Ba0.05Sr0.94‑zWO40.01Tm3+zDy3+, z=0.01~0.06.It is shone under the excitation wavelength of 352~366nm in white light area, under especially 354nm excitations, when z=0.03, fluorescent powder shines closest to standard white light, and chromaticity coordinates is (0.321,0.347), colour temperature 6000K.Therefore, Ba of the invention0.05Sr0.94‑zWO4 0.01Tm3+zDy3+It can be used as the application material of near ultraviolet chip excited white light.
Description
Technical field
The present invention relates to luminescent material technical fields, and in particular to a kind of white emitting fluorescent powder and its preparation method and application.
Background technology
LED has many advantages, such as pollution-free, long-life, energy conservation and environmental protection, is widely used in various displays, indicator light, backlight
Source, domestic or commercial illumination.The tungstates of scheelite-type structure is due to stable chemical property and low phonon energy,
It is proved to be important optical material.BO4 2-Ion has tetrahedral structure, B6+Ion is located at tetrahedral center, 4 O2-From
Son is located at tetrahedral 4 apex angles.Ground state B6+The out orbit of ion is full of electronics, when being stimulated, O2-One 2p electricity of ion
Son transits to B6+The empty d tracks of ion are returned to ground state immediately, generate transition radiation, therefore, tungstates is typical self-activation
Luminescent material.Meanwhile ABO4Type tungstates is also a kind of important luminous host material.Since common blue LED die swashs
Turn to be yellow color YAG:White light lacks red color components obtained by Ce fluorescent powders, and colour rendering index is low, therefore, using tungstates as matrix, Eu3+For hair
The red fluorescence powder research of light center is the most universal.
Invention content
The purpose of the present invention is to provide a kind of single-component phosphor wolframic acid alkali white light emitting materials, can be in black light
White light is sent out under excitation.
The technical scheme is that:
The chemical formula of a kind of wolframic acid alkali white light emitting material, the luminescent material is Ba0.05Sr0.94-zWO4∶0.01Tm3+
zDy3+, z=0.01~0.06.
Preferably described z=0.01~0.04 of the luminescent material of the present invention.The most preferably z=0.03.
The luminescent material of the present invention, can emit white light under the excitation wavelength of 352~366nm.Under most preferred excitation wavelength
354nm。
The application of the present invention is the luminescent material using the material as near ultraviolet chip excited white light.
A kind of preparation method of wolframic acid alkali white light emitting material of the present invention, the luminescent material is by raw material by life
At Ba0.05Sr0.94-zWO4∶0.01Tm3+zDy3+Required stoichiometric ratio is mixed and heated to 500 DEG C~900 DEG C conditions, and through combustion
Phase reaction is baked to be made.It is preferably heated to 800 DEG C~900 DEG C.
The raw material includes Ba (NO3)2、Sr(NO3)2、(NH4)6H2W12O40.nH2O、Tm2O3And Dy2O3。
Urea and ethylene glycol are added in the raw material.
Reaction time is 15~40min.
Inventor in the long-term doping to tungstates find in research process, specifically as shown in fig. 6, Fig. 6 is
BamSr0.99-mWO4:0.01Tm3+Launching light spectrogram (λex=359nm).With a small amount of Ba2+The doping of ion, the hair of fluorescent powder
Luminous intensity enhances, and works as Ba2+When the doping concentration of ion is 0.05, shines best, continue growing Ba2+The doping concentration of ion, then
It shines and starts to weaken.Thus, a small amount of Ba2+The doping of ion exacerbates SrWO4The distortion of lattice of crystal, this is conducive to Tm3+Ion
To Sr2+The substitution of ion, while being conducive to Tm3+Shine.Ba is determined in experimental study through inventor2+The best of ion is mixed
Miscellaneous a concentration of 0.05, work as Ba2+When the doping concentration of ion is 0.05, Ba0.05Sr0.94-zWO4, it is abbreviated as BSWO.Inventor with
On the basis of the matrix composition of upper research, through further research, it has been found that, Dy is carried out on the matrix3+And Tm3+Codope, can
With the fluorescent powder to be emitted white light.Chemical formula by controlling the present invention is Ba0.05Sr0.94-zWO4∶0.01Tm3+zDy3+Series is glimmering
Light powder, not only XRD show that sample that 900 degree are sintered out is SrWO4Pure phase.More that crux is Ba0.05Sr0.94-zWO4:
0.01Tm3+zDy3+(z=001~0.06) shines under the excitation wavelength of 352~366nm swashs in white light area, especially 354nm
It gives, when z=0.03, fluorescent powder shines closest to standard white light, and chromaticity coordinates is (0.321,0.347), colour temperature 6000K.
Therefore, Ba of the invention0.05Sr0.94-zWO4∶0.01Tm3+zDy3+It can be used as the application material of near ultraviolet chip excited white light.
Description of the drawings
Fig. 1 is Ba0.05Sr0.91WO4:0.01Tm3+0.03Dy3+Scanning electron microscope (SEM) photo.The crystallization shape of product with
Based on uniform ellipsoid, average particle size particle size is about 0.5um.
Fig. 2 a are Ba0.05Sr0.93WO4:0.01Tm3+0.01Dy3+Exciting light spectrogram (λem=573nm and λem=454nm);
Fig. 2 b are Ba0.05Sr0.93WO4:0.01Tm3+0.01Dy3+Excitation wavelength be 352-366nm emission spectrum;
Fig. 2 c are Ba0.05Sr0.94-zWO4:0.01Tm3+zDy3+Emission spectrum (λex=353nm, z=0.01-0.04);
Fig. 2 d are Ba0.05Sr0.94-zWO4:0.01Tm3+zDy3+Emission spectrum (λex=359nm, z=0.01-0.04);
Fig. 3 is Ba0.05Sr0.91WO4:0.01Tm3+0.03Dy3+CIE1931 chromatic diagrams;
Fig. 4 is Ba0.05Sr0.91WO4:0.01Tm3+0.03Dy3+Decay of afterglow curve after 353nm is excited 1 minute;
Fig. 5 is Ba0.05Sr0.91WO4:0.01Tm3+0.03Dy3+The XRD diagram of sample.
Material phase analysis DMAX-2500 types X-ray diffractometer (XRD).Test parameter is Cu (Kα) target, 40KV tube voltages,
250mA tube currents, 10-70 ° of scanning range, 0.02 ° of scanning step, 8 °/min of sweep speed.Morphology microstructure is analyzed in Quanta
It is carried out in 200 scanning electron microscope (SEM).The illuminating Hitachi F-4500 type fluorescence spectrophotometer measurements of powder, test
Condition is:Xenon source, voltage 400V, slit width 2.5nm, sweep speed 240nm/min.
Fig. 6 is BamSr0.99-mWO4:0.01Tm3+Launching light spectrogram (λex=359nm).
Specific implementation mode
By generation Ba0.05Sr0.94-zWO4:0.01Tm3+zDy3+(z=0.01-0.06) stoichiometric ratio weighs Ba (NO3)2
(A.R.),Sr(NO3)2(A.R.),(NH4)6H2W12O40.nH2O(A.R.),Tm2O3(4N) and Dy2O3(4N), it is 3 times respectively to weigh
The ethylene glycol of the urea of BSWO molar ratios and 12 times of BSWO molar ratios, (first by Tm2O3(4N) and Dy2O3(4N) is dissolved in dense nitre
Tm (NO are made in acid3)3With Dy (NO3)3Mixed solution, the pH value that solution is adjusted with PH test paper is alkalinity, then by this solution and
Remaining substance weighed is put into magnetic stirrer completely) mixing, according to sample detection determine optimum temperature carry out reaction and
Sample is made in sintering.
Fig. 2 (a) is Ba obtained0.05Sr0.91WO4:0.01Tm3+0.01Dy3+Excitation spectrum, monitoring wavelength be respectively
There is superposition in 353nm and 366nm in 454nm and 573nm, two excitation spectrums.Fig. 2 (b) is Ba0.05Sr0.91WO4:0.01Tm3+
0.01Dy3+In the emission spectrum that excitation wavelength is 352-366nm.When excitation wavelength is between 352-366nm, Tm3+And Dy3+
It is excited simultaneously, emitted luminescence intensity changes regular variation with excitation wavelength.It emits white light near 353nm and 366nm,
Near 359, it is in white light area, but close to blue region.
Fig. 2 (c) is Ba0.05Sr0.94-zWO4:0.01Tm3+zDy3+(z=0.01-0.04) launching light spectrogram, excitation wavelength
353nm.With Dy3+The increase of ion doping molar concentration, the luminous intensity of fluorescent powder first enhances to be weakened afterwards, and doping concentration is
The most strong tables 1 that shine when 0.03 list z=0.01-0.06, and excitation wavelength is the chromaticity coordinates of 352-366nm fluorescent powders.Work as z=
When 0.01, the light-emitting zone of fluorescent powder is close to blue region, and as z values increase, shine, z=close to yellow region through white light
0.03 near yellow light area, then again close to white light area.It is found that working as z=0.03, excitation wavelength is for compares figure 3 and table 1
It when 354nm, shines near standard white light (0.333,0.333), chromaticity coordinates at this time is (0.321,0.347), and colour temperature is
6000K。
1 Ba of table0.05Sr0.94-zWO4:0.01Tm3+zDy3+Chromaticity coordinates (z=0.01-0.06)
Claims (10)
1. a kind of wolframic acid alkali white light emitting material, which is characterized in that the chemical formula of the luminescent material is Ba0.05Sr0.94-zWO4∶
0.01Tm3+zDy3+, z=0.01~0.06.
2. white light emitting material according to claim 1, which is characterized in that z=0.01~0.04.
3. white light emitting material according to claim 1, which is characterized in that the z=0.03.
4. a kind of application of wolframic acid alkali white light emitting material of claim 1-3 any one of them, which is characterized in that will be described
Luminescent material using material as near ultraviolet chip excited white light.
5. application according to claim 4, which is characterized in that excitation wavelength of the luminescent material in 352~366nm
Under, it emits white light.
6. application according to claim 4, which is characterized in that the luminescent material whitens at excitation wavelength 354nm
Light.
7. a kind of preparation method of wolframic acid alkali white light emitting material of claim 1-3 any one of them, which is characterized in that institute
The luminescent material stated is by raw material by generation Ba0.05Sr0.94-zWO4∶0.01Tm3+zDy3+Required stoichiometric ratio is blended in 500
DEG C~900 DEG C of heating conditions under through combustion reaction be made.
8. preparation method according to claim 7, which is characterized in that the raw material includes Ba (NO3)2、Sr(NO3)2、
(NH4)6H2W12O40.nH2O、Tm2O3And Dy2O3。
9. preparation method according to claim 7, which is characterized in that be added with urea and ethylene glycol in the raw material.
10. preparation method according to claim 7, which is characterized in that the reaction time is 15~40min.
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Citations (2)
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---|---|---|---|---|
CN101864307A (en) * | 2010-07-05 | 2010-10-20 | 聊城大学 | Method for preparing double-tungstate green fluorescent powder |
CN103254898A (en) * | 2013-03-28 | 2013-08-21 | 中国科学院福建物质结构研究所 | Thulium and dysprosium co-doped sodium yttrium tungstate white luminescent material and its use |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101864307A (en) * | 2010-07-05 | 2010-10-20 | 聊城大学 | Method for preparing double-tungstate green fluorescent powder |
CN103254898A (en) * | 2013-03-28 | 2013-08-21 | 中国科学院福建物质结构研究所 | Thulium and dysprosium co-doped sodium yttrium tungstate white luminescent material and its use |
Non-Patent Citations (2)
Title |
---|
"Host composition dependent tuneable morphology and luminescent property of the CaXSrYBa1-X-YWO4:RE3+ (RE=Pr, Ho, and Er) phosphors";Linlin Li et al.;《Journal of Alloys and Compounds》;20170125;第702卷;第106-119页 * |
"Growth and characterization of Nd:Sr0.95Ba0.05WO4 single crystal";GAO Lihong et al.;《JOURNAL OF RARE EARTHS》;20090215;第27卷(第1期);第71-75页 * |
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