CN108865143A - A kind of near ultraviolet excited single-matrix white light emitting and preparation method and white light are adjusted - Google Patents
A kind of near ultraviolet excited single-matrix white light emitting and preparation method and white light are adjusted Download PDFInfo
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- CN108865143A CN108865143A CN201810888896.XA CN201810888896A CN108865143A CN 108865143 A CN108865143 A CN 108865143A CN 201810888896 A CN201810888896 A CN 201810888896A CN 108865143 A CN108865143 A CN 108865143A
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- 239000011159 matrix material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 53
- 239000000463 material Substances 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 229910001477 LaPO4 Inorganic materials 0.000 claims abstract description 6
- 239000012190 activator Substances 0.000 claims abstract description 3
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 7
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 7
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 4
- 239000003086 colorant Substances 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
- 238000003836 solid-state method Methods 0.000 claims description 3
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 2
- 230000005284 excitation Effects 0.000 abstract description 16
- 238000009877 rendering Methods 0.000 abstract description 7
- 229910001415 sodium ion Inorganic materials 0.000 description 31
- 229910019142 PO4 Inorganic materials 0.000 description 16
- 150000002500 ions Chemical group 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 2
- 240000002853 Nelumbo nucifera Species 0.000 description 2
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 2
- 241001025261 Neoraja caerulea Species 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000013456 study Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 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
- C09K11/7709—Phosphates
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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)
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- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
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- Computer Hardware Design (AREA)
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- Luminescent Compositions (AREA)
Abstract
The present invention provides near ultraviolet excited single-matrix white light emittings, and fluorescent powder is with LaPO4For host material, Bi3+For fluorescent powder activator, pass through trace doped Li+,Na+The chromaticity coordinates and colour temperature of fluorescent powder are adjusted, fluorescent powder chemical formula is La0.97‑x‑yPO4:Bi3+ 0.03,Li+ x,Na+ y, (x=0.00,0.01,0.02,0.03, y=0.00,0.01,0.02,0.03).Preparation method of the present invention is simple, easy to operate, under the excitation of 335nm wavelength, adulterates charge compensator Li+、Na+, available required white light emission.Work as Na+When doping concentration is 0.02, the colour rendering index of fluorescent powder is (0.3008,0.3203), colour temperature 7302K, and white light performance reaches best.
Description
Technical field
The invention belongs to luminescent material technical fields, are specifically related to a kind of near ultraviolet excitation single-matrix white fluorescence
Powder and preparation method.
Background technique
Light LED is known as due to having many advantages, such as that small in size, low energy consumption, luminous efficiency is high, the service life is long and environmentally friendly
It is the forth generation lighting source after incandescent lamp, fluorescent lamp and high-pressure discharge lamp.Business white light mainly passes through blue-ray LED at present
Excite yellow fluorescent powder YAG:Ce3+, obtained by yellow light and blue light, however this white light acquisition methods have certain lack
It falls into, the luminous efficiency of blue-ray LED first is not very high, and the luminescent color of device is with operating temperature and voltage and fluorescent powder
The variation of coating layer thickness and cause white light emission unstable, color reducibility is poor.Secondly as lacking what red light component obtained
White light makes the disadvantages of colour temperature is high, and colour rendering index is higher.To solve the above-mentioned problems, using near ultraviolet excitation single-phase matrix
It is a kind of preferable alternative solution that fluorescent powder, which obtains high-quality white light,.
For phosphate since chemical property is stablized, phonon energy is lower, and synthesis temperature is mild, is a kind of preferable fluorescent powder base
Material.Simultaneously as Bi3+There is ion very excellent optical property can generate under near ultraviolet excitation3P1→1S0,1P1→1S0Electron transition is influenced the capable of emitting transmitting light in visibility region different-waveband by host material.According to reports,
LaPO is prepared about solid phase method at present4:Bi3+,Li+,Na+There are no correlative studys for fluorescent powder, by the way that charge compensator Li is added+,
Na+Improve the white light performance of this single-matrix fluorescent powder.Thus there is the work of this part extraordinary innovation to probe into meaning.
Summary of the invention
The present invention is in order to solve the above technical problems, provide a kind of near ultraviolet excitation single-matrix fluorescent powder, in 335nm
Under wavelength excitation, 485nm or so (blue light), 530nm or so (green light) and 637nm or so (blue light) three main transmittings are obtained
Peak, the mutual superimposion of the light of three kinds of colors, available required white light emission.
The technical solution adopted by the present invention is：A kind of near ultraviolet excited single-matrix white light emitting, the fluorescent powder
With LaPO4For host material, Bi3+For fluorescent powder activator, pass through trace doped Li+,Na+Adjust the chromaticity coordinates and color of fluorescent powder
Temperature, fluorescent powder chemical formula are LaPO4:Bi3+,Li+,Na+。
Further, the fluorescent powder chemical formula is La0.97-x-yPO4:Bi3+ 0.03,Li+x,Na+ y, wherein x=0.00,
0.01,0.02,0.03, y=0.00,0.01,0.02,0.03.
A kind of preparation method of near ultraviolet excited single-matrix white light emitting, the preparation method is that high temperature solid-state
Method includes the following steps：La is stoichiometrically weighed first2O3、Bi2O3、NH4H2PO4、Li2CO3、Na2CO3, mix to be added and grind
3h is persistently ground in alms bowl and obtains presoma, and presoma is finally obtained into target product in 1200 DEG C of temperature lower calcination 8h.
Further, the La2O3、Bi2O3、NH4H2PO4、Li2CO3、Na2CO3Metering compare for (0.97-x-y):0.03:
2.04:X (x=0.00,0.01,0.02,0.03):Y (y=0.00,0.01,0.02,0.03).
A kind of white light adjusting of near ultraviolet excited single-matrix white light emitting, under the excitation of 335nm wavelength, doping electricity
Lotus compensation Li+、Na+, fluorescent powder system obtains 485nm or so (blue light), 530nm or so (green light) and 637nm or so (blue light)
Three main emission peaks, the mutual superimposion of the light of three kinds of colors, available required white light emission.
Further, the Na+Doping concentration is 0.02, i.e. y=0.02.
What the present invention obtained has the beneficial effect that：Preparation method of the present invention is simple, easy to operate, the La of preparation0.97-x-yPO4:Bi3 + 0.03,Li+ x,Na+ y(x=0.00,0.01,0.02,0.03, y=0.00,0.01,0.02,0.03) fluorescent powder is in 335nm wavelength
Under excitation, three main emission peaks of 485nm or so (blue light), 530nm or so (green light) and 637nm or so (blue light) are obtained, three
The mutual superimposion of light of kind color, available required white light emission.By the way that charge compensator Li is added+,Na+, fluorescence
The white light colour rendering index of powder is preferably improved with colour temperature.
Detailed description of the invention
Fig. 1 is sample La of the present invention0.97PO4:Bi3+ 0.03The excitation (Detection wavelength λ em=637nm) and transmitting of fluorescent powder
(excitation wavelength lambda ex=335nm) spectrogram.
Fig. 2 is that charge compensator Li is added+, fluorescent powder La0.97-xPO4:Bi3+ 0.03,Li+ x, (x=0.00,0.01,0.02,
0.03) fluorescence emission spectrogram of compound under 335nm excitation.
Fig. 3 is that charge compensator Na is added+, fluorescent powder La0.97-yPO4:Bi3+ 0.03,Na+ y, (y=0.00,0.01,0.02,
0.03) fluorescence emission spectrogram of compound under 335nm excitation.
Fig. 4 a is that charge compensator Li+, fluorescent powder La is added0.97-xPO4:Bi3+ 0.03,Li+ x, (x=0.00,0.01,
0.02,0.03) luminous CIE chromaticity coordinates.
Fig. 4 b is that charge compensator Na+, fluorescent powder La is added0.97-yPO4:Bi3+ 0.03,Na+ y, (y=0.00,0.01,
0.02,0.03) luminous CIE chromaticity coordinates.
Fig. 5 a is that charge compensator Li is added+, fluorescent powder La0.97-x-yPO4:Bi3+ 0.03,Li+ x,Na+ y, (x=0.00,
0.01,0.02,0.03, y=0.00,0.01,0.02,0.03) XRD spectra.
Fig. 5 b is that charge compensator Na is added+, fluorescent powder La0.97-x-yPO4:Bi3+ 0.03,Li+ x,Na+ y, (x=0.00,
0.01,0.02,0.03, y=0.00,0.01,0.02,0.03) XRD spectra.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
A kind of near ultraviolet excited single-matrix white light emitting, with LaPO4For host material, Bi3+For fluorescent powder activation
Agent passes through trace doped Li+,Na+The chromaticity coordinates and colour temperature of fluorescent powder are adjusted, fluorescent powder chemical formula is La0.97-x-yPO4:Bi3 + 0.03,Li+ x,Na+ y, wherein x=0.00,0.01,0.02,0.03, y=0.00,0.01,0.02,0.03.Preparation method is high temperature
Solid phase method includes the following steps：La is stoichiometrically weighed first2O3、Bi2O3、Li2CO3、Na2CO3、NH4H2PO4, metering ratio
For (0.97-x-y):0.03:2.04:X (x=0.00,0.01,0.02,0.03):Y (y=0.00,0.01,0.02,0.03) is mixed
3h is persistently ground in conjunction addition mortar and obtains presoma, and presoma is finally obtained into target production in 1200 DEG C of temperature lower calcination 8h
Object.
Experiment reagent：Y2O3(99.9%), Bi2O3(99.9%), NH4H2PO4(analysis is pure), Li2CO3(analysis is pure),
Na2CO3(analysis is pure).Laboratory apparatus：Mortar, electronic balance, crucible, Muffle furnace and fluorescence spectrum tester (PE company of the U.S.,
Model PE LS55), powder single crystal diffractometer XRD.
The preparation process of fluorescent powder：La0.97-x-yPO4:Bi3+ 0.03,Li+ x,Na+ y, wherein x=0.00,0.01,0.02,
0.03, y=0.00,0.01,0.02,0.03 is prepared by high temperature solid-state method.La is stoichiometrically weighed first2O3、
Bi2O3、Li2CO3、Na2CO3、NH4H2PO4, mixing is added in mortar and persistently grinds 3h and obtain presoma, finally presoma exists
1200 DEG C of temperature lower calcination 8h, obtain target product.
Sample emission spectrum and the test of emission spectrum relative intensity under 335nm excitation use the fluorescence light of U.S. PE company
Compose tester, model PE LS55.
As shown in Figure 1, La0.97PO4:Bi3+ 0.03The excitation peak of fluorescent powder is located at 335nm near ultraviolet region, belongs to Bi3+
Ion1S0→3P1Transition, 335nm wavelength excitation under, obtain 485nm or so (blue light), 530nm or so (green light) with
Three main emission peaks of 637nm or so (blue light), the mutual superimposion of the light of three kinds of colors, available white light emission.
Such as Fig. 2, shown in 3, under the excitation of 335nm wavelength, with Li+ adulterate, the red emission peak of fluorescent powder becomes strong, makes
It is mobile to standard white light direction to obtain white light chromaticity coordinates and colour temperature, best when Li+ doping concentration is 0.01, the colour developing of fluorescent powder refers to
Number is (0.2956,0.3221), colour temperature 7520K.With Na+ doping, the red emission peak of fluorescent powder becomes strong, can equally make
White light chromaticity coordinates and colour temperature are mobile to standard white light direction, when adulterating 0.02, the colour rendering index of fluorescent powder be (0.3008,
0.3203), colour temperature 7302K, white light performance reach best.Charge compensator Li+, Na+ are adulterated, fluorescent powder system obtains
Three main emission peaks of 485nm or so (blue light), 530nm or so (green light) and 637nm or so (blue light), with Li+, Na+
Doping, the red emission peak intensity of fluorescent powder are improved, so that white light chromaticity coordinates and colour temperature are mobile to standard white light direction, when
Na+When doping concentration is 0.02, the colour rendering index of fluorescent powder is (0.3008,0.3203), colour temperature 7302K, and white light performance reaches
To best.
As shown in Figs. 4a and 4b, charge compensator Li is added+、Na+, the luminous CIE chromaticity coordinates of fluorescent powder system.With electricity
Lotus compensation Li+、Na+Doping, chromaticity coordinates is mobile to white light baseline.With charge compensator Li+Doping, chromaticity coordinates to
White light baseline is mobile.Work as Li+When doping concentration is 0.01, the colour rendering index of fluorescent powder is (0.2956,0.3221), and colour temperature is
7520K.Work as Na+When doping concentration is 0.02, the colour rendering index of fluorescent powder is (0.3008,0.3203) (in Fig. 4 b shown in f point),
Colour temperature is 7302K, and white light performance reaches best.
As shown in figure 5a and 5b, charge compensator Li is added+、Na+, fluorescent powder La0.97-x-yPO4:Bi3+ 0.03,Li+ x,Na+ y
The XRD spectra and LaPO of (x=0.00,0.01,0.02,0.03, y=0.00,0.01,0.02,0.03)4Standard card
JCPDS 35-0731 is almost the same, without miscellaneous phase.And with Li+、Na+The doping of ion, since the ionic radius of the two is small
In La3+Ion, therefore, the peak of spectrogram are displaced to wide-angle, illustrate Li+、Na+Ion be successfully doped into matrix cell configuration it
In, do not cause phase transformation.
Table 1 is doping charge compensator Li+、Na+Afterwards, fluorescent powder La0.97-x-yPO4:Bi3+ 0.03,Li+ x,Na+ y(x=0.00,
0.01,0.02,0.03, y=0.00,0.01,0.02,0.03) white light chromaticity coordinates position and colour temperature relationship.
Table 1：Fluorescent powder La0.97-x-yPO4:Bi3+ 0.03,Li+ x,Na+ y, (x=0.00,0.01,0.02,0.03, y=0.00,
0.01,0.02,0.03) serial chromaticity coordinates and colour temperature
Claims (6)
1. a kind of near ultraviolet excited single-matrix white light emitting, it is characterised in that：The fluorescent powder is with LaPO4For matrix material
Material, Bi3+For fluorescent powder activator, pass through trace doped Li+,Na+Adjust the chromaticity coordinates and colour temperature of fluorescent powder, fluorescent powder chemical formula
For LaPO4:Bi3+,Li+,Na+。
2. a kind of near ultraviolet excited single-matrix white light emitting according to claim 1, it is characterised in that：The fluorescence
Powder chemical formula is La0.97-x-yPO4:Bi3+ 0.03,Li+ x,Na+ y, wherein x=0.00,0.01,0.02,0.03, y=0.00,0.01,
0.02,0.03。
3. a kind of preparation method of near ultraviolet excited single-matrix white light emitting, it is characterised in that：The preparation method is that
High temperature solid-state method includes the following steps：La is stoichiometrically weighed first2O3、Bi2O3、NH4H2PO4、Li2CO3、Na2CO3, mix
3h is persistently ground in conjunction addition mortar and obtains presoma, and presoma is finally obtained into target production in 1200 DEG C of temperature lower calcination 8h
Object.
4. a kind of preparation method of near ultraviolet excited single-matrix white light emitting, feature exist according to claim 3
In：The La2O3、Bi2O3、NH4H2PO4、Li2CO3、Na2CO3Metering compare for (0.97-x-y):0.03:2.04:X (x=
0.00,0.01,0.02,0.03):Y (y=0.00,0.01,0.02,0.03).
5. a kind of white light of near ultraviolet excited single-matrix white light emitting is adjusted, it is characterised in that：It is excited in 335nm wavelength
Under, adulterate charge compensator Li+、Na+, fluorescent powder system obtains 485nm or so (blue light), 530nm or so (green light) and 637nm
Left and right (blue light) three main emission peaks, the mutual superimposion of the light of three kinds of colors, available required white light emission.
6. a kind of near ultraviolet excited single-matrix white light emitting according to claim 2, it is characterised in that：The Na+It mixes
Miscellaneous concentration is 0.02, i.e. y=0.02.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115820255A (en) * | 2022-12-21 | 2023-03-21 | 云南大学 | Single-matrix warm white fluorescent powder and preparation method thereof |
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| CN1893976A (en) * | 2003-12-17 | 2007-01-10 | 皇家飞利浦电子股份有限公司 | Radiation therapy and medical imaging using uv emitting nanoparticles |
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| Title |
|---|
| F. B. M. VAN ZOU ET AL.: "An EXAFS Study of the Luminescent Bi3+ Center in LaPO4-Bi", 《JOURNAL OF SOLID STATE CHEMISTRY》 * |
| SANTOSH K. GUPTA ET AL.: "Tunable white light emitting Sr2V2O7:Bi3+ phosphors: Role of Bis", 《MATERIALS & DESIGN》 * |
| WEI LI ET AL.: "Microwave-Assisted Sol-Gel Synthesis and Photoluminescence Characterization of LaPO4:Eu3+,Li+ Nanophosphors", 《J. PHYS. CHEM. C》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115820255A (en) * | 2022-12-21 | 2023-03-21 | 云南大学 | Single-matrix warm white fluorescent powder and preparation method thereof |
| CN115820255B (en) * | 2022-12-21 | 2023-09-26 | 云南大学 | Single-matrix warm white fluorescent powder and preparation method thereof |
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