CN108949175A - A kind of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping and preparation method thereof - Google Patents
A kind of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping and preparation method thereof Download PDFInfo
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- CN108949175A CN108949175A CN201811117727.2A CN201811117727A CN108949175A CN 108949175 A CN108949175 A CN 108949175A CN 201811117727 A CN201811117727 A CN 201811117727A CN 108949175 A CN108949175 A CN 108949175A
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- fluorescent powder
- blue colour
- yttrium borate
- cerium dopping
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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
- C09K11/778—Borates
Abstract
The invention discloses a kind of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping and preparation method thereof, chemical general formulas are as follows: Sr3‑xY(BO3)3: xCe, wherein 0.01≤x≤0.15.It can effectively be excited by black light, issue the high blue light of excitation purity.The present invention is that blue colour fluorescent powder is prepared based on solid-phase synthesis, is prepared under reducing atmosphere, simple process, favorable reproducibility, short preparation period, and non-pollutant discharge is environmental-friendly, easily operated and industrialized production.
Description
Technical field
The invention belongs to the phosphor technologies field LED, be related to a kind of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping and
Preparation method.
Background technique
Light emitting diode (Light Emitting Diode, LED) is acknowledged as the new light sources of 21st century, has
Many advantages, such as energy conservation, fast, environmentally protective, the service life is long, small in size, luminous efficiency is high response, has in illumination and display field
Huge application prospect.
Realize that commercialized blue colour fluorescent powder is mainly BaMgAl at present10O17:Eu2+(BAM), however BAM stability is poor,
Serious light decay can be generated by the irradiation of long-time vacuum-ultraviolet light, in order to overcome BAM in the application the shortcomings that, therefore develop
It synthesizes at high temperature and the blue colour fluorescent powder that can be approached ultraviolet excitation has huge practical application value.In near ultraviolet
Redgreenblue fluorescent powder is coated on LED chip, green red near ultraviolet excitation, blue colour fluorescent powder form feux rouges, green
Light, blue light combination can also issue white light.This method can not only overcome the problems, such as that conventional white light LED exists, and is also easy to control
The luminous color of system, colour rendering are good.Due to Ce3+4f-5d transition, make Ce3+Very strong suction is shown near ultraviolet wave-length coverage
It receives, and blue light can be emitted under the excitation of near ultraviolet wavelength.Therefore, research can effectively be excited by black light, luminous intensity height,
The good three strontium yttrium borate base blue light fluorescent powder of cerium dopping of purity has good practical application value.
Summary of the invention
The object of the present invention is to provide a kind of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping and preparation method thereof, solve to pass
Blue light fluorescent powder BAM stability of uniting is poor, can lead to the problem of serious light decay by the irradiation of long-time vacuum ultraviolet.
The technical scheme adopted by the invention is that
A kind of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping, the chemical general formula of the fluorescent powder are Sr3-xY(BO3)3: xCe,
Wherein 0.01≤x≤0.15.
The excitation spectrum of the fluorescent powder in 200-400nm, main excitation peak near 338nm, emission spectrum 400~
650nm, main peak is near 420nm.
The fluorescent powder can issue blue light under near ultraviolet excitation.
A kind of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping and preparation method thereof, comprising the following steps:
(1) according to the chemical structural formula Sr of fluorescent powder3-xY(BO3)3: the mol ratio amount of xCe, weigh respectively containing Sr, Y,
B, weighed raw material is fully ground and is uniformly mixed as raw material by the compound of Ce element；
(2) it by uniform raw material under air atmosphere, is calcined 5-8 hours at 1200 DEG C -1300 DEG C；
(3) it after the completion of calcining, is taken out after being cooled to room temperature, is fully ground crushing, obtains Ce3+Adulterate three strontium yttrium borate fluorescence
Powder Sr3Y1-x(BO3)3: xCe, wherein 0.01≤x≤0.15.
The compound containing Sr, Y, B, Ce element, respectively SrCO3、Y2O3、H3BO3、CeO2。
The calcining is carried out in SGQ-5-14 tube type resistance furnace, reducing atmosphere 5%H2+ 95%Ar, from room temperature with 8
The heating rate of~10 DEG C/min rises to 1200 DEG C -1300 DEG C, keeps the temperature 5-8h, later furnace cooling.
The grinding of the raw material, calcined its milling time of grinding are 20~60min.
The beneficial effects of the present invention are:
It is provided by the invention with Sr3Y(BO3)3It is not only at low cost, stability is good, easy preparation for the fluorescent powder of matrix, but also
There is a very strong excitation peak near ultraviolet region, is suitble to UV excitation, can be applied to LED.Therefore, Sr3Y(BO3)3It being capable of conduct
Good fluorescent powder basis material.By adulterating active ions Ce3+, main peak position can be obtained under black light (338nm) excitation
Luminous intensity is compared with strong, the higher blue light of excitation purity near 420nm.The Sr that the present invention is prepared3Y(BO3)3Base fluorescent powder
It learns property to stablize, good luminous performance, luminous intensity is high, and colour rendering is good, can meet the application requirement in White-light LED illumination field.This
The fluorescent powder of invention preparation is suitble near ultraviolet excitated, and emission peak is located at 420nm, and chromaticity coordinates is located at blue region (x=0.162, y
=0.106) it, is matched near ultraviolet chip light emitting diode, illustrates that fluorescent powder prepared by the present invention is a kind of good luminescence property
Blue light fluorescent powder.
The preparation method of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping provided by the invention, preparation method are based on solid
Phase synthesi is come what is prepared, and strong operability is prepared under reducing atmosphere, and temperature-rise period is simple, and preparation method is simple, reappears
Good, the short preparation period of property.
Detailed description of the invention
Fig. 1 is the Sr that embodiment 3 is prepared2.96Y(BO3)3: 0.07Ce fluorescent powder and Sr3Y(BO3)3The X-ray of matrix
Diffracting spectrum and Ba3Dy(BO3)3Standard card (PDF#50-0098) comparison diagram；
Fig. 2 is the Sr that embodiment 3 is prepared2.96Y(BO3)3: the excitation spectrum and emission spectrum of 0.07Ce fluorescent powder；
Fig. 3 is the Sr that embodiment 3 is prepared2.96Y(BO3)3: the CIE chromaticity coordinates figure of 0.07Ce fluorescent powder.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping of the present invention and preparation method thereof, it is specifically real according to the following steps
It applies:
(1) according to the chemical structural formula Sr of fluorescent powder1-xY(BO3)3: the mol ratio amount of xCe, weigh respectively containing Sr, Y,
B, weighed raw material is fully ground and is uniformly mixed as raw material by the compound of Ce element；
(2) it by uniform raw material under air atmosphere, is calcined 5-8 hours at 1200-1300 DEG C；
(3) it after the completion of calcining, is taken out after being cooled to room temperature, is fully ground crushing, obtains Ce3+Adulterate three strontium yttrium borate fluorescence
Powder Sr1-xY(BO3)3: xCe, wherein 0.01≤x≤0.15.
A kind of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping of the present invention and preparation method thereof, is prepared using solid phase method,
Its luminous intensity is high, simple process, strong operability, short preparation period.
Embodiment 1
By chemical formula Sr2.99Y(BO3)3: the stoichiometric of 0.01Ce accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、CeO2, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.Above-mentioned raw materials are ground
After mixing, it is packed into corundum crucible, is placed in high temperature process furnances, is risen in reducing atmosphere with the heating rate of 5 DEG C/min
1200 DEG C, 5 hours are kept the temperature, then furnace cooling is cooled to room temperature to sample.Sample regrinding is taken out to crush to get Ce is arrived3+
Adulterate three strontium yttrium borate blue colour fluorescent powders.
Embodiment 2
By chemical formula Sr2.98Y(BO3)3: the stoichiometric of 0.02Ce accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、CeO2, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.Above-mentioned raw materials are ground
After mixing, it is packed into corundum crucible, is placed in high temperature process furnances, is risen in reducing atmosphere with the heating rate of 8 DEG C/min
1200 DEG C, 5 hours are kept the temperature, then furnace cooling is cooled to room temperature to sample.Sample regrinding is taken out to crush to get Ce is arrived3+
Adulterate three strontium yttrium borate blue colour fluorescent powders.
Embodiment 3
By chemical formula Sr2.96Y(BO3)3: the stoichiometric of 0.07Ce accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、CeO2, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.Above-mentioned raw materials are ground
After mixing, it is packed into corundum crucible, is placed in high temperature process furnances, is risen in reducing atmosphere with the heating rate of 10 DEG C/min
1250 DEG C, 5 hours are kept the temperature, then furnace cooling is cooled to room temperature to sample.Sample regrinding is taken out to crush to get Ce is arrived3+
Adulterate three strontium yttrium borate blue colour fluorescent powders.
Fig. 1 is Sr prepared by the present embodiment 32.96Y(BO3)3: 0.07Ce fluorescent powder and Sr3Y(BO3)3The X-ray of matrix is spread out
Penetrate map and Ba3Dy(BO3)3Standard card (PDF#50-0098) comparison diagram.At present without discovery Sr in PDF card base3Y
(BO3)3Standard card, but find compared with the crystal structure of this substance similar Ba3Dy(BO3)3Standard card PDF#
Standard card of the 50-0098 as sample diffraction atlas analysis.It can be found that main diffraction peak all with Ba3Dy(BO3)3Standard
Card is corresponding, but all has to big angle of diffraction direction and a little deviate.Reason is that the ionic radius of Sr and Ba is differentCause to deviate to wide-angle；The ionic radius of Y and Dy is very closeInfluence very little to the angle of diffraction.It is seen that object is mutually with high purity, crystallinity
Good, significant change does not occur for doping front and back principal crystalline phase.
Fig. 2 is Sr prepared by the present embodiment 32.96Y(BO3)3: the excitation spectrum and emission spectrum of 0.07Ce fluorescent powder.This is glimmering
The excitation spectrum of light powder is in 200~400nm, and main excitation peak is near 338nm, and emission spectrum is in 350~650nm, transmitting
Peak is located near 454nm.It can be seen that the fluorescent powder can effectively be excited by black light and issue blue light, white light can be applied to
LED。
Fig. 3 is Sr prepared by the present embodiment 32.96Y(BO3)3: the CIE chromaticity coordinates figure of 0.07Ce fluorescent powder.Chromaticity coordinates is located at
Blue region (x=0.162, y=0.106) illustrates that fluorescent powder prepared by the present invention is a kind of blue-fluorescence of good luminescence property
Powder.
Embodiment 4
By chemical formula Sr2.9Y(BO3)3: the stoichiometric of 0.1Ce accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、CeO2, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.Above-mentioned raw materials are ground
After mixing, it is packed into corundum crucible, is placed in high temperature process furnances, is risen in reducing atmosphere with the heating rate of 10 DEG C/min
1250 DEG C, 7 hours are kept the temperature, then furnace cooling is cooled to room temperature to sample.Sample regrinding is taken out to crush to get Ce is arrived3+
Adulterate three strontium yttrium borate blue colour fluorescent powders.
Embodiment 5
By chemical formula Sr2.85Y(BO3)3: the stoichiometric of 0.15Ce accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、CeO2, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.Above-mentioned raw materials are ground
After mixing, it is packed into corundum crucible, is placed in high temperature process furnances, is risen in reducing atmosphere with the heating rate of 10 DEG C/min
1300 DEG C, 8 hours are kept the temperature, then furnace cooling is cooled to room temperature to sample.Sample regrinding is taken out to crush to get Ce is arrived3+
Adulterate three strontium yttrium borate blue colour fluorescent powders.
Claims (7)
1. a kind of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping, which is characterized in that the chemical general formula of the fluorescent powder is Sr3-xY
(BO3)3: xCe, wherein 0.01≤x≤0.15.
2. three strontium yttrium borate base blue colour fluorescent powder of cerium dopping as described in claim 1, which is characterized in that the excitation of the fluorescent powder
Spectrum is in 200~400nm, and main excitation peak is near 338nm, and for emission spectrum in 350~650nm, main peak is attached in 420nm
Closely.
3. three strontium yttrium borate base blue colour fluorescent powder of cerium dopping as claimed in claim 2, which is characterized in that the fluorescent powder energy
It is enough to issue blue light under near ultraviolet excitation.
4. a kind of preparation method of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping, which comprises the following steps:
(1) according to the chemical structural formula Sr of fluorescent powder3-xY(BO3)3: the mol ratio amount of xCe is weighed respectively containing Sr, Y, B, Ce
The compound of element is fully ground and is uniformly mixed as raw material, by weighed raw material；
(2) it by uniform raw material under air atmosphere, is calcined 5-8 hours at 1200 DEG C -1300 DEG C；
(3) it after the completion of calcining, is taken out after being cooled to room temperature, is fully ground crushing, obtains Ce3+Adulterate three strontium yttrium borate fluorescent powders
Sr3-xY(BO3)3: xCe, wherein 0.01≤x≤0.15.
5. the preparation method of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping as claimed in claim 4, which is characterized in that described
The compound containing Sr, Y, B, Ce element, respectively SrCO3、Y2O3、H3BO3、CeO2。
6. the preparation method of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping as claimed in claim 4, which is characterized in that described
Calcining, carried out in high temperature process furnances, under reducing atmosphere, from room temperature with the heating rate of 5~10 DEG C/min rise to 1200 DEG C-
1300 DEG C, keep the temperature 5-8h, later furnace cooling.
7. the preparation method of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping as claimed in claim 4, which is characterized in that described
The grinding of raw material and the grinding of post-calcination sample, milling time are 20~60min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110699079A (en) * | 2019-10-30 | 2020-01-17 | 西安建筑科技大学 | Near-infrared luminescent material and preparation method thereof |
| CN116731715A (en) * | 2023-06-13 | 2023-09-12 | 内蒙古大学 | Borate blue fluorescent powder suitable for ultraviolet excitation and preparation method thereof |
| WO2024027105A1 (en) * | 2022-08-05 | 2024-02-08 | 广东省科学院资源利用与稀土开发研究所 | Lithium sodium yttrium borate and cerium-doped compound and crystal thereof, and preparation methods therefor and use thereof |
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| JP2010285596A (en) * | 2009-03-27 | 2010-12-24 | Tohoku Univ | Oxide crystal for neutron scintillator and neutron scintillator using the same |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2010285596A (en) * | 2009-03-27 | 2010-12-24 | Tohoku Univ | Oxide crystal for neutron scintillator and neutron scintillator using the same |
Non-Patent Citations (2)
| Title |
|---|
| KRISTIN A. DENAULT等: "Structure–composition relationships and optical properties in cerium-substituted (Sr,Ba)3(Y,La)(BO3)3 borate phosphors", 《J. MATER. CHEM. C》 * |
| RAYKO SIMURA等: "Valence state of dopant and scintillation properties of Ce-doped Sr3Y(BO3)3 crystal", 《JOURNAL OF CRYSTAL GROWTH》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110699079A (en) * | 2019-10-30 | 2020-01-17 | 西安建筑科技大学 | Near-infrared luminescent material and preparation method thereof |
| CN110699079B (en) * | 2019-10-30 | 2022-07-12 | 西安建筑科技大学 | Near-infrared luminescent material and preparation method thereof |
| WO2024027105A1 (en) * | 2022-08-05 | 2024-02-08 | 广东省科学院资源利用与稀土开发研究所 | Lithium sodium yttrium borate and cerium-doped compound and crystal thereof, and preparation methods therefor and use thereof |
| CN116731715A (en) * | 2023-06-13 | 2023-09-12 | 内蒙古大学 | Borate blue fluorescent powder suitable for ultraviolet excitation and preparation method thereof |
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