CN116891741B - Broadband yellow-green fluorescent powder and preparation method thereof - Google Patents
Broadband yellow-green fluorescent powder and preparation method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 6
- 229910052788 barium Inorganic materials 0.000 claims description 6
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052796 boron Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052706 scandium Inorganic materials 0.000 claims description 6
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 4
- 229910001940 europium oxide Inorganic materials 0.000 claims description 4
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 4
- GXUARMXARIJAFV-UHFFFAOYSA-L barium oxalate Chemical compound [Ba+2].[O-]C(=O)C([O-])=O GXUARMXARIJAFV-UHFFFAOYSA-L 0.000 claims description 2
- 229940094800 barium oxalate Drugs 0.000 claims description 2
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 229910052810 boron oxide Inorganic materials 0.000 claims description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 2
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 2
- DBTMQFKUVICLQN-UHFFFAOYSA-K scandium(3+);triacetate Chemical compound [Sc+3].CC([O-])=O.CC([O-])=O.CC([O-])=O DBTMQFKUVICLQN-UHFFFAOYSA-K 0.000 claims description 2
- NYMLCLICEBTBKR-UHFFFAOYSA-H scandium(3+);tricarbonate Chemical compound [Sc+3].[Sc+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NYMLCLICEBTBKR-UHFFFAOYSA-H 0.000 claims description 2
- WYXIGTJNYDDFFH-UHFFFAOYSA-Q triazanium;borate Chemical compound [NH4+].[NH4+].[NH4+].[O-]B([O-])[O-] WYXIGTJNYDDFFH-UHFFFAOYSA-Q 0.000 claims description 2
- DFCYEXJMCFQPPA-UHFFFAOYSA-N scandium(3+);trinitrate Chemical compound [Sc+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O DFCYEXJMCFQPPA-UHFFFAOYSA-N 0.000 claims 1
- 238000005286 illumination Methods 0.000 abstract description 7
- 238000006862 quantum yield reaction Methods 0.000 abstract description 7
- 238000009877 rendering Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 12
- 238000000295 emission spectrum Methods 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 238000000695 excitation spectrum Methods 0.000 description 3
- 238000005424 photoluminescence Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000003086 colorant Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 235000005105 Pinus pinaster Nutrition 0.000 description 1
- 241001236212 Pinus pinaster Species 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction 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
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7797—Borates
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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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Abstract
The invention discloses a broadband yellow-green fluorescent powder and a preparation method thereof, wherein the molecular formula of the fluorescent powder is Ba 2‑xSc2B4O11:xEu2+, wherein x is more than or equal to 0.01 and less than or equal to 0.24. The fluorescent powder is prepared by a high-temperature solid phase method, is ground after being mixed according to the material ratio, is placed in a muffle furnace for pre-calcining for 2-10 hours at 350-650 ℃ in the air atmosphere, and is placed in a tube furnace for calcining for 8-48 hours at 900-1000 ℃ in the reducing atmosphere, thus obtaining the fluorescent powder. The quantum yield of the fluorescent powder can reach 96.0% at most, the half-width of the fluorescent powder is larger than 100nm, the fluorescent powder belongs to broadband emission fluorescent powder, can be effectively matched with other fluorescent powder and applied to a Light Emitting Diode (LED) for illumination, can improve the color rendering index of the LED, improves the high lumen efficiency, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and particularly relates to efficient broadband yellow-green fluorescent powder and a preparation method thereof.
Background
With the continuous improvement of living standard, the requirements of people on the quality of illumination are higher and higher, and high-quality and full-spectrum illumination has become a new trend of healthy green illumination worldwide. The full-spectrum white light LED is an LED with wide spectrum coverage (380-780 nm), close to a solar visible light spectrum, good spectrum continuity, no obvious wave crest and wave trough in spectrum distribution, excellent color rendering index and strong color reduction capability on objects. The full spectrum white light LED has wide application in the fields of operating rooms, museums, high-end stages, health illumination, plant growth and the like.
Currently, there are two main ways to realize full spectrum LEDs. The first is a 5-color LED chip structure, i.e., a plurality of LED chips of blue, cyan, green, yellow and red light are combined to produce a continuous spectrum. The white light generated by the method has the advantages of high light efficiency and high color rendering, but the single-color chip has different performances, especially the green light and yellow light chips have much lower efficiency than other chips, so that green light gap is caused, the light attenuation difference of the chips is larger, and the problems of unstable color temperature of the white light, complex control circuit, high cost, poor application performance and the like are caused. The second method is a single-chip LED fluorescent powder coating method, namely, the ultraviolet/near ultraviolet chips are matched with fluorescent powder with various colors. Compared with a multi-chip LED, the method has the advantages of stable and uniform light color, simple manufacturing method, low cost and the like, and therefore, the method becomes a main stream mode of the current full-spectrum white light LED. To obtain an LED with high color rendering properties similar to solar spectrum, fluorescent powder with multiple colors including blue (400-480 nm), cyan (470-505 nm), yellow-green (515-535 nm), yellow (540-575 nm) and red (600-780) needs to be compounded by a single purple light or near ultraviolet light chip.
Disclosure of Invention
The invention aims to provide high-efficiency broadband emission yellow-green fluorescent powder capable of being excited by near ultraviolet light and a preparation method thereof.
Aiming at the purposes, the molecular formula of the yellow-green fluorescent powder adopted by the invention is Ba 2-xSc2B4O11:xEu2+, wherein x is more than or equal to 0.01 and less than or equal to 0.24.
In the molecular formula of the yellow-green fluorescent powder, x is preferably more than or equal to 0.04 and less than or equal to 0.16.
The preparation method of the yellow-green fluorescent powder comprises the following steps: adding a barium source, a scandium source, a boron source and europium oxide into a mortar according to the molar ratio of 1.88-2:2:4-4.5:0.01-0.24, grinding and mixing uniformly, placing the mixture into a muffle furnace, pre-calcining for 2-10 hours in an air atmosphere at 350-650 ℃, taking out, continuously grinding, placing the mixture into a tube furnace, calcining for 8-48 hours in a reducing atmosphere at 900-1000 ℃, and controlling the gas flow to be 20-40 mL/min; grinding the calcined product, washing with distilled water and ethanol at 60-80 ℃ in sequence, and drying to obtain the broadband yellow-green fluorescent powder.
In the preparation method, preferably, a barium source, a scandium source, a boron source and europium oxide are added into a mortar, ground and mixed uniformly, placed into a muffle furnace, pre-calcined for 3-4 hours in an air atmosphere at 450-550 ℃, taken out and continuously ground, placed into a tube furnace, calcined for 24-48 hours in a reducing atmosphere at 930-950 ℃, and the gas flow rate is controlled to be 25-35 mL/min.
The barium source is any one of barium carbonate, barium oxalate and barium oxide.
The scandium source is any one of scandium oxide, scandium acetate, nitric acid, and scandium carbonate.
The boron source is any one of boric acid, boron oxide and ammonium borate.
In the preparation method, the reducing atmosphere is a mixed gas of hydrogen and nitrogen, wherein the volume concentration of the hydrogen is 10%.
The beneficial effects of the invention are as follows:
The invention takes Ba 2Sc2B4O11 as a matrix to prepare the novel high-efficiency broadband yellow-green fluorescent powder taking Eu 2+ as an activator, the quantum yield is up to 96.0%, the half-peak width is up to 116.0nm, the fluorescent powder can be effectively matched with other fluorescent powder and applied to a light-emitting diode (LED) for illumination, the color rendering index of the LED can be improved, the high lumen efficiency is improved, and the fluorescent powder has wide application prospect.
Drawings
Fig. 1 is an XRD pattern of Ba 1.96Sc2B4O11:0.04Eu2+ phosphor prepared in example 1.
FIG. 2 is a photoluminescence fluorescence plot (solid line is excitation spectrum plot, and dotted line is emission spectrum plot) of Ba 1.96Sc2B4O11:0.04Eu2+ phosphor prepared in example 1.
Fig. 3 is an XRD pattern of Ba 1.92Sc2B4O11:0.08Eu2+ phosphor prepared in example 2.
FIG. 4 is a photoluminescence fluorescence plot (solid line is excitation spectrum plot, and dotted line is emission spectrum plot) of Ba 1.92Sc2B4O11:0.08Eu2+ phosphor prepared in example 2.
Fig. 5 is an XRD pattern of Ba 1.84Sc2B4O11:0.16Eu2+ phosphor prepared in example 3.
FIG. 6 is a photoluminescence fluorescence plot (solid line is excitation spectrum plot, dotted line is emission spectrum plot) of Ba 1.84Sc2B4O11:0.16Eu2+ phosphor prepared in example 3.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, but the scope of the present invention is not limited to these examples.
Example 1
Weighing 0.774g(3.92mmol)BaCO3、0.275g(2mmol)Sc2O3、0.519g(8.4mmol)H3BO3、0.0141g(0.04mmol)Eu2O3,, uniformly mixing, grinding in an agate mortar for 30 minutes, then placing a ground sample into an alumina crucible, placing the alumina crucible into a box-type resistance furnace, calcining at 550 ℃ for 3 hours in an air atmosphere, grinding a calcined product, placing the calcined product into the alumina crucible, placing the alumina crucible into a tube furnace, and calcining at 950 ℃ for 36 hours in a reducing atmosphere, wherein the reducing atmosphere is a mixed gas of hydrogen and nitrogen, and the volume concentration of the hydrogen is 10 percent and the gas flow is 25mL/min. Washing with distilled water and ethanol at 60-80 deg.c successively and drying to obtain Ba 1.96Sc2B4O11:0.04Eu2+ fluorescent powder.
The prepared fluorescent powder is tested by using a DX-2700BH powder X-ray diffractometer of the company of Dandong instruments; the test conditions were: cuK alpha radiation, 40KV voltage, 30mA current, 5-70 DEG scanning range, 10 DEG/min scanning speed and 0.02 DEG step length), and a F-7100 fluorescence spectrometer manufactured by Hitachi Corp.to perform luminescence performance test, followed by a C9920-02G quantum yield measurement system of Pinus maritima to perform quantum yield test. As can be seen from fig. 1, the diffraction peak of the prepared fluorescent powder is consistent with the simulated diffraction peak of the Ba 2Sc2B4O11 crystal, which indicates that the prepared fluorescent powder is in a pure phase. As shown in FIG. 2, under 365nm excitation light, the prepared fluorescent powder has an emission peak at 550nm, and belongs to d- & gt f characteristic transition emission of Eu 2+, which indicates that the sample emits yellow light, and the half-peak width of the emission spectrum is 116nm, and the half-peak width is wider, and belongs to obvious broadband emission, and the fluorescent powder can be used for a full-spectrum illumination LED excited by near ultraviolet. The quantum yield was measured to be 90.6%.
Example 2
Weighing 0.758g(3.84mmol)BaCO3、0.275g(2mmol)Sc2O3、0.544g(8.8mmol)H3BO3、0.0281g(0.08mmol)Eu2O3,, uniformly mixing, grinding in an agate mortar for 30 minutes, then placing a ground sample into an alumina crucible, placing the alumina crucible into a box-type resistance furnace, calcining at 450 ℃ for 4 hours in an air atmosphere, grinding a calcined product, placing the calcined product into the alumina crucible, placing the alumina crucible into a tube furnace, and calcining at 950 ℃ for 24 hours in a reducing atmosphere, wherein the reducing atmosphere is a mixed gas of hydrogen and nitrogen, and the volume concentration of the hydrogen is 10 percent and the gas flow is 30mL/min. Washing with distilled water and ethanol at 60-80 deg.c successively and drying to obtain Ba 1.92Sc2B4O11:0.08Eu2+ fluorescent powder.
As can be seen from fig. 3, the diffraction peak of the prepared fluorescent powder is consistent with the simulated diffraction peak of the Ba 2Sc2B4O11 crystal, which indicates that the prepared fluorescent powder is in a pure phase. As shown in FIG. 4, under 365nm excitation light, the emission peak of the prepared fluorescent powder is located at 543nm, and the emission peak belongs to d- & gt f characteristic transition emission of Eu 2+, which indicates that the sample emits yellow light, and the half-peak width of the emission spectrum is 110nm, and the half-peak width is wider, and the fluorescent powder belongs to obvious broadband emission, and can be used for full-spectrum LEDs excited by near ultraviolet. The quantum yield was determined to be 96.0%.
Example 3
Weighing 0.726g(3.68mmol)BaCO3、0.275g(2mmol)Sc2O3、0.495g(8mmol)H3BO3、0.0562g(0.16mmol)Eu2O3,, uniformly mixing, grinding in an agate mortar for 30 minutes, then placing a ground sample into an alumina crucible, placing the alumina crucible into a box-type resistance furnace, calcining at 450 ℃ for 4 hours in an air atmosphere, grinding a calcined product, placing the calcined product into the alumina crucible, placing the alumina crucible into a tube furnace, and calcining at 930 ℃ for 48 hours in a reducing atmosphere, wherein the reducing atmosphere is a mixed gas of hydrogen and nitrogen, and the volume concentration of the hydrogen is 10 percent and the gas flow is 35mL/min. Washing with distilled water and ethanol at 60-80 deg.c successively and drying to obtain Ba 1.84Sc2B4O11:0.16Eu2+ fluorescent powder.
As can be seen from fig. 3, the diffraction peak of the prepared fluorescent powder is consistent with the simulated diffraction peak of the Ba 2Sc2B4O11 crystal, which indicates that the prepared fluorescent powder is in a pure phase. As shown in FIG. 4, under 365nm excitation light, the emission peak of the prepared fluorescent powder is located at 530nm, and the fluorescent powder belongs to d- & gt f characteristic transition emission of Eu 2+, which indicates that the sample emits yellow green light, the half-peak width of the emission spectrum is 103nm, the half-peak width is wider, and the fluorescent powder belongs to obvious broadband emission, and can be used for a full-spectrum LED excited by near ultraviolet. The quantum yield was found to be 91.4%.
Claims (5)
1. A broadband yellow-green fluorescent powder is characterized in that: the molecular formula of the fluorescent powder is Ba 2-xSc2B4O11:xEu2+, wherein x is more than or equal to 0.01 and less than or equal to 0.24.
2. The broadband yellow-green phosphor of claim 1, wherein: x in the molecular formula is more than or equal to 0.04 and less than or equal to 0.16.
3. A method for preparing the broadband yellow-green fluorescent powder according to claim 1, which is characterized in that: adding a barium source, a scandium source, a boron source and europium oxide into a mortar according to the molar ratio of 1.88-2:2:4-4.5:0.01-0.24, grinding and mixing uniformly, placing the mixture into a muffle furnace, pre-calcining for 2-10 hours in an air atmosphere at 350-650 ℃, taking out, continuously grinding, placing the mixture into a tube furnace, calcining for 8-48 hours in a reducing atmosphere at 900-1000 ℃, and controlling the gas flow to be 20-40 mL/min; grinding the calcined product, washing with distilled water and ethanol at 60-80 ℃ in sequence, and drying to obtain broadband yellow-green fluorescent powder;
The barium source is any one of barium carbonate, barium oxalate and barium oxide;
the scandium source is any one of scandium oxide, scandium acetate, scandium nitrate and scandium carbonate;
The boron source is any one of boric acid, boron oxide and ammonium borate.
4. The method for preparing the broadband yellow-green fluorescent powder according to claim 3, wherein the method comprises the following steps: adding a barium source, a scandium source, a boron source and europium oxide into a mortar, grinding and mixing uniformly, placing the mixture into a muffle furnace, pre-calcining for 3-4 hours in an air atmosphere at 450-550 ℃, taking out and continuously grinding, placing the mixture into a tube furnace, calcining for 24-48 hours in a reducing atmosphere at 930-950 ℃, and controlling the gas flow to be 25-35 mL/min.
5. The method for preparing the broadband yellow-green fluorescent powder according to claim 3 or 4, wherein the method comprises the following steps: the reducing atmosphere is a mixed gas of hydrogen and nitrogen, wherein the volume concentration of the hydrogen is 10%.
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