CN117050749A - Europium-doped spherical fluorescent powder and preparation method thereof - Google Patents
Europium-doped spherical fluorescent powder and preparation method thereof Download PDFInfo
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- CN117050749A CN117050749A CN202311057261.2A CN202311057261A CN117050749A CN 117050749 A CN117050749 A CN 117050749A CN 202311057261 A CN202311057261 A CN 202311057261A CN 117050749 A CN117050749 A CN 117050749A
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- 239000000843 powder Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910004283 SiO 4 Inorganic materials 0.000 claims abstract description 10
- 229910017855 NH 4 F Inorganic materials 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000002243 precursor Substances 0.000 claims description 48
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 33
- 238000007873 sieving Methods 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 26
- 238000005245 sintering Methods 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 238000011068 loading method Methods 0.000 claims description 9
- 238000000967 suction filtration Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 2
- 239000006184 cosolvent Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 8
- 230000004907 flux Effects 0.000 claims 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 239000004005 microsphere Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000001000 micrograph Methods 0.000 description 15
- 239000004677 Nylon Substances 0.000 description 14
- 229910004298 SiO 2 Inorganic materials 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 14
- 229920001778 nylon Polymers 0.000 description 14
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 13
- 239000002245 particle Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 230000032683 aging Effects 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009827 uniform distribution Methods 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
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/77342—Silicates
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention relates to europium-doped spherical fluorescent powder and a preparation method thereof, belonging to the field of fluorescent powder preparation, wherein the fluorescent powder has a chemical formula A 2‑x SiO 4 :xEu 2+ Wherein A is one or two or more than two of Mg, ca, sr, ba, the value range of x is 0.005-0.2, the fluorescent powder is of a microsphere structure, and the size of the fluorescent powder is 10-30 mu m. In the preparation process of the fluorescent powder, fluxing agent is added, and the fluxing agent is prepared from NaF and NaHCO 3 And NH 4 F, the obtained fluorescent powder has the advantages of microsphere shape, regular morphology, good monodispersity, high luminous intensity and the like, is simple to prepare, is beneficial to industrial production, and has very broad application prospect.
Description
Technical Field
The invention relates to europium-doped spherical fluorescent powder and a preparation method thereof, and belongs to the field of fluorescent powder preparation.
Background
White light LEDs are a novel light source for solid illumination, and fluorescent powder conversion white light LEDs are currently in the mainstream position in the market. In the technology of converting fluorescent powder into white light LED, the fluorescent powder has very important influence on the performances of the white light LED such as luminous efficiency, service life and the like. The silicate fluorescent powder has wider adjustable emission wavelength, can emit white light when being matched with red fluorescent powder under the excitation of a blue light chip, and is mainly applied to the fields of warm white light illumination and medium-low end backlight display with low requirement on color rendering index. However, the silicate fluorescent powder prepared by the conventional method has low brightness and poor appearance, thereby influencing luminous efficiency and service life.
Disclosure of Invention
The present invention aims to provide a new technical solution to improve or solve the technical problems existing in the prior art as described above.
The technical scheme provided by the invention is as follows: europium-doped spherical fluorescent powder with chemical formula A 2-x SiO 4 :xEu 2+ Wherein A is one or more than one of Mg, ca, sr, ba, and x has a value ranging from 0.005 to 0.2.
On the basis of the technical scheme, the invention can be improved as follows.
Further, the fluorescent powder is of a microsphere structure, and the size of the fluorescent powder is 10-30 mu m.
The invention also provides a preparation method of the europium-doped spherical fluorescent powder, and a fluxing agent is added in the preparation process.
Further, the fluxing agent is prepared from NaF and NaHCO 3 And NH 4 F, one or two or more of F.
Further, the preparation method comprises the following steps:
(1) Weighing oxide and SiO corresponding to metal in fluorescent powder 2 Placing the cosolvent in a beaker, and adding absolute ethyl alcohol to obtain mixed feed liquid;
(2) Ultrasonically stirring the mixed material liquid obtained in the step (1) to completely and uniformly mix the raw materials;
(3) Carrying out suction filtration and drying on the uniform feed liquid obtained in the step (2) to obtain a fluorescent powder precursor;
(4) Sieving the precursor obtained in the step (3), loading the precursor into a crucible, sintering at a high temperature in a furnace, crushing, and sieving to obtain a fluorescent powder oxidation material;
(5) And (3) placing the fluorescent powder oxidized material obtained in the step (4) into a crucible, sintering at a high temperature in a furnace, cooling along with the furnace after the heat treatment is finished, taking out a product, crushing, and sieving to obtain the europium-doped spherical fluorescent powder.
Further, in the step (2), the ultrasonic stirring is carried out for 60 to 90 minutes at the temperature of 50 to 60 ℃.
Further, in the step (3), the mixture is dried at 90 to 120 ℃ for 10 to 14 hours.
Further, in the step (4), the sintering temperature is 800-1050 ℃, and the heat treatment is carried out for 8-10 hours.
Further, in the step (5), the sintering temperature is 1100-1300 ℃, and the heat treatment is carried out for 5-7 hours.
Further, in the step (5), heat treatment is performed in a hydrogen reducing atmosphere.
Compared with the prior art, the invention has the beneficial effects that: the europium-doped spherical fluorescent powder has the advantages of microsphere shape, regular shape, good monodispersity, high luminous intensity, easy realization of uniform distribution of rare earth elements, simple preparation, easy industrial production and very wide application prospect.
Drawings
FIG. 1 is a scanning electron microscope image of the phosphor obtained in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of the phosphor obtained in example 2 of the present invention;
FIG. 3 is a scanning electron microscope image of the phosphor powder obtained in example 3 of the present invention;
FIG. 4 is a scanning electron microscope image of the phosphor powder obtained in example 4 of the present invention;
FIG. 5 is a scanning electron microscope image of the phosphor powder obtained in example 5 of the present invention;
FIG. 6 is a scanning electron microscope image of the phosphor powder obtained in example 6 of the present invention;
FIG. 7 is a scanning electron microscope image of the phosphor obtained in comparative example 1 of the present invention;
FIG. 8 is a fluorescence spectrum of the phosphor obtained in example 1 of the present invention.
Detailed Description
The principles and features of the present invention are described below in connection with examples, which are set forth only to illustrate the present invention and not to limit the scope of the invention.
Example 1
(1) 30.72g of BaCO was weighed out 3 5.75g SrCO 3 Eu 0.95g 2 O 3 6.1g of SiO 2 0.059g NaF, 0.68g NaHCO 3 NH 0.25g 4 F, placing the mixture in a 500ml beaker, and adding 250ml of absolute ethyl alcohol to obtain a mixed solution.
(2) Stirring the mixed material liquid obtained in the step (1) for 90min at 50 ℃ by ultrasonic, so as to lead BaCO to be 3 、SrCO 3 、Eu 2 O 3 、SiO 2 Completely and uniformly mixing.
(3) And (3) transferring the uniform feed liquid obtained in the step (2) into a Buchner funnel for suction filtration, and drying at 120 ℃ for 12 hours to obtain a precursor of the fluorescent powder.
(4) And (3) sieving the precursor obtained in the step (3) with a 100-mesh nylon sieve, loading the precursor into an alumina crucible, sintering the precursor in a high-temperature furnace at a high temperature of 850 ℃, performing heat treatment for 8 hours, and crushing the precursor and sieving the crushed precursor with the 100-mesh nylon sieve to obtain the fluorescent powder oxidized material.
(5) Placing the silicate oxide obtained in the step (4) in an alumina crucible, sintering at a high temperature in a reduction furnace at 1150 ℃ for 5 hours in a hydrogen reduction atmosphere, taking out the product after the heat treatment is finished, crushing, and sieving with a 200-mesh sieve to obtain Ba 1.557 Sr 0.389 SiO 4 :0.054Eu 2+ Fluorescent powder.
FIG. 1 is a scanning electron microscope image of the phosphor powder prepared in example 1, and it can be seen from the image that the phosphor powder has a spherical morphology, a particle size of about 25 μm, a uniform particle size, and good dispersibility.
FIG. 8 is a graph showing the fluorescence spectrum of the phosphor prepared in example 1, which has an emission spectrum of about 525nm under an excitation condition of 450nm, and thus the prepared phosphor is a silicate green phosphor.
Example 2
(1) 26.8g of BaCO was weighed out 3 8.59g SrCO 3 Eu 1.06g 2 O 3 6.07g of SiO 2 0.043g NaF, 0.12g NaHCO 3 NH 0.21g 4 F, placing the mixture in a 500ml beaker, and adding 250ml of absolute ethyl alcohol to obtain a mixed solution.
(2) Stirring the mixed material liquid obtained in the step (1) for 90min at 50 ℃ by ultrasonic, so as to lead BaCO to be 3 、SrCO 3 、Eu 2 O 3 、SiO 2 Completely and uniformly mixing.
(3) And (3) transferring the uniform feed liquid obtained in the step (2) into a Buchner funnel for suction filtration, and drying at 120 ℃ for 12 hours to obtain a precursor of the fluorescent powder.
(4) And (3) sieving the precursor obtained in the step (3) with a 100-mesh nylon sieve, loading the precursor into an alumina crucible, sintering the precursor in a high-temperature furnace at a high temperature of 850 ℃, performing heat treatment for 8 hours, and crushing the precursor and sieving the crushed precursor with the 100-mesh nylon sieve to obtain the fluorescent powder oxidized material.
(5) Placing the silicate oxide obtained in the step (4) in an alumina crucible, sintering at a high temperature in a reduction furnace at 1150 ℃ for 5 hours in a hydrogen reduction atmosphere, taking out the product after the heat treatment is finished, crushing, and sieving with a 200-mesh sieve to obtain Ba 1.358 Sr 0.582 SiO 4 :0.06Eu 2+ Fluorescent powder.
FIG. 2 is a scanning electron microscope image of the phosphor powder prepared in example 2, and it can be seen from the image that the phosphor powder has a spherical morphology, uniform particle size and good dispersibility.
Example 3
(1) 22.5g of BaCO3 and 11.22g of SrCO are weighed out 3 Eu 1.76g 2 O 3 6.07g of SiO 2 0.15g NaF, 0.29g NaHCO 3 NH 0.36g 4 F, placing the mixture in a 500ml beaker, and adding 250ml of absolute ethyl alcohol to obtain a mixed solution.
(2) Stirring the mixed material liquid obtained in the step (1) for 90min at 50 ℃ by ultrasonic, so as to lead BaCO to be 3 、SrCO 3 、Eu 2 O 3 、SiO 2 Completely and uniformly mixing.
(3) And (3) transferring the uniform feed liquid obtained in the step (2) into a Buchner funnel for suction filtration, and drying at 110 ℃ for 12 hours to obtain a precursor of the fluorescent powder.
(4) And (3) sieving the precursor obtained in the step (3) with a 100-mesh nylon sieve, loading the precursor into an alumina crucible, sintering the precursor in a high-temperature furnace at a high temperature of 900 ℃, performing heat treatment for 8.5 hours, and crushing the precursor and sieving the crushed precursor with the 100-mesh nylon sieve to obtain the fluorescent powder oxidized material.
(5) Placing the silicate oxide material obtained in the step (4) into an alumina crucible, sintering at a high temperature in a reduction furnace, wherein the sintering temperature is 1150 ℃, performing heat treatment for 5.5 hours in a hydrogen reduction atmosphere, taking out the product after the heat treatment is finished, crushing, and sieving with a 200-mesh sieve to obtain Ba 1.14 Sr 0.76 SiO 4 :0.1Eu 2+ Fluorescent powder.
FIG. 3 is a scanning electron microscope image of the phosphor powder prepared in example 3, and it can be seen from the image that the phosphor powder has a spherical morphology, uniform particle size and good dispersibility.
Example 4
(1) 18.25g of BaCO was weighed out 3 13.66g SrCO 3 Eu 2.64g 2 O 3 6.07g of SiO 2 0.55g NaF, 0.49g NaHCO 3 NH 0.52g 4 F, placing the mixture in a 500ml beaker, and adding 250ml of absolute ethyl alcohol to obtain a mixed solution.
(2) Stirring the mixed material liquid obtained in the step (1) for 90min at 50 ℃ by ultrasonic, so as to lead BaCO to be 3 、SrCO 3 、Eu 2 O 3 、SiO 2 Completely and uniformly mixing.
(3) And (3) transferring the uniform feed liquid obtained in the step (2) into a Buchner funnel for suction filtration, and drying at 100 ℃ for 12 hours to obtain a precursor of the fluorescent powder.
(4) And (3) sieving the precursor obtained in the step (3) with a 100-mesh nylon sieve, loading the precursor into an alumina crucible, sintering the precursor in a high-temperature furnace at a high temperature of 1000 ℃, performing heat treatment for 9 hours, and crushing the precursor and sieving the crushed precursor with the 100-mesh nylon sieve to obtain the fluorescent powder oxidized material.
(5) Placing the silicate oxide obtained in the step (4) in an alumina crucible, sintering at a high temperature of 1200 ℃ in a reducing furnace, performing heat treatment in a hydrogen reducing atmosphere for 6 hours, taking out the product after the heat treatment is finished, crushing, and sieving with a 200-mesh sieve to obtain Ba 0.925 Sr 0.925 SiO 4 :0.15Eu 2+ Fluorescent powder.
FIG. 4 is a scanning electron microscope image of the phosphor powder prepared in example 4, and it can be seen from the image that the phosphor powder has a spherical morphology, uniform particle size and good dispersibility.
Example 5
(1) 10.66g of BaCO was weighed out 3 18.6g SrCO 3 Eu 3.49g 2 O 3 6.07g of SiO 2 1.3g NaF, 0.8g NaHCO 3 NH 0.63g 4 F, placing the mixture in a 500ml beaker, and adding 250ml of absolute ethyl alcohol to obtain a mixed solution.
(2) Stirring the mixed material liquid obtained in the step (1) for 90min at 50 ℃ by ultrasonic, so as to lead BaCO to be 3 、SrCO 3 、Eu 2 O 3 、SiO 2 Completely and uniformly mixing.
(3) And (3) transferring the uniform feed liquid obtained in the step (2) into a Buchner funnel for suction filtration, and drying at 90 ℃ for 12 hours to obtain a precursor of the fluorescent powder.
(4) And (3) sieving the precursor obtained in the step (3) with a 100-mesh nylon sieve, loading the precursor into an alumina crucible, sintering the precursor in a high-temperature furnace at a high temperature of 1050 ℃, performing heat treatment for 10 hours, and crushing the precursor and sieving the crushed precursor with the 100-mesh nylon sieve to obtain the fluorescent powder oxidized material.
(5) Placing the silicate oxide obtained in the step (4) in an alumina crucible, sintering at a high temperature in a reduction furnace at 1300 ℃, performing heat treatment in a hydrogen reduction atmosphere for 7 hours, taking out the product after the heat treatment is finished, crushing, and sieving with a 200-mesh sieve to obtain Ba 0.54 Sr 1.26 SiO 4 :0.2Eu 2+ Fluorescent powder.
FIG. 5 is a scanning electron microscope image of the phosphor powder prepared in example 5, and it can be seen from the image that the phosphor powder has a spherical morphology, uniform particle size and good dispersibility.
Example 6
(1) 7.6g of BaCO was weighed out 3 21.26g SrCO 3 Eu 3.5g 2 O 3 6.07g of SiO 2 1.3g NaF, 0.8g NaHCO 3 NH 0.63g 4 F, placing the mixture in a 500ml beaker, and adding 250ml of absolute ethyl alcohol to obtain a mixed solution.
(2) Stirring the mixed material liquid obtained in the step (1) for 90min at 50 ℃ by ultrasonic, so as to lead BaCO to be 3 、SrCO 3 、Eu 2 O 3 、SiO 2 Completely and uniformly mixing.
(3) And (3) transferring the uniform feed liquid obtained in the step (2) into a Buchner funnel for suction filtration, and drying at 90 ℃ for 12 hours to obtain a precursor of the fluorescent powder.
(4) And (3) sieving the precursor obtained in the step (3) with a 100-mesh nylon sieve, loading the precursor into an alumina crucible, sintering the precursor in a high-temperature furnace at a high temperature of 1050 ℃, performing heat treatment for 10 hours, and crushing the precursor and sieving the crushed precursor with the 100-mesh nylon sieve to obtain the fluorescent powder oxidized material.
(5) Placing the silicate oxide obtained in the step (4) in an alumina crucible, sintering at a high temperature in a reduction furnace at 1300 ℃, performing heat treatment in a hydrogen reduction atmosphere for 7 hours, taking out the product after the heat treatment is finished, crushing, and sieving with a 200-mesh sieve to obtain Ba 0.36 Sr 1.44 SiO 4 :0.2Eu 2+ Fluorescent powder.
FIG. 6 is a scanning electron microscope image of the phosphor powder prepared in example 6, and it can be seen from the image that the phosphor powder has a spherical morphology, uniform particle size and good dispersibility.
Comparative example 1
(1) 30.72g of BaCO was weighed out 3 5.75g SrCO 3 Eu 0.95g 2 O 3 6.1g of SiO 2 NH 0.3g 4 Cl was placed in a 500ml beaker, and 250ml of absolute ethanol was added to obtain a mixed solution. .
(2) Stirring the mixed material liquid obtained in the step (1) for 90min at 50 ℃ by ultrasonic, so as to lead BaCO to be 3 、SrCO 3 、Eu 2 O 3 、SiO 2 Completely and uniformly mixing.
(3) And (3) transferring the uniform feed liquid obtained in the step (2) into a Buchner funnel for suction filtration, and drying at 120 ℃ for 12 hours to obtain a precursor of the fluorescent powder.
(4) And (3) sieving the precursor obtained in the step (3) with a 100-mesh nylon sieve, loading the precursor into an alumina crucible, sintering the precursor in a high-temperature furnace at a high temperature of 850 ℃, performing heat treatment for 8 hours, and crushing the precursor and sieving the crushed precursor with the 100-mesh nylon sieve to obtain the fluorescent powder oxidized material.
(5) Placing the silicate oxide obtained in the step (4) in an alumina crucible, sintering at a high temperature in a reduction furnace at 1150 ℃ for 5 hours in a hydrogen reduction atmosphere, taking out the product after the heat treatment is finished, crushing, and sieving with a 200-mesh sieve to obtain Ba 1.557 Sr 0.389 SiO 4 :0.054Eu 2+ Silicate fluorescent powder.
TABLE 1 comparison of the performance of the example 1 phosphor and the comparative example 1 phosphor
From the data in table 1, it can be seen that the relative brightness, the package light efficiency and other performances of the phosphor of the embodiment 1 of the present invention are better than those of the phosphor of the comparative embodiment 1, and the 1000-hour aging light efficiency and aging attenuation are lower than those of the phosphor of the comparative embodiment 1, which indicates that the silicate phosphor of the present invention has the advantages of good luminescence performance and long service life.
FIG. 7 is a scanning electron microscope image of the phosphor powder produced in comparative example 1; compared with comparative example 1, the fluorescent powder scanning electron microscope images of examples 1-6 have micro-spherical appearance, more regular appearance and more uniform particle size, so the fluorescent powder of examples 1-6 is added by NaF and NaHCO by adopting the invention 3 And NH 4 Compared with the fluorescent powder prepared by adding the traditional fluxing agent, the silicate fluorescent powder has the characteristics of regular microsphere morphology, uniform particle size and good monodispersity.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (10)
1. A europium-doped spherical fluorescent powder is characterized in that the chemical formula of the fluorescent powder is A 2-x SiO 4 :xEu 2+ Wherein A is one or two or more than two of Mg, ca, sr, ba, and x has a value ranging from 0.005 to 0.2.
2. The europium-doped spherical phosphor according to claim 1, which has a micro-spherical structure and has a size of 10 to 30 μm.
3. The method for preparing the europium-doped spherical fluorescent powder according to claim 1 or 2, wherein a flux is added during the preparation.
4. The method for preparing europium-doped spherical fluorescent powder according to claim 3, wherein the flux consists of NaF and NaHCO 3 And NH 4 F, one or two or more of F.
5. The method for preparing the europium-doped spherical fluorescent powder according to claim 4, which comprises the following steps:
(1) Weighing oxide and SiO corresponding to metal in fluorescent powder 2 Placing the cosolvent in a beaker, and adding absolute ethyl alcohol to obtain mixed feed liquid;
(2) Ultrasonically stirring the mixed material liquid obtained in the step (1) to completely and uniformly mix the raw materials;
(3) Carrying out suction filtration and drying on the uniform feed liquid obtained in the step (2) to obtain a fluorescent powder precursor;
(4) Sieving the precursor obtained in the step (3), loading the precursor into a crucible, sintering at a high temperature in a furnace, crushing, and sieving to obtain a fluorescent powder oxidation material;
(5) And (3) placing the fluorescent powder oxidized material obtained in the step (4) into a crucible, sintering at a high temperature in a furnace, cooling along with the furnace after the heat treatment is finished, taking out a product, crushing, and sieving to obtain the europium-doped spherical fluorescent powder.
6. The method of preparing europium-doped spherical fluorescent powder according to claim 5, wherein in step (2), the mixture is stirred at 50℃to 60℃for 60 minutes to 90 minutes by ultrasonic wave.
7. The method according to claim 5, wherein in the step (3), the phosphor is dried at 90 to 120℃for 10 to 14 hours.
8. The method according to claim 5, wherein in the step (4), the sintering temperature is 800 to 1050 ℃, and the heat treatment is performed for 8 to 10 hours.
9. The method of preparing a europium-doped spherical phosphor according to claim 5, wherein in step (5), the sintering temperature is 1100 to 1300 ℃ and the heat treatment is carried out for 5 to 7 hours.
10. The method of preparing a europium-doped spherical fluorescent powder according to claim 9, wherein in step (5), the heat treatment is carried out in a hydrogen reducing atmosphere.
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