CN117343729A - Eu (Eu) 2+ High quantum efficiency doped cyan fluorescent powder and preparation method thereof - Google Patents
Eu (Eu) 2+ High quantum efficiency doped cyan fluorescent powder and preparation method thereof Download PDFInfo
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- CN117343729A CN117343729A CN202311278160.8A CN202311278160A CN117343729A CN 117343729 A CN117343729 A CN 117343729A CN 202311278160 A CN202311278160 A CN 202311278160A CN 117343729 A CN117343729 A CN 117343729A
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- 239000000843 powder Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims description 15
- 239000002994 raw material Substances 0.000 claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 229910001940 europium oxide Inorganic materials 0.000 claims abstract description 8
- 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 abstract description 8
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 7
- 239000011777 magnesium Substances 0.000 claims description 27
- 238000000227 grinding Methods 0.000 claims description 23
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 18
- 238000001354 calcination Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000012752 auxiliary agent Substances 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 29
- 230000005284 excitation Effects 0.000 abstract description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 4
- 238000005286 illumination Methods 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 2
- 238000004020 luminiscence type Methods 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 229910052693 Europium Inorganic materials 0.000 abstract 2
- -1 europium ions Chemical class 0.000 abstract 2
- 238000000034 method Methods 0.000 abstract 1
- 239000007790 solid phase Substances 0.000 abstract 1
- 229910052878 cordierite Inorganic materials 0.000 description 6
- 229910052593 corundum Inorganic materials 0.000 description 6
- 239000010431 corundum Substances 0.000 description 6
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 6
- 238000000695 excitation spectrum Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 108010043121 Green Fluorescent Proteins Proteins 0.000 description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000003086 colorant Substances 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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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
- C09K11/77344—Aluminosilicates
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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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses Eu 2+ High quantum efficiency cyan phosphor is doped. The chemical composition of the cyan fluorescent powder is as follows: (Mg) 1‑ x Eu x ) 2 Al 4 Si 5 O 18 Wherein x is Eu 2+ Doped with Mg 2+ The mole percentage of the position is more than or equal to 0.05 and less than or equal to 0.13. Silica, alumina, magnesia and europium oxide are used as raw material powder, and the solid phase sintering method is adopted. According to the cyan fluorescent material provided by the invention, the europium ions of the luminescent ions are doped in high concentration, so that the europium ions are promoted to enter the pore canal, and high-efficiency luminescence is realized. The fluorescent material emits green light under the excitation of ultraviolet light, the emission wavelength range is 400-700 nm, and the quantum efficiency of the fluorescent material can reach 90.2%. Compared with red fluorescent powder SrAlSiN in the prior art 3 :Eu 2+ ,CaAlSiN 3 :Eu 2+ And the like, can obtain high quality under the excitation of ultraviolet lightCan meet the requirements of the general illumination field on different types of light sources.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and in particular relates to Eu 2+ A high quantum efficiency cyan fluorescent powder and a preparation method thereof.
Background
The white light emitting diode (w-LED) has the advantages of high luminous efficiency, low energy consumption, environmental protection, long service life and the like, and is widely applied to various illumination fields. The most popular w-LEDs on the market to date are phosphor converted LEDs, which are typically composed of a blue chip and a yellow phosphor Y 3 Al 5 O 12 :Ce 3+ (YAG:Ce 3+ ) Composition is prepared. However, the emission spectrum of Ce-YAG is in disorder, the light color proportion is not enough red light component, and the packaged w-LED has the difficult problems of poor color rendering property (CRI-60) and low light color quality. Recently, near ultraviolet excited white light LED schemes have been favored. The scheme adopts three primary colors (red, green and blue) mixed fluorescent powder to be coated on a chip capable of generating near ultraviolet emission, and the three primary colors fluorescent powder fully absorbs the emission of the chip and is excited to emit red, green and blue emission light, so that white light is obtained through compounding. The luminous performance is only determined by the fluorescent powder, so that the color rendering index is high, the color temperature is low, and the stability is good.
However, the green phosphor currently on the market has relatively low luminous efficiency, such as commercial (Ba, sr) 2 SiO 4 :Eu 2+ The quantum efficiency of the green fluorescent powder is about 70%, more green fluorescent powder is needed to be added to meet the same light-emitting requirement, and the production cost is increased. Therefore, a chip which is well matched with the near ultraviolet chip and has luminous efficiency is soughtThe high green fluorescent powder reduces the production cost of near ultraviolet excitation type white light, and becomes a problem to be solved by the technicians in the field.
Disclosure of Invention
It is an object of the present invention to provide Eu 2+ High quantum efficiency cyan fluorescent powder doped by Eu 2+ As the luminescent ion, high concentration doping is adopted to realize Eu 2+ The cordierite pore canal is occupied to realize high-efficiency luminescence, so that the problems of low luminous efficiency and low luminous brightness of the green fluorescent powder in the prior art are solved.
It is another object of the present invention to provide Eu as described above 2+ The preparation method of the doped high quantum efficiency cyan fluorescent powder is environment-friendly and energy-saving, and is easy to realize industrial production.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
eu (Eu) 2+ The high quantum efficiency cyan fluorescent powder is doped, and the chemical composition of the cyan fluorescent powder is as follows:
(Mg 1-x Eu x ) 2 Al 4 Si 5 O 18 ；
wherein x is Eu 2+ Doped with Mg 2+ The mole percentage of the position is more than or equal to 0.05 and less than or equal to 0.13.
The cyan fluorescent material provided by the invention emits cyan light under ultraviolet excitation, the emission wavelength range is 400-700 nm, and the quantum efficiency of the fluorescent material can reach 90.2%.
The present invention also provides Eu 2+ The preparation method of the doped high quantum efficiency cyan fluorescent powder specifically comprises the following steps:
(1) According to the chemical formula (Mg 1-x Eu x ) 2 Al 4 Si 5 O 18 The stoichiometric ratio of each element in x is more than or equal to 0.05 and less than or equal to 0.13, silicon dioxide, aluminum oxide, magnesium oxide and europium oxide are respectively weighed as raw material powder, and lanthanum oxide is added as sintering auxiliary agent;
(2) Adding the raw material powder weighed in the step (1) into an agate grinding pot according to the proportion, and grinding until the raw material powder is uniformly mixed;
(3) Calcining the ground powder in the step (1) in a reducing atmosphere at 1250-1400 ℃ for 3-8 h; and cooling the sintered body, and grinding the cooled sintered body into powder to obtain the cyan fluorescent powder.
Preferably, the addition amount of the sintering aid lanthanum oxide in the step (1) is 1-8wt% of the total mass of the raw material powder.
Preferably, the grinding time in the step (2) is 40 min-100 min.
Preferably, the reducing atmosphere in step (3) is 10 to 20vol% H 2 With 80-90vol% N 2 Is a mixed gas of (a) and (b).
Compared with the prior art, the invention has the following beneficial effects:
1. eu of the present invention 2+ The doped high quantum efficiency cyan fluorescent powder has wider excitation and emission ranges, has wider strong excitation in a near ultraviolet band, can realize a near white light LED device after being assembled with a near ultraviolet chip, and can meet the industrial requirements to a greater extent.
2. The preparation method is simple, easy to operate, low in equipment cost and pollution-free; can generate huge social benefit and economic benefit, and is suitable for popularization and use;
3. eu of the present invention 2+ The high-quantum-efficiency cyan fluorescent powder is doped to be combined with the red fluorescent powder in the prior art, so that high-quality white light can be obtained under near ultraviolet excitation, and the requirements of the general illumination field on different types of light sources can be met.
Drawings
FIG. 1 is an XRD pattern of fluorescent materials prepared in examples 1 to 5 of the present invention;
FIG. 2 is an excitation spectrum of the fluorescent material of example 5 of the present invention at 500nm emission;
FIG. 3 is an emission spectrum of the fluorescent material prepared in example 5 of the present invention under ultraviolet excitation at 380 nm;
FIG. 4 shows the composition of the present invention (Mg 0.87 Eu 0.13 ) 2 Al 4 Si 5 O 18 And (3) testing the luminous quantum efficiency of the sample.
Detailed Description
The invention will be described in further detail with reference to the drawings and the specific examples.
Example 1: preparation of the compound of formula (Mg) 0.95 Eu 0.05 ) 2 Al 4 Si 5 O 18 Is a blue fluorescent material of (a).
(1) The mass of the target product was set to 20g, according to the chemical formula (Mg 0.95 Eu 0.05 ) 2 Al 4 Si 5 O 18 The stoichiometric ratios of the respective elements were respectively weighed out as raw material powders of silica (10.038 g), alumina (6.814 g), magnesia (2.558 g) and europium oxide (0.587 g). Lanthanum oxide (0.2 g) was added as a sintering aid in an amount of 1% by mass of the total raw material powder.
(2) Adding the raw material powder weighed in the step (1) into an agate grinding pot according to the proportion, grinding for 40min, and uniformly mixing;
(3) The ground powder is placed in a corundum crucible and is placed in a tube furnace at 10vol%H 2 ～90vol％N 2 Calcining at 1400 ℃ in a reducing atmosphere, wherein the heating rate is 3 ℃/min, and the heat preservation time is 3h. And cooling the sintered body, and grinding the cooled sintered body into powder to obtain the silicate cyan fluorescent powder.
The (Mg) obtained in this example 0.95 Eu 0.05 ) 2 Al 4 Si 5 O 18 XRD measured on the fluorescent material of (C) indicates that the fluorescent material is prepared by cordierite Mg 2 Al 4 Si 5 O 18 As pure phase, as in fig. 1; the excitation spectrum of the fluorescent material is between 220 and 440 nm. Green light is emitted under the excitation of 380nm ultraviolet light, and the emission wavelength range is 400-700 nm. Through the test, the internal quantum efficiency of the sample was 78.4%.
Example 2: preparation of the compound of formula (Mg) 0.93 Eu 0.07 ) 2 Al 4 Si 5 O 18 Is a blue fluorescent material of (a).
(1) The mass of the target product was set to 20g, according to the chemical formula (Mg 0.93 Eu 0.07 ) 2 Al 4 Si 5 O 18 The stoichiometric ratio of each element is respectively weighing silicon dioxide (9.948 g), aluminum oxide (6.753 g) and oxidationMagnesium (2.482 g) and europium oxide (0.8157 g) were used as raw material powders. Lanthanum oxide (0.6 g) was added as a sintering aid in an amount of 3% by mass of the total raw material powder.
(2) Adding the raw material powder weighed in the step (1) into an agate grinding pot according to the proportion, grinding for 50min, and uniformly mixing;
(3) Placing the ground powder into a corundum crucible, and placing into a tube furnace at 15% H 2 ～85％N 2 Calcining at 1350 ℃ in a reducing atmosphere, heating at a rate of 3 ℃/min, and preserving the heat for 4h. Cooling the sintered body, grinding into powder to obtain the silicate cyan fluorescent powder
The (Mg) obtained in this example 0.93 Eu 0.07 ) 2 Al 4 Si 5 O 18 XRD measured on the fluorescent material of (C) indicates that the fluorescent material is prepared by cordierite Mg 2 Al 4 Si 5 O 18 As pure phase, as in fig. 1; the excitation spectrum of the fluorescent material is between 220 and 440 nm. Green light is emitted under the excitation of 380nm ultraviolet light, and the emission wavelength range is 400-700 nm. The internal quantum efficiency of this sample was 81.3% by testing.
Example 3: preparation of the compound of formula (Mg) 0.91 Eu 0.09 ) 2 Al 4 Si 5 O 18 Is a blue fluorescent material of (a).
(1) The mass of the target product was set to 20g, according to the chemical formula (Mg 0.91 Eu 0.09 ) 2 Al 4 Si 5 O 18 The stoichiometric ratios of the respective elements were respectively weighed out as raw material powders of silica (9.860 g), alumina (6.692 g), magnesia (2.407 g) and europium oxide (1.039 g). Lanthanum oxide (1.0 g) was added as a sintering aid in an amount of 5% by mass of the total raw material powder.
(2) Adding the raw material powder weighed in the step (1) into an agate grinding pot according to the proportion, grinding for 60min, and uniformly mixing;
(3) Placing the ground powder into a corundum crucible, placing the corundum crucible into a tube furnace, calcining at 1350 ℃ in a reducing atmosphere of 15% H2 to 85% N2, heating at a rate of 3 ℃/min, and preserving the heat for 5h. Cooling the sintered body, grinding into powder to obtain the silicate cyan fluorescent powder
The (Mg) obtained in this example 0.91 Eu 0.09 ) 2 Al 4 Si 5 O 18 XRD measured on the fluorescent material of (C) indicates that the fluorescent material is prepared by cordierite Mg 2 Al 4 Si 5 O 18 As pure phase, as in fig. 1; the excitation spectrum of the fluorescent material is between 220 and 440 nm. Green light is emitted under the excitation of 380nm ultraviolet light, and the emission wavelength range is 400-700 nm. The internal quantum efficiency of this sample was 85.4% by testing.
Example 4: preparation of the compound of formula (Mg) 0.89 Eu 0.11 ) 2 Al 4 Si 5 O 18 Is a blue fluorescent material of (a).
(1) The mass of the target product was set to 20g, according to the chemical formula (Mg 0.89 Eu 0.11 ) 2 Al 4 Si 5 O 18 The stoichiometric ratios of the respective elements were respectively weighed out as raw material powders of silica (9.773 g), alumina (6.634 g), magnesia (2.334 g) and europium oxide (1.259 g). Lanthanum oxide (1.4 g) was added as a sintering aid in an amount of 7% by mass of the total raw material powder.
(2) Adding the raw material powder weighed in the step (1) into an agate grinding pot according to the proportion, grinding for 80min, and uniformly mixing;
(3) Placing the ground powder into a corundum crucible, and placing into a tube furnace at 20% H 2 ～80％N 2 Calcining at 1300 ℃ in a reducing atmosphere, wherein the heating rate is 3 ℃/min, and the heat preservation time is 7h. Cooling the sintered body, grinding into powder to obtain the silicate cyan fluorescent powder
The (Mg) obtained in this example 0.89 Eu 0.11 ) 2 Al 4 Si 5 O 18 XRD measured on the fluorescent material of (C) indicates that the fluorescent material is prepared by cordierite Mg 2 Al 4 Si 5 O 18 As pure phase, as in fig. 1; the excitation spectrum of the fluorescent material is between 220 and 440 nm. Green light is emitted under the excitation of 380nm ultraviolet light, and the emission wavelength range is 400-700 nm. Through the test, the internal quantum efficiency of the sample was 87.8%.
Example 5: preparation of the compound of formula (Mg) 0.87 Eu 0.13 ) 2 Al 4 Si 5 O 18 Is a blue fluorescent material of (a).
(1) The mass of the target product was set to 20g, according to the chemical formula (Mg 0.87 Eu 0.13 ) 2 Al 4 Si 5 O 18 The stoichiometric ratio of each element was respectively weighed out as raw material powders of silica (9.687 g), alumina (6.575 g), magnesia (2.261 g) and europium oxide (1.475 g). Lanthanum oxide (1.6 g) was added as a sintering aid in an amount of 8% by mass of the total raw material powder.
(2) Adding the raw material powder weighed in the step (1) into an agate grinding pot according to the proportion, grinding for 100min, and uniformly mixing;
(3) Placing the ground powder into a corundum crucible, and placing into a tube furnace at 20% H 2 ～80％N 2 Calcining at 1250 ℃ in reducing atmosphere, wherein the heating rate is 3 ℃/min, and the heat preservation time is 8h. And cooling the sintered body, and grinding the cooled sintered body into powder to obtain the cyan fluorescent powder.
The (Mg) obtained in this example 0.87 Eu 0.13 ) 2 Al 4 Si 5 O 18 XRD measured on the fluorescent material of (C) indicates that the fluorescent material is prepared by cordierite Mg 2 Al 4 Si 5 O 18 As pure phase, as in fig. 1; the excitation spectrum of the fluorescent material is between 220 and 440nm, as shown in figure 2; green light is emitted under the excitation of 380nm ultraviolet light, and the emission wavelength range is between 400 and 700nm, as shown in figure 3; the internal quantum efficiency of this sample was 90.2% by testing, as shown in fig. 4.
The foregoing is merely illustrative of specific embodiments of the present invention, and the scope of the invention is not limited thereto, but any modifications, equivalents, improvements and alternatives falling within the spirit and principles of the present invention will be apparent to those skilled in the art within the scope of the present invention.
Claims (5)
1. Eu (Eu) 2+ The high quantum efficiency cyan fluorescent powder is doped, and is characterized in that the cyan fluorescent powder comprises the following chemical components:
(Mg 1-x Eu x ) 2 Al 4 Si 5 O 18 ；
wherein x is Eu 2+ Doped with Mg 2+ The mole percentage of the position is more than or equal to 0.05 and less than or equal to 0.13.
2. Eu as claimed in claim 1 2+ The preparation method of the doped high quantum efficiency cyan fluorescent powder is characterized by comprising the following steps of:
(1) According to the chemical formula (Mg 1-x Eu x ) 2 Al 4 Si 5 O 18 The stoichiometric ratio of each element in x is more than or equal to 0.05 and less than or equal to 0.13, silicon dioxide, aluminum oxide, magnesium oxide and europium oxide are respectively weighed as raw material powder, and lanthanum oxide is added as sintering auxiliary agent;
(2) Adding the raw material powder weighed in the step (1) into an agate grinding pot according to the proportion, and grinding until the raw material powder is uniformly mixed;
(3) Calcining the ground powder in the step (1) in a reducing atmosphere at 1250-1400 ℃ for 3-8 h; and cooling the sintered body, and grinding the cooled sintered body into powder to obtain the cyan fluorescent powder.
3. The Eu of claim 2 2+ The preparation method of the doped high quantum efficiency cyan fluorescent powder is characterized in that the addition amount of the sintering aid lanthanum oxide in the step (1) is 1-8wt% of the total mass of the raw material powder.
4. The Eu of claim 2 2+ The preparation method of the doped high quantum efficiency cyan fluorescent powder is characterized in that the grinding time in the step (2) is 40-100 min.
5. The Eu of claim 2 2+ The preparation method of the doped high quantum efficiency cyan fluorescent powder is characterized in that the reducing atmosphere in the step (3) is 10-20vol% H 2 With 80-90vol% N 2 Is a mixed gas of (a) and (b).
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