CN115746838B - Preparation method and application of novel blue-green fluorescent powder - Google Patents
Preparation method and application of novel blue-green fluorescent powder Download PDFInfo
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- CN115746838B CN115746838B CN202211444249.2A CN202211444249A CN115746838B CN 115746838 B CN115746838 B CN 115746838B CN 202211444249 A CN202211444249 A CN 202211444249A CN 115746838 B CN115746838 B CN 115746838B
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- 239000000843 powder Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920000642 polymer Polymers 0.000 claims abstract description 43
- 238000010438 heat treatment Methods 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000000178 monomer Substances 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000004132 cross linking Methods 0.000 claims abstract description 13
- 238000001704 evaporation Methods 0.000 claims abstract description 13
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 4
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 230000000379 polymerizing effect Effects 0.000 claims description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 238000005286 illumination Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 description 25
- 238000000295 emission spectrum Methods 0.000 description 22
- 230000005284 excitation Effects 0.000 description 22
- 238000000695 excitation spectrum Methods 0.000 description 13
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 12
- 238000000197 pyrolysis Methods 0.000 description 9
- 238000009826 distribution Methods 0.000 description 8
- UWGIJJRGSGDBFJ-UHFFFAOYSA-N dichloromethylsilane Chemical compound [SiH3]C(Cl)Cl UWGIJJRGSGDBFJ-UHFFFAOYSA-N 0.000 description 6
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 description 3
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 3
- 239000005052 trichlorosilane Substances 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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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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- Luminescent Compositions (AREA)
Abstract
The invention discloses a preparation method of novel blue-green fluorescent powder, which comprises the following steps: dispersing polymer monomers into an organic solvent to form a uniform solution, carrying out hydrolytic polymerization under the stirring condition, and then transferring into a heating furnace; step two, slowly heating the solution in a reducing atmosphere, preserving the temperature for a period of time in a low temperature area, evaporating the solvent and generating a crosslinking reaction between polymers; and thirdly, continuously increasing the temperature in a reducing atmosphere to enable the polymer to undergo an inorganic decomposition reaction, naturally cooling to obtain target powder, and further discloses the blue-green fluorescent material obtained by the preparation method and the application thereof.
Description
Technical Field
The invention belongs to the technical field of fluorescent powder preparation, and particularly relates to a preparation method and application of novel blue-green fluorescent powder.
Background
Fluorescent materials are widely applied to industries such as illumination, display and the like, and mainly comprise red powder, yellow powder, green powder and the like. The traditional fluorescent powder material mostly adopts an inorganic ceramic structure with rare earth elements as luminous centers, such as BAM powder, YAG powder and the like. These fluorescent materials require doping with rare earth elements and require high sintering temperatures, so the manufacturing costs are very high. In addition, the ceramic structure sintered at high temperature is easy to agglomerate or grow up, so that the ceramic fluorescent powder prepared by sintering is unevenly distributed, and small-particle powder is difficult to obtain.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method and application of novel blue-green fluorescent powder.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the novel blue-green fluorescent powder is characterized in that the novel blue-green fluorescent material is inorganic submicron powder formed by polymerizing monomers to form polymers and then pyrolyzing the polymers, and the preparation method comprises the following steps:
dispersing polymer monomers into an organic solvent to form a uniform solution, carrying out hydrolytic polymerization under the stirring condition, and then transferring into a heating furnace;
step two, slowly heating the solution in a reducing atmosphere, preserving the temperature for a period of time in a low temperature area, evaporating the solvent and generating a crosslinking reaction between polymers;
and thirdly, continuously increasing the temperature in a reducing atmosphere to enable the polymer to undergo an inorganic decomposition reaction, and naturally cooling to obtain target powder.
Preferably, the polymer monomer in the first step is a silane structure substituted by two or three chlorine atoms
Or->Wherein R is 1 ，R 2 ，R 3 Is hydrogen atom or alkyl group, and the alkyl group comprises methyl, ethyl, propyl and isopropyl.
Preferably, the solution in the first step is any one or more of polymer monomers mixed and dispersed in an organic solvent, and the organic solvent is common organic solvents such as ethanol, n-heptane, acetone and the like.
Preferably, the reducing atmosphere in the second step is ammonia or hydrogen.
Preferably, the slow heating in the second step means 0.5-2 ℃/min.
Preferably, the low temperature condition in the second step is 150-300 ℃.
Preferably, the low-temperature heat preservation time in the second step is 0.5-2 h.
Preferably, the temperature range of the continuous rise in the third step is 400-1000 ℃.
Preferably, the high temperature heat preservation time in the third step is 1h-4h.
In a second aspect, a novel blue-green fluorescent material obtained by a preparation method of blue-green fluorescent powder and application thereof.
In summary, due to the adoption of the technical scheme, the beneficial effects of the invention are as follows:
compared with the traditional rare earth luminescent fluorescent powder material, the novel fluorescent powder prepared by the method does not need rare earth element doping, and reduces the cost of raw materials.
The novel fluorescent powder prepared by the method can be obtained under the low-temperature condition, and compared with the traditional fluorescent powder, the novel fluorescent powder has the advantage of reduced manufacturing cost.
The raw material of the invention is liquid polymer monomer, and the liquid phase method can lead the particles of the fluorescent powder to be smaller, the nano-scale and the particle size distribution to be more uniform.
Drawings
FIG. 1 is a morphology of a phosphor obtained in example 2 of the present invention;
FIG. 2 is the excitation and emission spectra of the phosphor obtained in example 2 of the present invention;
FIG. 3 is an excitation and emission spectrum of the phosphor obtained in example 3 of the present invention;
FIG. 4 shows excitation and emission spectra of the phosphor obtained in example 4 of the present invention;
FIG. 5 is a morphology of the phosphor obtained in example 5 of the present invention;
FIG. 6 is an excitation and emission spectrum of the phosphor obtained in example 5 of the present invention;
FIG. 7 is a morphology of the phosphor obtained in example 6 of the present invention;
FIG. 8 is an excitation and emission spectrum of the phosphor obtained in example 6 of the present invention;
FIG. 9 is a morphology of the phosphor obtained in example 6 of the present invention;
FIG. 10 is an excitation and emission spectrum of the phosphor obtained in example 7 of the present invention.
Detailed Description
The following is a detailed description of a preparation method and application of the novel blue-green fluorescent powder according to the present invention with reference to fig. 1 to 10. The preparation method and application of the novel blue-green fluorescent powder are not limited to the description of the following examples.
Example 1:
the embodiment provides a specific implementation mode of a preparation method of novel blue-green fluorescent powder, wherein the novel blue-green fluorescent material is inorganic submicron powder formed by polymerizing monomers to form polymers and then pyrolyzing the polymers, and the preparation method comprises the following steps:
dispersing polymer monomers into an organic solvent to form a uniform solution, carrying out hydrolytic polymerization under the stirring condition, and then transferring into a heating furnace;
step two, slowly heating the solution in a reducing atmosphere, preserving the temperature for a period of time in a low temperature area, evaporating the solvent and generating a crosslinking reaction between polymers;
and thirdly, continuously increasing the temperature in a reducing atmosphere to enable the polymer to undergo an inorganic decomposition reaction, and naturally cooling to obtain target powder.
Further, the polymer monomer in the first step is a silane structure substituted by two or three chlorine atoms
Or->Wherein R is 1 ，R 2 ，R 3 Is hydrogen atom or alkyl group, and the alkyl group comprises methyl, ethyl, propyl and isopropyl.
Further, in the first step, the solution is any one or more of polymer monomers mixed and dispersed in an organic solvent, and the organic solvent is common organic solvents such as ethanol, n-heptane, acetone and the like.
Further, in the second step, the reducing atmosphere is ammonia or hydrogen.
Further, the slow heating in the second step means 0.5-2 ℃/min.
Further, the low temperature condition in the second step is 150-300 ℃.
Further, the low-temperature heat preservation time in the second step is 0.5-2 h.
Further, the temperature range of the continuous rise in the third step is 400-1000 ℃.
Further, the high-temperature heat preservation time in the third step is 1-4 h.
Example 2
Dispersing 20% dichlorodimethylsilane and 20% dichloromethylsilane into ethanol to form a uniform solution, stirring for 30min, and performing polymerization reaction to obtain a solution with certain viscosity. Transferring the solution into a heating furnace, heating the solution at a heating rate of 1 ℃/min under an ammonia gas atmosphere, preserving the temperature for 1h at 200 ℃, evaporating the solvent in the solution, and performing a crosslinking reaction between polymers to form fluffy powder. Continuously increasing the temperature to 600 ℃ and preserving the heat for 2 hours, carrying out inorganic pyrolysis reaction on the polymer, and naturally cooling to obtain the target fluorescent powder.
As shown in FIG. 1, the obtained target fluorescent powder has the shape of nano-scale spherical particles, and the particle size distribution of the particles is relatively uniform.
As shown in fig. 2, the obtained target fluorescent powder fluorescence excitation and emission spectrum, the powder emission spectrum showed blue-green light, the maximum excitation wavelength was 365nm, and the maximum emission wavelength was 475nm.
Example 3
Dispersing 20% dichlorodimethylsilane and 20% dichloromethylsilane into ethanol to form a uniform solution, stirring for 30min, and performing polymerization reaction to obtain a solution with certain viscosity. Transferring the solution into a heating furnace, heating the solution at a heating rate of 1 ℃/min under an ammonia gas atmosphere, preserving the temperature for 1h at 200 ℃, evaporating the solvent in the solution, and performing a crosslinking reaction between polymers to form fluffy powder. Continuously increasing the temperature to 600 ℃ and preserving the heat for 1h, carrying out inorganic pyrolysis reaction on the polymer, and naturally cooling to obtain the target fluorescent powder.
As shown in fig. 3, the obtained target fluorescent powder fluorescence excitation and emission spectrum, the powder emission spectrum showed blue-green light, the maximum excitation wavelength was 365nm, and the maximum emission wavelength was 475nm.
Example 4
Dispersing 20% dichlorodimethylsilane and 20% dichloromethylsilane into ethanol to form a uniform solution, stirring for 30min, and performing polymerization reaction to obtain a solution with certain viscosity. Transferring the solution into a heating furnace, heating the solution at a heating rate of 1 ℃/min under an ammonia gas atmosphere, preserving the temperature for 1h at 200 ℃, evaporating the solvent in the solution, and performing a crosslinking reaction between polymers to form fluffy powder. Continuously increasing the temperature to 600 ℃ and preserving the heat for 4 hours, carrying out inorganic pyrolysis reaction on the polymer, and naturally cooling to obtain the target fluorescent powder.
As shown in fig. 4, the obtained target fluorescent powder fluorescence excitation and emission spectrum, the powder emission spectrum showed blue-green light, the maximum excitation wavelength was 365nm, and the maximum emission wavelength was 475nm.
As is clear from examples 2,3 and 4, the holding time has no influence on the maximum excitation and emission wavelength of the obtained fluorescent powder, but has a great influence on the fluorescence intensity, the optimal holding time is 2 hours, and the holding time is too long or too short, so that the fluorescence intensity of the material is reduced.
Example 5
Dispersing 20% of trichlorosilane and 20% of trichloromethylsilane into ethanol to form a uniform solution, stirring for 30min, and carrying out polymerization reaction to obtain a solution with certain viscosity. Transferring the solution into a heating furnace, heating the solution at a heating rate of 1 ℃/min under an ammonia gas atmosphere, preserving the temperature for 1h at 200 ℃, evaporating the solvent in the solution, performing a crosslinking reaction between polymers to form fluffy powder, continuously increasing the temperature to 400 ℃, preserving the temperature for 2h, performing an inorganic pyrolysis reaction on the polymers, and naturally cooling to obtain the target fluorescent powder.
As shown in FIG. 5, the obtained target fluorescent powder has micron-sized particles, the particle size distribution is relatively uniform, and the particles are agglomerated.
As shown in fig. 6, the obtained target fluorescent powder fluorescence excitation and emission spectrum, the powder emission spectrum showed blue-green light, the maximum excitation wavelength was 345nm, and the maximum emission wavelength was 440nm.
Example 6
Dispersing 20% of trichlorosilane and 20% of trichloromethylsilane into ethanol to form a uniform solution, stirring for 30min, and carrying out polymerization reaction to obtain a solution with certain viscosity. Transferring the solution into a heating furnace, heating the solution at a heating rate of 1 ℃/min under an ammonia gas atmosphere, preserving the temperature for 1h at 200 ℃, evaporating the solvent in the solution, and performing a crosslinking reaction between polymers to form fluffy powder. Continuously increasing the temperature to 800 ℃ and preserving heat for 2 hours, carrying out inorganic pyrolysis reaction on the polymer, and naturally cooling to obtain the target fluorescent powder.
As shown in fig. 7, the morphology of the obtained target fluorescent powder is nano-scale sphere particles, the particle size distribution is relatively uniform, but agglomeration occurs among the particles.
As shown in fig. 8, the obtained target phosphor fluorescence excitation and emission spectrum, the powder emission spectrum showed blue-green light, and the maximum emission wavelength was 460nm.
Example 7
Dispersing 20% of trichlorosilane and 20% of trichloromethylsilane into ethanol to form a uniform solution, stirring for 30min, and carrying out polymerization reaction to obtain a solution with certain viscosity. Transferring the solution into a heating furnace, heating the solution at a heating rate of 1 ℃/min under an ammonia gas atmosphere, preserving the temperature for 1h at 200 ℃, evaporating the solvent in the solution, and performing a crosslinking reaction between polymers to form fluffy powder. Continuously increasing the temperature to 1000 ℃ and preserving heat for 2 hours, carrying out inorganic pyrolysis reaction on the polymer, and naturally cooling to obtain the target fluorescent powder.
As shown in fig. 9, the obtained target phosphor has irregular particle morphology, large particle size, micron-sized particle size, and uneven particle distribution.
As shown in fig. 10, the obtained target fluorescent powder fluorescence excitation and emission spectrum, the powder emission spectrum showed blue-green light, the maximum excitation wavelength was 350nm, and the maximum emission wavelength was 450nm.
As is clear from examples 2,5,6 and 7, the heating temperature has a great influence on the morphology and fluorescence spectrum of the powder, the optimal temperature is 600 ℃, the powder particles are grown and agglomerated due to the too low or too high temperature, the intensity of the fluorescence spectrum is reduced, and the maximum emission wavelength moves like the blue light direction.
Example 8
Dispersing 20% of dichlorodimethylsilane and 20% of dichloromethylsilane into n-heptane to form a uniform solution, stirring for 30min, and carrying out polymerization reaction to obtain a solution with certain viscosity. Transferring the solution into a heating furnace, heating the solution at a heating rate of 1 ℃/min under an ammonia gas atmosphere, preserving the temperature for 1h at 200 ℃, evaporating the solvent in the solution, and performing a crosslinking reaction between polymers to form fluffy powder. Continuously increasing the temperature to 600 ℃ and preserving the heat for 2 hours, carrying out inorganic pyrolysis reaction on the polymer, and naturally cooling to obtain the target fluorescent powder.
The obtained target fluorescent powder has the shape of nano-scale sphere particles, and the particle size distribution of the particles is relatively uniform. The powder emission spectrum shows blue-green light, the maximum excitation wavelength is 365nm, and the maximum emission wavelength is 475nm.
Example 9
Dispersing 20% dichlorodimethylsilane and 20% dichloromethylsilane into ethanol to form a uniform solution, stirring for 30min, and performing polymerization reaction to obtain a solution with certain viscosity. Transferring the solution into a heating furnace, heating the solution at a heating rate of 1 ℃/min under the hydrogen atmosphere, preserving the temperature for 1h at 200 ℃, evaporating the solvent in the solution, and performing a crosslinking reaction between polymers to form fluffy powder. Continuously increasing the temperature to 600 ℃ and preserving the heat for 2 hours, carrying out inorganic pyrolysis reaction on the polymer, and naturally cooling to obtain the target fluorescent powder.
The obtained target fluorescent powder has the shape of nano-scale sphere particles, and the particle size distribution of the particles is relatively uniform. The obtained powder emission spectrum shows blue-green light, the maximum excitation wavelength is 365nm, and the maximum emission wavelength is 475nm.
Example 10
Dispersing 20% dichlorodimethylsilane and 20% dichloromethylsilane into ethanol to form a uniform solution, stirring for 30min, and performing polymerization reaction to obtain a solution with certain viscosity. Transferring the solution into a heating furnace, heating the solution at a heating rate of 1 ℃/min under an ammonia gas atmosphere, preserving the temperature for 1h at 300 ℃, evaporating the solvent in the solution, and performing a crosslinking reaction between polymers to form fluffy powder. Continuously increasing the temperature to 600 ℃ and preserving the heat for 2 hours, carrying out inorganic pyrolysis reaction on the polymer, and naturally cooling to obtain the target fluorescent powder.
The obtained target fluorescent powder has the shape of nano-scale sphere particles, and the particle size distribution of the particles is relatively uniform. Powder fluorescence excitation and emission spectrum, powder emission spectrum shows blue-green light, and the maximum excitation wavelength is 365nm, and the maximum emission wavelength is 475nm.
Example 11:
the embodiment provides a specific implementation mode of the novel blue-green fluorescent powder preparation method, which comprises the following steps: in examples 1 to 10, a novel blue-green fluorescent material obtained by the preparation method of the blue-green fluorescent powder and application thereof are provided.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (6)
1. The preparation method of the blue-green fluorescent material is characterized in that the blue-green fluorescent material is inorganic submicron powder formed by polymerizing monomers to form polymers and then pyrolyzing the polymers, and the preparation method comprises the following steps:
dispersing polymer monomers into an organic solvent to form a uniform solution, carrying out hydrolytic polymerization under the stirring condition, and then transferring into a heating furnace;
step two, slowly heating the solution in a reducing atmosphere, preserving the temperature for a period of time in a low temperature area, evaporating the solvent and generating a crosslinking reaction between polymers;
step three, continuously increasing the temperature in a reducing atmosphere to enable the polymer to undergo an inorganic decomposition reaction, and naturally cooling to obtain target powder;
the temperature range of the continuous rise in the third step is 400-800 ℃;
the high-temperature heat preservation time in the third step is 1h-4h;
the polymer monomer in the first step is a silane structure with two or three chlorine atoms substitutedOr alternativelyWherein R is 1 ，R 2 ，R 3 Is hydrogen atom or alkyl group, and the alkyl group is methyl, ethyl, propyl or isopropyl;
the low temperature condition in the second step is 150-300 ℃.
2. The method for preparing a blue-green fluorescent material according to claim 1, wherein: in the first step, the solution is any one or more of polymer monomers, which are mixed and dispersed in an organic solvent, wherein the organic solvent is ethanol, n-heptane or acetone.
3. The method for preparing a blue-green fluorescent material according to claim 1, wherein: and in the second step, the reducing atmosphere is ammonia or hydrogen.
4. The method for preparing a blue-green fluorescent material according to claim 1, wherein: the slow heating in the second step means 0.5-2 ℃/min.
5. The method for preparing a blue-green fluorescent material according to claim 1, wherein: the low-temperature heat preservation time in the second step is 0.5h-2h.
6. Use of a blue-green fluorescent material obtainable by a process according to any one of claims 1 to 5 in the field of illumination/display.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6018002A (en) * | 1998-02-06 | 2000-01-25 | Dow Corning Corporation | Photoluminescent material from hydrogen silsesquioxane resin |
| CN1934216A (en) * | 2004-03-25 | 2007-03-21 | 株式会社丰田中央研究所 | Luminescent material and method for producing same |
| CN103666463A (en) * | 2012-09-10 | 2014-03-26 | 中国石油化工股份有限公司 | Fluorescent material, and preparation method and application thereof |
| JP5700659B2 (en) * | 2011-03-29 | 2015-04-15 | 公立大学法人大阪府立大学 | Phosphor and method for producing the same |
-
2022
- 2022-11-18 CN CN202211444249.2A patent/CN115746838B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6018002A (en) * | 1998-02-06 | 2000-01-25 | Dow Corning Corporation | Photoluminescent material from hydrogen silsesquioxane resin |
| CN1934216A (en) * | 2004-03-25 | 2007-03-21 | 株式会社丰田中央研究所 | Luminescent material and method for producing same |
| JP5700659B2 (en) * | 2011-03-29 | 2015-04-15 | 公立大学法人大阪府立大学 | Phosphor and method for producing the same |
| CN103666463A (en) * | 2012-09-10 | 2014-03-26 | 中国石油化工股份有限公司 | Fluorescent material, and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| Eric J. Henderson et al..Influence of HSiO1.5 Sol-Gel Polymer Structure and Composition on the Size and Luminescent Properties of Silicon Nanocrystals.《Chem. Mater.》.2009,第21卷第5426-5434页. * |
| Influence of HSiO1.5 Sol-Gel Polymer Structure and Composition on the Size and Luminescent Properties of Silicon Nanocrystals;Eric J. Henderson et al.;《Chem. Mater.》;第21卷;第5426-5434页 * |
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