CN116396753B - Single-doped nitrogen oxide cold white light fluorescent powder - Google Patents
Single-doped nitrogen oxide cold white light fluorescent powder Download PDFInfo
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- CN116396753B CN116396753B CN202310482710.1A CN202310482710A CN116396753B CN 116396753 B CN116396753 B CN 116396753B CN 202310482710 A CN202310482710 A CN 202310482710A CN 116396753 B CN116396753 B CN 116396753B
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000000843 powder Substances 0.000 title claims abstract description 36
- 230000005284 excitation Effects 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000001228 spectrum Methods 0.000 claims abstract description 3
- 238000005245 sintering Methods 0.000 claims description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052721 tungsten Inorganic materials 0.000 claims description 7
- 239000010937 tungsten Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000007790 solid phase Substances 0.000 abstract description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 8
- 238000000295 emission spectrum Methods 0.000 description 7
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 6
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 6
- 238000000695 excitation spectrum Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- 238000005286 illumination Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 description 1
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002284 excitation--emission spectrum Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- -1 nitride silicate Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000009103 reabsorption Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/77747—Silicon Nitrides or Silicon Oxynitrides
-
- 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
Abstract
The invention discloses a single doped nitrogen oxide cold white light fluorescent powder, which has a chemical formula of La 4‑xSr4Si7N10O9:xCe3+, x is more than 0 and less than or equal to 4. In the invention, the excitation wavelength of the series of fluorescent powder is 200-400 nm, the cold white fluorescent powder with 400-600 nm range is emitted, and the half-peak width of the spectrum is about 110 nm. The series of fluorescent powder has wide emission wavelength range, simple process of the adopted high-temperature solid phase preparation method, easy operation and control, good repeatability, high safety and short preparation time, and is suitable for industrialized mass production and popularization and application.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and particularly relates to a single-doped nitrogen oxide cold white fluorescent powder.
Background
As a new generation illumination light source, the white light LED has high efficiency, energy conservation, small volume, long service life and excellent performance, so that the white light LED has very wide research and development and commercial prospect. The fluorescent powder has stable physical and chemical properties, can be well matched with the output wavelength of the current commercial LED chip, has a wider emission band in the visible light range, and has great application potential in the field of lighting devices. Firstly, the near ultraviolet chip is used for excitation, so that the color difference problem caused by different color ratios and different thicknesses of fluorescent powder coatings is not needed to be considered; secondly, the single-matrix white light fluorescent powder has no problem of color reabsorption and has high color rendering index. Therefore, the single-matrix white light LED fluorescent powder is the most potential fluorescent powder in the future illumination field and is the first choice as a fourth-generation illumination light source.
The nitrogen (oxygen) silicate has good chemical temperature property and excellent fluorescence property. In particular, phosphors based on nitrogen (oxy) silicates have received increasing attention in the development of phosphors for white light LEDs. The prepared product has excellent performance, and the rare earth luminescent material with high brightness is easy to obtain, so that the nitrogen (oxygen) silicate is a luminescent matrix with research potential. Meanwhile, in recent years, the research of the fluorescent powder of the (oxy) nitride silicate is greatly advanced, but the fluorescent powder is still in the stage of research and development. Therefore, the development of the single-doped nitrogen oxide cold white fluorescent powder has important significance.
Disclosure of Invention
The invention aims to provide a single-doped nitrogen oxide cold white fluorescent powder and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
The chemical formula La 4-xSr4Si7N10O9: xCe3+ for the fluorescent powder solves the technical problems, wherein x is more than 0 and less than or equal to 4. In addition, since N and O can be substituted for each other to some extent, the nitrogen-oxygen ratio under the La 4-xSr4Si7N10O9: xCe3+ structure can be expanded to some extent, that is, the nitrogen-oxygen ratio is not limited to the chemical formula, and up-and-down fluctuation of the nitrogen-oxygen ratio is allowed within a certain range of maintaining the structural framework, specifically based on the structure characterized by XRD.
The invention relates to a preparation method of single-doped nitrogen oxide cold white light fluorescent powder, which is synthesized by adopting a high-temperature solid phase method, and comprises the following specific steps:
(a) According to the molecular formula La 4-xSr4Si7N10O9: xCe3+, wherein x is more than 0 and less than or equal to 4; accurately weighing raw materials LaN (99.0%), la 2O3（99.9%）、Sr3N2 (99.0%), srO (99.9%), srCO 3（99.9%）、Si3N4（99.9%）、SiO2（99.99%）、CeCl3 (99.9%), ceN (99.9%) or CeO 2 (99.9%) according to stoichiometric ratio, fully mixing the raw materials in an agate mortar, grinding the raw materials to 20-80 min, putting the ground mixture into a tungsten crucible, sealing the tungsten crucible by a sealing film, and finishing the operations in a glove box;
(b) Transferring the tungsten crucible with the sample into a high-temperature tube furnace, performing a sintering process under a reducing atmosphere of N 2/H2 (9:1), heating at a speed of 5-10 ℃/min, sintering at 1300-1650 ℃ for 3-30 hours, and cooling to room temperature to obtain the sample;
(c) And cooling the obtained sintered body to room temperature, and fully grinding to obtain the single-doped nitrogen oxide cold white light fluorescent powder.
In the preparation method, in the chemical formula La 4-xSr4Si7N10O9: xCe3+, x is preferably more than or equal to 0.005 and less than or equal to 0.02.
In the above preparation method, a raw material combination of La 2O3（99.9%）、Sr3N2（99.0%）、Si3N4 (99.9%) and CeN (99.9%) is preferable.
In the above preparation method, the grinding time is preferably 40 min.
In the above preparation method, sintering is preferably performed at 1500 ℃ for 8 hours, and the temperature rising rate of sintering is 10 ℃/min.
In the invention, ce 3+ is doped in La 4Sr4Si7N10O9 matrix material, the excitation wavelength is 300-400 nm, and cold white light in the range of 400-600 nm is emitted. The excitation band of the fluorescent powder can be well matched with the near ultraviolet chip. The series of fluorescent powder has wide emission wavelength range, the adopted high-temperature solid phase preparation method has simple process, easy operation and control, good repeatability, high safety and short preparation time, and is suitable for industrialized mass production and popularization and application.
Drawings
FIG. 1 is an X-ray diffraction pattern of a single doped oxynitride cool white phosphor prepared in examples 1-6.
FIG. 2 is a series of concentration emission spectra of a single doped oxynitride cool white phosphor prepared in examples 1-6.
FIG. 3 is a series of concentration excitation spectra of a single doped oxynitride cool white phosphor prepared in examples 1-6.
FIG. 4 is a graph showing excitation and emission spectra of La 3.99Sr4Si7N10O9: 0.01Ce3+ prepared in example 3.
FIG. 5 is a graph of quantum efficiency of La 3.99Sr4Si7N10O9: 0.01Ce3+ prepared in example 3.
FIG. 6 is a plot of fluorescence lifetime decay for La 3.99Sr4Si7N10O9: 0.01Ce3+ prepared in example 3 under 360 nm excitation.
FIG. 7 is a graph of the temperature change emission spectrum of La 3.99Sr4Si7N10O9: 0.01Ce3+ prepared in example 3 under excitation of 360 nm.
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
According to the stoichiometric ratio of La 3.995Sr4Si7N10O9: 0.005Ce3+, weighing La2O3 1.4285 g、Sr3N20.8513 g、Si3N4 0.7185 g、CeN 0.0017g,, fully mixing and grinding uniformly in an agate mortar, about 40 min, putting the ground powder into a tungsten crucible for packaging, then putting the tungsten crucible into a high-temperature tube furnace, and performing the sintering process under the reducing atmosphere of N 2/H2 (9:1), wherein the sintering process is as follows: 10. heating to 1500 ℃ at the heating rate of DEG C/min, sintering at constant temperature for 8 hours, naturally cooling, cooling to room temperature, and fully grinding to obtain the single-doped nitrogen oxide cold white light fluorescent powder La 3.995Sr4Si7N10O9: 0.005Ce3+.
Example 2
Other steps of weighing La2O3 1.4277 g、Sr3N20.8513 g、Si3N4 0.7185 g、CeN 0.0025g, are the same as in example 1 according to the stoichiometric ratio of La 3.9925Sr4Si7N10O9: 0.0075Ce3+, and a single doped nitrogen oxide cool white light fluorescent powder La 3.9925Sr4Si7N10O9: 0.0075Ce3+ is obtained.
Example 3
Other steps of weighing La2O3 1.4268 g、Sr3N20.8513 g、Si3N4 0.7185 g、CeN 0.0034g, are the same as in example 1 according to the stoichiometric ratio of La 3.99Sr4Si7N10O9: 0.01Ce3+, and a single doped nitrogen oxide cool white light fluorescent powder La 3.99Sr4Si7N10O9: 0.01Ce3+ is obtained.
Example 4
Other steps of weighing La2O3 1.4259 g、Sr3N20.8513 g、Si3N4 0.7185 g、CeN 0.0042g, are the same as in example 1 according to the stoichiometric ratio of La 3.9875Sr4Si7N10O9: 0.0125Ce3+, and a single doped nitrogen oxide cool white light fluorescent powder La 3.9875Sr4Si7N10O9: 0.0125Ce3+ is obtained.
Example 5
Other steps of weighing La2O3 1.4250 g、Sr3N20.8513 g、Si3N4 0.7185 g、CeN 0.0051g, are the same as in example 1 according to the stoichiometric ratio of La 3.985Sr4Si7N10O9: 0.015Ce3+, and a single doped nitrogen oxide cool white light fluorescent powder La 3.985Sr4Si7N10O9: 0.015Ce3+ is obtained.
Example 6
Other steps of weighing La2O3 1.4233 g、Sr3N20.8513 g、Si3N4 0.7185 g、CeN 0.0068g, are the same as in example 1 according to the stoichiometric ratio of La 3.98Sr4Si7N10O9: 0.02Ce3+, and a single doped nitrogen oxide cool white light fluorescent powder La 3.98Sr4Si7N10O9: 0.02Ce3+ is obtained.
XRD analysis was performed on the series of single doped oxynitride cool white phosphors obtained in examples 1-6, see FIG. 1. The resulting material was single phase and all diffraction peaks matched to standard cards, indicating that the prepared phosphor was pure phase and Ce 3+ successfully entered the host lattice with the crystal structure maintained unchanged.
The luminescence performance test, namely the excitation emission spectrum, of the series of single-doped nitrogen oxide cold white light fluorescent powders obtained in examples 2 to 8 is carried out by adopting a fluorescence spectrometer, and is shown in fig. 2 and 3. The excitation spectrum shows that the excitation range of the compound is 200-400 nm, and the main peak is 360 nm; the emission spectrum shows that under the excitation of 360 nm wavelengths, the emission spectrum range is 400-600 nm, the main emission peak is red-shifted from 436 nm to 462 nm along with the increase of the doping concentration of Ce 3+, and the fluorescence intensity is maximum when the doping concentration of Ce 3+ is x=0.01.
Excitation and emission spectra were measured for the phosphor prepared in example 3, see fig. 4. The excitation spectrum shows that the fluorescent powder can effectively absorb near ultraviolet light of 200-400 nm so as to be matched with a near ultraviolet LED chip; the light emits 400-600 nm orange light under the excitation of near ultraviolet 360 nm, the peak is positioned at 440 nm, the emission is from the 5 d-4 f transition of Ce 3+, the half-peak width of the spectrum is about 110 nm, and the light belongs to broad-spectrum cold white light emission.
The La 3.99Sr4Si7N10O9: 0.01Ce3+ phosphor prepared in example 3 has an internal quantum efficiency of La 3.99Sr4Si7N10O9: 0.01Ce3+ of 7.10% under excitation by 360 nm wavelength near uv light, see fig. 5.
The average fluorescence lifetime of La 3.99Sr4Si7N10O9: 0.01Ce3+ of La 3.99Sr4Si7N10O9: 0.01Ce3+ fluorescent powder prepared in example 3 under the excitation of ultraviolet light with the wavelength of 360 nm is 4.825 nanoseconds, and lifetime curve shows multi-exponential fit, which indicates that Ce 3+ occupies a plurality of crystallographic lattice sites, see FIG. 6.
For the emission spectra of La 3.99Sr4Si7N10O9: 0.01Ce3+ obtained in example 3 at different temperatures under excitation of 360: 360 nm, see FIG. 6. As the temperature is gradually increased from 298K to 498K, the relative intensity of la 3.99Sr4Si7N10O9: 0.01Ce3+ phosphor gradually decreases. The main peak position hardly drifts, which indicates that the color drift resistance is good at high temperature.
Since La < 3+ > and Ce < 3+ > are equivalent and have similar atomic radii, la and Ce contained in a plurality of compounds are of isomorphic structures, and in the text, only samples with smaller doping concentration are selected in the scope, the protection scope is not limited to the embodiment, la 4- xSr4Si7N10O9: xCe3+, wherein 0 < x is less than or equal to 4, and the scope can be realized.
Claims (5)
1. A single doped nitrogen oxide cold white fluorescent powder is characterized in that: the chemical formula is La 4-xSr4Si7N10O9:xCe3+, x is more than 0 and less than or equal to 0.02.
2. The single doped oxynitride cool white phosphor of claim 1, wherein: excitation wavelength is 200-400 nm, emission wavelength is 400-600 nm, spectrum half-peak width is 110 nm, and the light belongs to cold white light emission.
3. The method for preparing the single-doped nitrogen oxide cold white fluorescent powder according to claim 1, which is characterized in that: the method adopts a high-temperature solid phase method and comprises the following specific steps:
(a) According to the molecular formula La 4-xSr4Si7N10O9: xCe3+, wherein x is more than 0 and less than or equal to 0.02; accurately weighing LaN with the purity of 99.0% or La 2O3 with the purity of 99.9%, sr 3N2 with the purity of 99.0% or SrO with the purity of 99.9% or SrCO 3 with the purity of 99.9%, si 3N4 with the purity of 99.9%, ceCl 3 with the purity of 99.9% or CeO 2 with the purity of 99.9% according to the stoichiometric ratio, fully mixing and grinding the raw materials in an agate mortar to 20-80 min, putting the ground mixture into a tungsten crucible, sealing by a sealing film, and finishing the above operations in a glove box;
(b) Transferring the tungsten crucible with the sample into a high-temperature tube furnace, sintering in a reducing atmosphere of N 2/H2 with the volume ratio of 9:1, heating at a speed of 5-10 ℃/min, sintering at 1300-1650 ℃ for 3-30 hours, and cooling to room temperature to obtain the sample;
(c) And cooling the obtained sintered body to room temperature, and fully grinding to obtain the single-doped nitrogen oxide cold white light fluorescent powder.
4. The method for preparing the single-doped nitrogen oxide cold white fluorescent powder according to claim 3, which is characterized in that: la 2O3 with purity of 99.0%, sr 3N2 with purity of 99.0%, si 3N4 with purity of 99.9% and CeN with purity of 99.9%.
5. The method for preparing the single-doped nitrogen oxide cold white fluorescent powder according to claim 3, which is characterized in that: the grinding duration is 40 min; sintering at 1500 deg.c for 8 hr at 10 deg.c/min.
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