CN115678548B - Nano Sialon nitride green fluorescent material and preparation method and application thereof - Google Patents
Nano Sialon nitride green fluorescent material and preparation method and application thereof Download PDFInfo
- Publication number
- CN115678548B CN115678548B CN202211344798.2A CN202211344798A CN115678548B CN 115678548 B CN115678548 B CN 115678548B CN 202211344798 A CN202211344798 A CN 202211344798A CN 115678548 B CN115678548 B CN 115678548B
- Authority
- CN
- China
- Prior art keywords
- nano
- sialon
- green fluorescent
- fluorescent material
- nitride green
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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 nanometer Sialon nitride green fluorescent material, a preparation method and application thereof, wherein the molecular general formula of the nanometer Sialon nitride green fluorescent material is Eu x Si 6‑z Al z O z N 8‑z Eu element enters a large pore canal in the z-axis direction and is used as a luminescence center and an activator; in the molecular general formula, x represents the doping amount of the light-emitting element, z represents the number of Al-O bonds substituted for Si-N bonds, and 0<z is less than or equal to 4.2. Can pass through at 10 5 The heating time of the pulse is regulated in the temperature rise and fall rate of the temperature/s to realize that the particle size of the nano Sialon fluorescent powder is 1-3 nm, the emission peak wavelength is 516nm, the half-peak width is 36nm, and the nano Sialon fluorescent powder has good application prospect in the field of ink-jet printing.
Description
Technical Field
The invention relates to the technical field of fluorescent materials, in particular to a nano Sialon nitride green fluorescent material, a preparation method and application thereof.
Background
The high temperature is one of the most basic and most common energy source forms for driving chemical reaction to occur, is also one of core regulation and control parameters in the material preparation process, and meanwhile, the state of a substance and the dynamic transition behavior of the substance are closely related to the temperature of the environment, so that the development of modern science and technology is greatly promoted to develop and apply new materials while the upper limit of the temperature is continuously improved. In the high temperature heat treatment process, factors affecting the final atomic structure of the material can be attributed to both thermodynamic and kinetic aspects, the thermodynamics determining the material with the lowest free energy and the most stable atomic arrangement, while the kinetics dominate the path and time to achieve a thermodynamically stable state, so that a localized free energy steady state product can be obtained by kinetic control. The preparation of nitride fluorescent powder belongs to the research category of synthetic chemistry, and the preparation process involves the breaking of old chemical bonds and the generation of new chemical bonds, the rearrangement of heat activated atoms and the doping of luminescence centers in a high-temperature environment. In the balanced stable high-temperature environment of the traditional synthesis equipment such as a tube furnace, a muffle furnace and a pneumatic furnace, which is heated slowly, kept warm for a long time and then cooled slowly, the obtained steady-state products are all thermodynamically dominant, while the obtained metastable products are kinetically dominant in the unbalanced high-temperature environment formed by the modes of rapid heating and cooling and ultra-short time heat preservation, and are characterized by ultra-small size, metastable phase structure and the like.
The nano Sialon nitride fluorescent material prepared by the patent has the advantages of beta-Si 3 N 4 The same phase structure is formed under conditions similar to those of silicon nitride, except that a small portion of the Al-O bonds replace Si-N bonds. alfa-Si 3 N 4 Is 3.183g/cm 3 beta-Si 3 N 4 Has a density of 3.2g/cm 3 Higher temperatures are required for synthesis, but both synthesis temperatures are below 1600 ℃. The high temperature environment of 1900-2000 ℃ required for Sialon nitride fluorescent material synthesis is therefore for successful introduction of luminescence centers, according to the literature reported so far on Sialon nitride fluorescent materials as follows:
1) Non-patent document Characterization and propertie/of green-refining Sialon Eu 2+ The beta-Sialon Eu synthesized by reacting powder pho/phor/for white light-emitting diode/-, hiro/aki, T., xie, R.—J., kimoto, K..Appl. Phy/. Lett.86,211905 (2004) under nitrogen at 1MPa and 1900 ℃ for 8 hours is disclosed 2+ A fluorescent material with a particle length of 4 microns and a diameter of 0.5 microns;
2) Non-patent document Lumine/cent property/of Sialon Eu 2+ Green pho/phor// ynthe/ized by ga/pre// ided/intervening Ryu, J.H., park, Y.G., won, H.S., suzuki, H., kim, S.H., yoon, C., J.Ceram.Soc.Jpn.116,389-394 (2008) disclose a reaction under nitrogen at 2000℃under 0.92MPabeta-Sialon Eu synthesized for 2h 2+ Fluorescent material with particle length of 3-5 microns and diameter of 0.5-1 micron;
3) Non-patent document Achieving high quantum efficiency narrow-band Sialon Eu 2+ pho/phor/for high-brightne//LCD backlight/by reducing the Eu 3+ The beta-Sialon Eu synthesized by reacting for 2 hours under nitrogen conditions of 1MPa, 1900 ℃ and 1MPa is disclosed in the following formula (Li, S.X., wang, L., tang, D.M., cho.Y., J., liu, X.J., zhou, X.T., lu, L., zhang, L., takeda, T., hiro/aki, N., xie, R. -J., chem.Mater.30,495-505 (2018)) 2+ A fluorescent material having a particle length of about 10 microns;
in summary, particle size reduction and successful incorporation of luminescent centers are a fundamental pair of contradictions in the preparation of nano Sialon nitride fluorescent materials. The successful doping of the luminescence center requires a long-time high-temperature environment, and the long-time high-temperature environment easily causes irreversible curing and sintering of the nano fluorescent particles, and finally grows into micron-sized particles after nucleation and growth, so that the nano-sized particles are difficult to obtain.
Disclosure of Invention
Therefore, the invention aims to provide a nano Sialon nitride green fluorescent material and a rapid preparation method thereof, so as to fill the blank of the Sialon nitride green fluorescent material in nano scale and break through the limitation of the Sialon nitride green fluorescent material in practical application.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
a nanometer Sialon nitride green fluorescent material with a molecular general formula of Eu x Si 6-z Al z O z N 8-z Wherein x represents the doping amount of the light-emitting element, z represents the number of Al-O bonds substituted for Si-N bonds, and 0<z is less than or equal to 4.2; wherein Eu element enters into a large pore canal in the z-axis direction and is used as a luminescence center and an activator.
Further, the crystals of the nano Sialon nitride green fluorescent material are generated in a manner of containing a mixture of other crystalline or non-crystalline compounds, and the mass content of the crystals of the nano Sialon nitride green fluorescent material in the mixture is not less than 40%.
Furthermore, the nanometer Sialon nitride green fluorescent material emits fluorescence with peak value of wavelength 510-560 nm under the excitation of ultraviolet or blue light source with wavelength 250-500 nm.
The invention also provides a preparation method of the nanometer Sialon nitride green fluorescent material, which comprises the following steps of 5 The temperature rise/fall rate is 1400-2200 ℃ in a high temperature field, and the pulse heating is performed within 3300 milliseconds.
Further, the preparation method of the nano Sialon nitride green fluorescent material specifically comprises the following steps:
1) Dispersing the precursor complex and dendritic mesoporous silica in anhydrous methanol, and then carrying out ultrasonic mixing and continuous vacuumizing treatment to promote complex particles to enter the aperture to obtain a mixed solution;
2) And (3) dripping the mixed solution on carbon cloth, installing the carbon cloth in a vacuum reaction cavity, respectively fixing two ends of the carbon cloth on a copper electrode, and triggering a carbothermic reduction reaction in a joule heating method under a nitrogen atmosphere to obtain the nano Sialon nitride green fluorescent material.
Further, the preparation method of the precursor complex in the step 1) includes:
a) Completely dissolving aluminum chloride hexahydrate and europium chloride hexahydrate in absolute methanol, adding urea, and continuously stirring at 60 ℃ and 400r/min until a clear and transparent solution is obtained;
b) And then placing the obtained stable clear solution in an oven for drying to obtain white precursor salt powder, taking out and grinding to obtain the precursor complex.
Further, the preparation method of the dendritic mesoporous silica in the step 1) comprises the following steps:
a) Adding TEA solution, sodium salicylate powder and CTAB powder into 25ml deionized water, and uniformly mixing;
b) After one hour of reaction at 80 ℃ and 800r/min, adding TEOS solution, and continuing the reaction for three hours under the same conditions;
c) And washing, drying and grinding the product, and roasting at 550 ℃ for three hours to obtain the dendritic mesoporous silica after sintering.
Further, in the step 2), 400 microliters of the mixed solution is dripped on a carbon cloth with the size of 2cm multiplied by 5 cm; the reaction voltage of carbothermic reaction is 30-50V, the current is 30-80A, the temperature is 1400-2200 ℃, and the reaction time is within 3300 milliseconds.
When the high-temperature pulse time is within 100 milliseconds at 30-50V, 30-80A and 1400-2200 ℃, the particle size of the prepared green fluorescent material is uniformly distributed within 10 nm;
when the high-temperature pulse time is 100-800 milliseconds at 30-50V, 30-80A and 1400-2200 ℃, the particle size of the prepared green fluorescent material is uniformly distributed at 10-50 nm, and the particles are spherical;
when the high-temperature pulse time is between 800 and 3300 milliseconds at the temperature of between 30 and 50V, between 30 and 80A and between 1400 and 2200 ℃, the particle size of the prepared green fluorescent material is evenly distributed between 50 and 100nm, and the particles are in a polygonal shape.
Preferably, the particle sizes of the precursor complex and the dendritic mesoporous silica in the step 1) are submicron or nanoscale; the vacuum pressure in the vacuumizing treatment is 0.098Mpa, and the vacuumizing time is 30min;
the nitrogen atmosphere in the step 2) is micro positive pressure, and the pressure value is 0.4 MPa-1 MPa;
the molar ratio of the aluminum chloride hexahydrate to the urea in the step a) is 6 to 12;
the dendritic mesoporous silica particles in the step C) have a size of 100-150 nm, a pore diameter of 13-15 nm and a specific surface area of 430-450 m 2/ g。
The nanometer Sialon nitride green fluorescent material is applied to the field of ink-jet printing. The nanometer Sialon nitride green fluorescent material is particle of 10nm or less obtained in pulse sintering at 30-50V, 30-80A, 1400-2200 deg.c and 100 ms, and has emission wavelength of 510-560 nm and half-peak width of 36nm under the excitation of 250-500 nm wavelength light source.
Compared with the prior art, the invention has the following beneficial effects:
1) The invention can prepare nanometer Sialon nitride green fluorescent materials with different particle diameters by regulating and controlling pulse heating time in a high temperature field formed under different current and voltage conditions, and can optimize the particle diameter and luminous performance of the nanometer Sialon nitride green fluorescent materials by optimizing a pretreatment process and sintering conditions to obtain the green luminescent materials which can be effectively excited by an ultraviolet light source, have emission wavelength peak values of 510-560 nm, half peak width of 36nm and particle diameters of 1-100 nm;
2) The ultra-rapid preparation method of the nano Sialon nitride green fluorescent material solves the contradiction between the mutual restriction of the miniaturization of the Sialon nitride green fluorescent material and the successful doping of the luminescence center in the high-temperature synthesis process, and has the advantages of low preparation energy consumption, simple raw material preparation and high sintering rate;
3) The nano Sialon nitride green fluorescent material has the advantages of simple process, easily available raw materials, low cost, effective excitation by an ultraviolet light source, narrow half-peak width of an emission spectrum, small particle size and the like, and can be used in the field of ink-jet printing. It is expected that the nano Sialon nitride green fluorescent material and the preparation method thereof can be widely applied, and greatly promote the development of the application field thereof.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a pore size analysis chart and a morphology chart of dendritic mesoporous silica;
FIG. 3 shows Al (CON) at various aluminum chloride hexahydrate-urea molar ratios 2 H 4 ) 6 Cl 3 :Eu 3+ XRD pattern, fourier transform infrared spectrum of the complex; (R6, R8, R10 and R12 in the figure correspond to each otherThe molar ratio of the aluminum chloride hexahydrate to the urea is 6, 8, 10 and 12, and the following is the same
FIG. 4 is a graph of the relationship between different current and voltage versus different temperatures for a vacuum Joule heating apparatus used in the preparation of nano Sialon nitride green fluorescent material according to the present invention;
FIG. 5 is a graph showing the morphology of a nano Sialon nitride green fluorescent material obtained by mixing a precursor obtained by mixing complexes with different aluminum chloride hexahydrate-urea molar ratios with mesoporous silica and pulsing at 30V,50A and 2000 ℃ for the same time;
FIG. 6 is an elemental analysis diagram of a nano Sialon nitride green fluorescent material obtained by mixing a precursor after mixing a complex of different aluminum chloride hexahydrate-urea molar ratios with mesoporous silica and pulsing at 30V,50A and 2000 ℃ for the same time; (the molar ratio of aluminum chloride hexahydrate to urea in the complex is 6, 8, 10 and 12 respectively from top to bottom)
FIG. 7 is a graph showing the morphology of a nano Sialon nitride green fluorescent material, a blank carbon carrier and a drop solution carbon carrier obtained by mixing a precursor obtained by mixing a complex with a molar ratio of aluminum chloride hexahydrate to urea of 10 with mesoporous silica under the conditions of 30V,50A and 2000 ℃ for different pulse times;
FIG. 8 is a graph showing the grain size growth curve of a nano Sialon nitride green fluorescent material obtained by mixing a precursor obtained by mixing a complex with a molar ratio of 10 aluminum chloride hexahydrate to urea with mesoporous silica under the conditions of 30V,50A and 2000 ℃ for different pulse times;
FIG. 9 is an elemental analysis diagram of a nano Sialon nitride green fluorescent material obtained by pulsing different times at 30V,50A, and 2000 ℃ using a precursor after mixing a complex with a molar ratio of aluminum chloride hexahydrate to urea of 10 with mesoporous silica; (the time from left to right in the figure is 0.38/, 0.75/, 1.24/, 1.97/, 3.3/, 4.95 /)
FIG. 10 is a transmission electron microscope morphology diagram and a high resolution diagram of a nanometer Sialon nitride green fluorescent material obtained by mixing a precursor after mixing a complex with a molar ratio of aluminum chloride hexahydrate to urea of 10 with mesoporous silica and pulse the precursor within 100 milliseconds at 30V,50A and 2000 ℃;
FIG. 11 is an electron diffraction diagram of SAED selective areas of a nano Sialon nitride green fluorescent material obtained at 30V,50A, and 2000 ℃ using a precursor after mixing a complex with a molar ratio of aluminum chloride hexahydrate to urea of 10 with mesoporous silica;
FIG. 12 is an excitation emission spectrum of a nano Sialon nitride green fluorescent material obtained at 30V,50A, and 2000 ℃ using a precursor after mixing a complex having a molar ratio of aluminum chloride hexahydrate to urea of 10 with mesoporous silica; wherein the half-width is 36nm;
FIG. 13 is a schematic diagram of a nano Sialon nitride green fluorescent material for ink-jet printing prepared by mixing a precursor of a complex with a molar ratio of aluminum chloride hexahydrate to urea of 10 and mesoporous silica and pulsing the precursor at 30V,50A and 2000 ℃ for less than 100 milliseconds.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The green fluorescent material is nano Sialon nitride, and only part of Si-N bonds are replaced by Al-O bonds. Wherein, the molecular general formula of the nanometer Sialon nitride green fluorescent material is Eu x Si 6-z Al z O z N 8-z (wherein x represents the doping amount of the light-emitting element, z represents the number of Al-O bonds substituted for Si-N bonds, 0)<z is less than or equal to 4.2), and Eu enters a large pore canal in the z-axis direction to be used as a luminescent element and an activator, thereby having fluorescence characteristic.
Wherein the crystal of the nano Sialon nitride green fluorescent material is generated in a manner of comprising a mixture of other crystalline or non-crystalline compounds, and the mass content of the crystal of the nano Sialon nitride green fluorescent material in the mixture is not less than 40%. The nanometer Sialon nitride green fluorescent material emits fluorescence with peak value of wavelength 510-560 nm under the excitation of ultraviolet or blue light source of wavelength 250-500 nm.
The invention also provides a preparation method of the nanometer Sialon nitride green fluorescent material, which comprises the steps of 10 percent 5 The temperature rise and fall rate is controlled by pulse heating within 3300 milliseconds in a high temperature field of 1400-2200 ℃; the method comprises the following steps:
preparing ultra-large aperture dendritic mesoporous silica;
respectively weighing TEA solution, sodium salicylate powder and CTAB powder, dissolving in 25ml of deionized water, pouring into a three-necked flask, reacting for one hour at 80 ℃ and 800r/min, adding a certain amount of TEOS solution, reacting for three hours under the same condition, taking out, loading into a centrifuge tube, washing with ethanol for 3-5 times, putting into an 80 ℃ oven, drying, taking out, grinding, loading into an alumina crucible, moving into a muffle furnace, roasting for three hours at 550 ℃, and taking out for standby after sintering. The size of the prepared mesoporous silica particles is 100-150 nm, the pore diameter is 13-15 nm, and the specific surface area is 430-450 m < 2 >/g.
Preparation of air-stable precursor Complex Al (CON 2 H 4 ) 6 Cl 3 :Eu 3+
Taking different mole ratios of aluminum chloride hexahydrate to urea, and weighing europium chloride hexahydrate with different masses according to the change of doping amount of a luminescence center. Firstly, after the hydrated chlorides with different masses are completely dissolved in absolute methanol, urea is added, and stirring is continued at 60 ℃ and 400r/min until a clear and transparent solution is obtained. Respectively placing the obtained stable clear solutions in an oven for drying to obtain white precursor salt powder, taking out and grinding for later use; the particle size of the prepared powder is submicron or nanometer.
Respectively weighing the two prepared raw materials according to the stoichiometric ratio of the chemical formula, dispersing in absolute methanol for ultrasonic treatment, mixing the two solutions, dispersing again, carrying out ultrasonic treatment again, and then placing in a vacuum drying oven for continuous vacuumizing at 0.098MPa for 30 minutes; promoting the complex particles to enter the mesoporous silica pores to finally obtain the white mixed solution.
Dripping 400 microliters of mixed solution on carbon cloth with the size of 2cm multiplied by 5cm, installing the carbon cloth in a vacuum reaction cavity, respectively fixing two ends of the carbon cloth on a copper electrode, triggering carbothermic reduction reaction by a joule heating method under nitrogen atmosphere, wherein the nitrogen atmosphere is micro-positive pressure, and the pressure value is 0.4-1 MPa; the reaction voltage of carbothermic reduction reaction is 30-50V, the current is 30-80A, the temperature is 1400-2200 ℃ (preferably 1900-2000 ℃), the reaction time is within 3300 milliseconds, and the nano nitride green fluorescent material is obtained.
The experimental detection shows that:
1) When the high-temperature pulse time is within 100 milliseconds at 30-50V, 30-80A and 1400-2200 ℃, the particle size of the prepared green fluorescent material is uniformly distributed within 10 nm;
when the high-temperature pulse time is 100-800 milliseconds at 30-50V, 30-80A and 1400-2200 ℃, the particle size of the prepared green fluorescent material is uniformly distributed at 10-50 nm, and the particles are spherical;
when the high-temperature pulse time is between 800 and 3300 milliseconds at the temperature of between 30 and 50V, between 30 and 80A and between 1400 and 2200 ℃, the particle size of the prepared green fluorescent material is evenly distributed between 50 and 100nm, and the particles are in a polygonal shape. The nanometer Sialon nitride green fluorescent material sintered within 100 milliseconds has the minimum particle size under the conditions of 30V,50A voltage and current sintering;
from the above, the nanometer Sialon nitride green fluorescent materials with different particle sizes can be prepared by adjusting and controlling the pulse heating time of the synthetic raw materials in a high temperature field formed under different current and voltage conditions.
2) The molar ratio of the aluminum chloride hexahydrate to the urea is 6-12; the nano Sialon nitride green fluorescent material prepared by sintering the precursor with the molar ratio of 10 has the highest brightness and the most uniform element distribution (shown in fig. 6).
The preparation method of the nano Sialon nitride green fluorescent material provided by the invention has the advantages of low energy consumption, high preparation speed and simplicity in operation.
The nano nitride green fluorescent material prepared by the invention can be applied in the field of ink-jet printing, can realize that the particle size of particles reaches 1-3 nm at least by regulating pulse heating time, has the emission peak wavelength of 516nm and the half-peak width of 36nm, and has better practical application potential.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. A nano Sialon nitride green fluorescent material is characterized in that the molecular general formula is Eu x Si 6-z Al z O z N 8-z Wherein x represents the doping amount of the light-emitting element, z represents the number of Al-O bonds substituted for Si-N bonds, and 0<z is less than or equal to 4.2; eu element enters a large pore canal in the z-axis direction and is used as a luminescence center and an activator;
the nanometer Sialon nitride green fluorescent material is 10 percent 5 The temperature rise and drop rate of the temperature is controlled within 3300 milliseconds in a high temperature field of 1400-2200 ℃.
2. The nano Sialon nitride green phosphor of claim 1, wherein the crystals of the nano Sialon nitride green phosphor are formed in a manner of containing a mixture of other crystalline or non-crystalline compounds, and the mass content of the crystals of the nano Sialon nitride green phosphor is not less than 40% in the mixture.
3. The nano Sialon nitride green fluorescent material according to claim 1, wherein the nano Sialon nitride green fluorescent material emits fluorescence having a peak value at a wavelength of 510-560 nm under excitation of an ultraviolet or blue light source having a wavelength of 250-500 nm.
4. The nano Sialon nitride green fluorescent material according to claim 1, wherein the preparation method specifically comprises the following steps:
1) Precursor Complex Al (CON) 2 H 4 ) 6 Cl 3 :Eu 3+ Dispersing dendritic mesoporous silica in absolute methanol, and then carrying out ultrasonic mixing and continuous vacuumizing treatment to obtain a mixed solution;
2) And (3) dripping the mixed solution on carbon cloth, installing the carbon cloth in a vacuum reaction cavity, respectively fixing two ends of the carbon cloth on a copper electrode, and triggering a carbothermic reduction reaction in a joule heating method under a nitrogen atmosphere to obtain the nano Sialon nitride green fluorescent material.
5. The green fluorescent nano Sialon nitride material of claim 4, wherein the method for preparing the precursor complex in step 1) comprises:
a) Completely dissolving aluminum chloride hexahydrate and europium chloride hexahydrate in absolute methanol, adding urea, and continuously stirring at 60 ℃ and 400r/min until a clear and transparent solution is obtained;
b) And then placing the obtained stable clear solution in an oven for drying to obtain white precursor salt powder, taking out and grinding to obtain the precursor complex.
6. The nano Sialon nitride green phosphor of claim 5, wherein the preparation method of the dendritic mesoporous silica in step 1) comprises:
a) Adding TEA solution, sodium salicylate powder and CTAB powder into 25ml deionized water, and uniformly mixing;
b) After one hour of reaction at 80 ℃ and 800r/min, adding TEOS solution, and continuing the reaction for three hours under the same conditions;
c) And washing, drying and grinding the product, and roasting at 550 ℃ for three hours to obtain the dendritic mesoporous silica after sintering.
7. The green fluorescent nano Sialon nitride material of claim 4, wherein 400 microliters of the mixed solution is dripped on a carbon cloth with a size of 2cm x 5cm in step 2); the reaction voltage of carbothermic reaction is 30-50V, the current is 30-80A, the temperature is 1400-2200 ℃, and the reaction time is within 3300 milliseconds.
8. The nano Sialon nitride green phosphor of claim 6, wherein the particle size of the precursor complex and the dendritic mesoporous silica in step 1) is submicron or nanoscale; the vacuum pressure in the vacuumizing treatment is 0.098MPa, and the vacuumizing time is 30min;
the nitrogen atmosphere in the step 2) is micro positive pressure, and the pressure value is 0.4 MPa-1 MPa;
the molar ratio of the aluminum chloride hexahydrate to the urea in the step a) is 6 to 12;
the dendritic mesoporous silica particles in the step C) have a size of 100-150 nm, a pore diameter of 13-15 nm and a specific surface area of 430-450 m 2 /g。
9. The application of the nano Sialon nitride green fluorescent material in the field of ink-jet printing is characterized in that the nano Sialon nitride green fluorescent material is particles within 10nm obtained in the pulse sintering 100 milliseconds at 30-50V, 30-80A and 1400-2200 ℃, and the emission wavelength is 510-560 nm and the half-peak width is 36nm under the excitation of a light source with the wavelength of 250-500 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211344798.2A CN115678548B (en) | 2022-10-31 | 2022-10-31 | Nano Sialon nitride green fluorescent material and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211344798.2A CN115678548B (en) | 2022-10-31 | 2022-10-31 | Nano Sialon nitride green fluorescent material and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115678548A CN115678548A (en) | 2023-02-03 |
| CN115678548B true CN115678548B (en) | 2023-10-20 |
Family
ID=85045304
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211344798.2A Active CN115678548B (en) | 2022-10-31 | 2022-10-31 | Nano Sialon nitride green fluorescent material and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115678548B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20100099451A (en) * | 2009-03-03 | 2010-09-13 | 서울대학교산학협력단 | Fabrication method for nitride phosphor using spark plasma sintering |
| KR20200000933A (en) * | 2018-06-26 | 2020-01-06 | 엘지이노텍 주식회사 | Phosphor composition, light emitting device package having thereof |
| CN113736455A (en) * | 2020-05-27 | 2021-12-03 | 厦门大学 | Narrow-band emission green nitride fluorescent material and preparation method and application thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5122765B2 (en) * | 2006-06-09 | 2013-01-16 | 電気化学工業株式会社 | Phosphor production method, phosphor and lighting apparatus |
| CN102639672B (en) * | 2009-11-10 | 2015-05-13 | 电气化学工业株式会社 | Beta-sialon, method for producing same and light-emitting device using same |
-
2022
- 2022-10-31 CN CN202211344798.2A patent/CN115678548B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20100099451A (en) * | 2009-03-03 | 2010-09-13 | 서울대학교산학협력단 | Fabrication method for nitride phosphor using spark plasma sintering |
| KR20200000933A (en) * | 2018-06-26 | 2020-01-06 | 엘지이노텍 주식회사 | Phosphor composition, light emitting device package having thereof |
| CN113736455A (en) * | 2020-05-27 | 2021-12-03 | 厦门大学 | Narrow-band emission green nitride fluorescent material and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 在发光二极管背光源上极具应用前景的Beta-sialon(Si_(6-z)Al_zO_zN_(8-z))∶Eu~(2+)窄带绿色荧光粉（英文）;解荣军;周天亮;高桥向星;广崎尚登;;应用化学(第08期) * |
| 解荣军 ; 周天亮 ; 高桥向星 ; 广崎尚登 ; .在发光二极管背光源上极具应用前景的Beta-sialon(Si_(6-z)Al_zO_zN_(8-z))∶Eu~(2+)窄带绿色荧光粉（英文）.应用化学.2016,(第08期), * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115678548A (en) | 2023-02-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7598194B2 (en) | Oxynitride powder and production method thereof | |
| JP4052136B2 (en) | Sialon oxynitride phosphor and method for producing the same | |
| Raju et al. | Eu 3+ ion concentration induced 3D luminescence properties of novel red-emitting Ba 4 La 6 (SiO 4) O: Eu 3+ oxyapatite phosphors for versatile applications | |
| JP4277666B2 (en) | Method for producing sialon phosphor and sialon phosphor | |
| Li et al. | Luminescence enhancement of CsPbBr 3 quantum dot glasses induced by two unexpected methods: mechanical and hydration crystallization | |
| Liu et al. | Microwave-assisted solvothermal preparation and photoluminescence properties of Y2O3: Eu3+ phosphors | |
| WO2009048150A1 (en) | Β-sialon phosphor powder and process for production of the same | |
| US9758720B2 (en) | Oxynitride phosphor powder, silicon nitride powder for production of oxynitride phosphor powder, and production method of oxynitride phosphor powder | |
| KR101762473B1 (en) | SILICON NITRIDE POWDER FOR SILICONITRIDE FLUORESCENT MATERIAL, SR3AL3SI13O2N21 FLUORESCENT MATERIAL AND β-SIALON FLUORESCENT MATERIAL BOTH OBTAINED USING SAME, AND PROCESSES FOR PRODUCING THESE | |
| Weng et al. | Yellowish green-emitting KSrPO4: Tb3+ phosphors with various doping concentrations prepared by using microwave assisted sintering | |
| Yuhang et al. | Luminescence properties of Eu3+ doped BaMoO4 transparent glass ceramics | |
| WO2012167517A1 (en) | Method for preparing nitride/oxynitride fluorescent powder used by white led | |
| CN114316956B (en) | Submicron green silicate fluorescent powder and preparation method thereof | |
| Qin et al. | Ultra-long Sialon nanobelts: large-scale synthesis via a pressure enhanced CVD process and photoluminescence characteristics | |
| JP2011213839A (en) | METHOD FOR PRODUCING Li CONTAINING α-SIALON PHOSPHOR | |
| Yang et al. | The optimum sintering condition for KSrPO4: Eu3+ phosphors applied in WLEDs | |
| CN115678548B (en) | Nano Sialon nitride green fluorescent material and preparation method and application thereof | |
| JP5190835B2 (en) | Method for producing multi-component oxynitride phosphor | |
| Gu et al. | Nitridation from core-shell oxides for tunable luminescence of BaSi 2 O 2 N 2: Eu 2+ LED phosphors | |
| Tran et al. | Achieving High Luminescent Performance K 2 SiF 6: Mn 4+ Phosphor by Co-precipitation Process with Controlling the Reaction Temperature | |
| Qu et al. | Synthesis of CdSiO3 powder by sol–gel method | |
| JP2012082269A (en) | Method for manufacturing high temperature-fired phosphor, and phosphor | |
| Cao et al. | BPO4@ B2O3 and (BPO4@ B2O3): Eu3+: The novel single-emitting-component phosphors for near UV-white LEDs | |
| JP6354326B2 (en) | Method for producing sialon powder | |
| CN113150777B (en) | Preparation method of crystallization-induced orange-red luminous solid carbon dots |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |