CN111646703A - Fluoride/oxyfluoride fluorescent glass ceramic and preparation method and application thereof - Google Patents
Fluoride/oxyfluoride fluorescent glass ceramic and preparation method and application thereof Download PDFInfo
- Publication number
- CN111646703A CN111646703A CN202010419991.2A CN202010419991A CN111646703A CN 111646703 A CN111646703 A CN 111646703A CN 202010419991 A CN202010419991 A CN 202010419991A CN 111646703 A CN111646703 A CN 111646703A
- Authority
- CN
- China
- Prior art keywords
- fluoride
- oxyfluoride
- glass ceramic
- sintering
- rare earth
- 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.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/006—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of microcrystallites, e.g. of optically or electrically active material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/20—Glass-ceramics matrix
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/30—Methods of making the composites
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Glass Compositions (AREA)
Abstract
The invention relates to a fluoride/oxyfluoride nanocrystalline composite fluorescent glass ceramic material and a preparation method and application thereof. The invention not only effectively retains the luminescence property of the fluoride/oxyfluoride nanocrystalline, but also has great application potential in the aspects of color displays, sensors, lasers, optical fiber amplifiers and the like due to simple preparation process, good thermal stability and long fluorescence service life.
Description
Technical Field
The invention belongs to the field of fluorescent glass ceramic materials, and particularly relates to fluoride/oxyfluoride fluorescent glass ceramic and a preparation method and application thereof.
Background
Fluorescent glass ceramic is a new type of luminescent material, also known as microcrystalline glass. Compared with the traditional glass material, the composite material obtained by the heat treatment process has the characteristics of glass, such as high hardness, high mechanical strength, good chemical stability, excellent wear resistance and stable dielectric constant, and simultaneously has the advantages of high thermal conductivity of ceramic phase crystals and capability of doping luminescent ions. Therefore, the composite material can be used as a structural material and a functional material and is gradually widely applied to the fields of energy, chemical engineering, biomedicine, automobiles, architectural decoration and the like.
At present, rare earth doped fluoride/oxyfluoride nanocrystals are always the research focus of fluorescent materials due to the advantages of low phonon energy, high luminous efficiency, long fluorescence lifetime and the like, but the application of the rare earth doped fluoride/oxyfluoride nanocrystals in the field of optical devices is limited due to poor thermal stability. The glass material is an ideal matrix material for the nanocrystalline material due to the advantages of high thermal conductivity, good transparency, high chemical stability and the like, and the research idea for preparing the nanocrystalline composite fluorescent glass ceramic composite material is widely favored by researchers. Natalia Pawlik et al in the literature (J.Euro.Ceram.Soc.,2019,39(15):5010-5017) describe a long fluorescence lifetime YF3:Eu3+A preparation method of composite glass ceramic. However, in the traditional preparation process, the rare earth ion active luminescent center of the fluoride nanocrystalline composite fluorescent glass ceramic cannot firmly and effectively occupy the fluoride lattice site, and defects are easily formed, so that the fluorescence emission intensity is reduced, the fluorescence life is shortened, and the actual application requirements are difficult to meet. Therefore, it is urgent and necessary to develop a fluorescent glass-ceramic having high luminous intensity and long fluorescence lifetime.
Disclosure of Invention
The invention aims to solve the technical problem of providing a fluoride/oxyfluoride nanocrystalline composite fluorescent glass ceramic material and a preparation method and application thereof, and through methods of reducing sintering temperature, shortening preparation time, improving matrix stability and the like, rare earth ions are stabilized on fluoride/oxyfluoride lattice sites to the maximum extent, the original fluorescence property of fluoride/oxyfluoride nanocrystals is kept, meanwhile, the fluorescence life is prolonged, and the thermal stability is improved.
The invention provides a fluoride/oxyfluoride nanocrystalline composite fluorescent glass ceramic material which is prepared by mixing and sintering 95-99 wt% of mesoporous silicon-based material and 1-5 wt% of fluoride/oxyfluoride fluorescent nanocrystalline.
The mesoporous silica-based material is one of SBA series, FDU series, ZSM series and MCM series.
The fluoride fluorescent nano crystal is rare earth element doped LaF3、YF3、Ba2YbF7、NaLuF4Or NaGdF4(ii) a Wherein, the rare earth elements are Eu, La, Er, Yb, Tm or Ho, and the doping proportion (mol percentage) of the rare earth elements is 1-5%.
The oxyfluoride fluorescent nano crystal is rare earth element doped YOF; wherein, the rare earth elements are Eu, La, Er, Yb, Tm or Ho, and the doping proportion (mol percentage) of the rare earth elements is 1-5%.
The average grain size of the fluoride/oxyfluoride fluorescent nano crystal is 10-100 nm.
The invention also provides a preparation method of the fluoride/oxyfluoride nanocrystalline composite fluorescent glass ceramic material, which comprises the following steps:
uniformly mixing 95-99% of silicon-based mesoporous powder and 1-5% of fluoride/oxyfluoride fluorescent nano-crystal according to weight percentage to obtain composite powder; loading the composite powder into a graphite mold, placing the graphite mold in a discharge plasma sintering furnace chamber, and sintering in a vacuum environment to obtain composite glass ceramic; and (4) after cooling, grinding and polishing to obtain the fluoride/oxyfluoride nanocrystalline composite fluorescent glass ceramic material.
The sintering pressure is 50-100 MPa, the sintering time is 5-10min, the heating rate is 50-150 ℃/min, the sintering temperature is 950-1050 ℃, and the heat preservation time is 1-3 min.
The invention also provides application of the fluoride/oxyfluoride nanocrystalline composite fluorescent glass ceramic material in optical devices, solid-state lasers or biological marks.
Advantageous effects
(1) The invention adopts the discharge plasma sintering technology to encapsulate the fluoride/oxyfluoride nanocrystalline in the mesoporous silicon-based glass, and the preparation process has little damage to the composite nanocrystalline due to the fast heating rate, the low sintering temperature and the short heat preservation time, thereby furthest keeping the original luminescence property of the fluoride/oxyfluoride nanocrystalline.
(2) The fluoride/oxyfluoride has low phonon energy, can well avoid non-radiative transition in the luminescence process, and has high light conversion efficiency, and the composite fluorescent glass ceramic has the characteristics of good thermal stability and high thermal conductivity of a glass substrate, and simultaneously has high-efficiency light conversion efficiency and luminescence property of the fluoride/oxyfluoride;
(3) the composite fluorescent glass ceramic obtained by the invention has the fluorescence lifetime of 6.891ms and has application potential in the fields of optical devices and biomarkers.
Drawings
FIGS. 1a-b are XRD patterns of a fluoride nanocrystalline composite fluorescent glass ceramic material prepared in example 1;
FIGS. 2a-b are graphs of the fluorescence lifetime of the fluoride nanocrystalline composite fluorescent glass ceramic material prepared in example 2;
FIGS. 3a-d are a fluorescence spectrum and a fluorescence spectrum of the oxyfluoride nanocrystalline composite fluorescent glass ceramic material prepared in example 3.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
La(NO3)3·6H2O and Eu (NO)3)3·XH2Accurately weighing O according to the molar ratio of (La: Eu 95:5), dissolving in deionized water at room temperature, placing in a 65 ℃ oil bath kettle, and magnetically stirring at the stirring speed of 500 rpm; excess NH4F is dissolved in a small amount of deionized water to remove NH4Slowly dripping the solution F into the mixed solution, observing a white precipitate, adding a nitric acid or hydrochloric acid solution to adjust the pH value to 2-3, and continuously stirring and heating for 90 min; further carrying out hydrothermal treatment on the mixed solution, transferring the mixed solution with the precipitate into a 100ml hydrothermal kettle, reacting for 18h at 180 ℃, taking out the hydrothermal kettle after the reaction is finished, naturally cooling to room temperature, pouring out supernatant, washing and centrifuging the precipitate for three times by using deionized water and absolute ethyl alcohol respectively, and drying the obtained white precipitate for 24h at 60 ℃ in a blast drying oven to obtain LaF3:Eu3+And (4) nanocrystals.
By using mesoporous FDU-12 silicon-based powder and LaF3:Eu3+The luminescent nanocrystalline powder is used as the starting material. Mixing the raw materials according to different weight ratios (LaF)3:Eu3+Luminescent nanocrystalline powder: 1 wt%, 2 wt%, 3 wt%, 4 wt%, 5 wt%) and then transferred into a graphite mold having an inner diameter of 10 mm. Sintering the mixed powder under a uniaxial pressure of 50MPa for about 10min according to specific sintering parameters by spark plasma sintering. The detailed sintering parameters are as follows: heating at 600 deg.C for 3min, and sintering at high temperature at a heating rate of 120 deg.C/min. And (3) keeping the temperature for about 1min at the sintering temperature of 950 ℃ to obtain the composite fluorescent glass ceramic sample. All samples were surface polished twice to a thickness of 1 mm. The crystal form is tested by XRD, and the results are shown in figures 1 a-b. The morphology of the LaF is characterized by SEM and TEM, and the LaF can be known3:Eu3+The nanocrystals are in the form of hexagonal nanoplatelets of about 50nm in size and proved to be uniformly dispersed in the glass matrix without severe interfacial reaction. The fluorescence spectrometer is adopted to test the excitation emission spectrogram, and the experimental result of red light emission with 590nm and 612nm under the excitation of 396nm shows that the fluoride nanocrystal is formedThe optical performance is effectively protected.
Example 2
Y(NO3)3·6H2O and Eu (NO)3)3·XH2Accurately weighing O according to the molar ratio of (Y: Eu: 95:5), dissolving in deionized water at room temperature, placing in a 65 ℃ oil bath kettle, and magnetically stirring at the stirring speed of 500 rpm; excess NH4F is dissolved in a small amount of deionized water to remove NH4Slowly dripping the solution F into the mixed solution, observing a white precipitate, adding a certain amount of nitric acid or hydrochloric acid solution to adjust the pH value to 2-3, and continuously stirring and heating for 90 min; further carrying out hydrothermal treatment on the mixed solution, transferring the mixed solution with the precipitate into a 100ml hydrothermal kettle, reacting for 18h at 180 ℃, taking out the hydrothermal kettle after the reaction is finished, naturally cooling to room temperature, pouring out supernatant, washing and centrifuging the precipitate for three times by using deionized water and absolute ethyl alcohol respectively, and drying the obtained white precipitate for 24h at 60 ℃ in a blast drying oven to obtain YF3:Eu3+And (4) nanocrystals.
By using mesoporous SBA-15 silicon-based powder and YF3:Eu3+The luminescent nanocrystalline powder is used as the starting material. Mixing the raw materials at different weight ratios (YF)3:Eu3+Luminescent nanocrystalline powder: 1 wt%, 2 wt%, 3 wt%, 4 wt%, 5 wt%) were uniformly ground and mixed, and then transferred into a graphite mold having an inner diameter of 10 mm. Sintering the mixed powder under a uniaxial pressure of 80MPa for about 10min according to specific sintering parameters by spark plasma sintering. The detailed sintering parameters are as follows: heating at 600 deg.C for 3min, and sintering at high temperature at a heating rate of 120 deg.C/min. And (3) keeping the temperature for about 1min at the sintering temperature of 1000 ℃ to obtain the composite glass ceramic sample. All samples were surface polished twice to a thickness of 1 mm. The existence of YF in the composite glass ceramic can be known through XRD (X-ray diffraction) test of crystal form3:Eu3+Nanocrystalline diffraction peaks. The morphology of the YF is characterized by SEM and TEM, and the YF can be known3:Eu3+The nanocrystal size was 150 nm and was uniformly dispersed. The fluorescence lifetime was tested using a fluorescence spectrometer transient spectrometer as shown in fig. 2 a-b.The excitation emission spectrum of the nano-crystalline glass ceramic composite material is tested by a fluorescence spectrometer, so that the nano-crystalline glass ceramic composite material has the same 592nm red light emission under 393nm excitation.
Example 3
Example 2 dried YF after centrifugation3:Eu3+Fully grinding the nanocrystalline in a mortar, then putting the powder into a muffle furnace to be respectively heated to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃ and 900 ℃ at the heating rate of 2 ℃/min, keeping the temperature for three hours, and then naturally cooling to room temperature to obtain YOF, Eu3+And (4) nanocrystals.
Using MCM-41 mesoporous silicon-based powder and YOF Eu3+The luminescent nanocrystalline powder is used as the starting material. Mixing the raw materials according to different weight ratios (YOF: Eu)3+Luminescent nanocrystalline powder: 1 wt%, 2 wt%, 3 wt%, 4 wt%, 5 wt%) were uniformly ground and mixed, and then transferred into a graphite mold having an inner diameter of 10 mm. Sintering the mixed powder under a uniaxial pressure of 100MPa for about 10min according to specific sintering parameters by spark plasma sintering. The detailed sintering parameters are as follows: heating at 600 deg.C for 3min, and sintering at high temperature at a heating rate of 120 deg.C/min. And (3) keeping the temperature for about 2min at the sintering temperature of 1050 ℃ to obtain the composite glass ceramic sample. All samples were surface polished twice to a thickness of 1 mm. The existence of YOF Eu in the composite glass ceramic can be known through XRD test of the crystal form3+Nanocrystalline diffraction peaks and no other hetero-phase diffraction peaks appear. The appearance of the film is characterized by SEM and TEM, and YOF is known3+The nanocrystals are uniformly dispersed and do not undergo significant interfacial reactions with silica. The fluorescence emission spectrum of the sample is measured by a fluorescence spectrometer, and the results are shown in FIG. 3, wherein, FIGS. 3a-b are YOF3+Glass ceramic composite and YOF Eu3+The excitation emission spectra of the nanocrystalline powders all have the same optimum excitation wavelength of 393nm, and the emission peak has no obvious change in the main emission peak position except the changes such as emission peak broadening caused by the internal structure defects of the glass ceramics. FIG. 3c is a graph of different YOF: Eu3+The emission spectra of the glass ceramics in the content are shown, and all show Eu3+The characteristic peak of the ion and the luminous intensity are enhanced along with the increase of the content of the nanocrystal. FIG. 3d shows YOF: Eu3+Glass ceramic material object diagram.
Claims (8)
1. A fluoride/oxyfluoride nanocrystalline composite fluorescent glass ceramic material is characterized in that: the material is prepared by mixing and sintering 95-99% of mesoporous silicon-based material and 1-5% of fluoride/oxyfluoride fluorescent nano crystal according to weight percentage.
2. The material of claim 1, wherein: the mesoporous silica-based material is one of SBA series, FDU series, ZSM series and MCM series.
3. The material of claim 1, wherein: the fluoride fluorescent nano crystal is rare earth element doped LaF3、YF3、Ba2YbF7、NaLuF4Or NaGdF4(ii) a Wherein the rare earth elements are Eu, La, Er, Yb, Tm or Ho, and the doping proportion of the rare earth elements is 1-5%.
4. The material of claim 1, wherein: the oxyfluoride fluorescent nano crystal is rare earth element doped YOF; wherein the rare earth elements are Eu, La, Er, Yb, Tm or Ho, and the doping proportion of the rare earth elements is 1-5%.
5. The material of claim 1, wherein: the average grain size of the fluoride/oxyfluoride fluorescent nano crystal is 10-100 nm.
6. A preparation method of a fluoride/oxyfluoride nanocrystalline composite fluorescent glass ceramic material comprises the following steps:
uniformly mixing 95-99% of silicon-based mesoporous powder and 1-5% of fluoride/oxyfluoride fluorescent nano-crystal according to weight percentage to obtain composite powder; loading the composite powder into a graphite mold, placing the graphite mold in a discharge plasma sintering furnace chamber, and sintering in a vacuum environment to obtain composite glass ceramic; and (4) after cooling, grinding and polishing to obtain the fluoride/oxyfluoride nanocrystalline composite fluorescent glass ceramic material.
7. The method of claim 6, wherein: the sintering pressure is 50-100 MPa, the sintering time is 5-10min, the heating rate is 50-150 ℃/min, the sintering temperature is 950-1050 ℃, and the heat preservation time is 1-3 min.
8. The use of the fluoride/oxyfluoride nanocrystalline composite fluorescent glass ceramic material of claim 1, wherein: application to optical devices, solid state lasers or biomarkers.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010419991.2A CN111646703A (en) | 2020-05-18 | 2020-05-18 | Fluoride/oxyfluoride fluorescent glass ceramic and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010419991.2A CN111646703A (en) | 2020-05-18 | 2020-05-18 | Fluoride/oxyfluoride fluorescent glass ceramic and preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111646703A true CN111646703A (en) | 2020-09-11 |
Family
ID=72352297
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010419991.2A Pending CN111646703A (en) | 2020-05-18 | 2020-05-18 | Fluoride/oxyfluoride fluorescent glass ceramic and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111646703A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116462510A (en) * | 2023-04-10 | 2023-07-21 | 东华大学 | Calcium fluoride-based fluorescent ceramic material and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2003237338A1 (en) * | 2002-08-02 | 2004-03-03 | 3M Innovative Properties Company | Plasma projection |
| CN101613183A (en) * | 2009-04-07 | 2009-12-30 | 上海师范大学 | Multi-functional fluorescent glass of long-wave broadband burst of ultraviolel and preparation method thereof |
| CN104310783A (en) * | 2014-10-09 | 2015-01-28 | 东华大学 | Long-afterglow luminescent glass and preparation method thereof |
| CN104876441A (en) * | 2015-04-10 | 2015-09-02 | 东华大学 | Quantum dot glass phosphor powder as well as preparation method and application thereof |
| CN105399335A (en) * | 2015-11-18 | 2016-03-16 | 天津工业大学 | Lanthanum-doped mesoporous bioactive glass, and preparation method and application thereof |
-
2020
- 2020-05-18 CN CN202010419991.2A patent/CN111646703A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2003237338A1 (en) * | 2002-08-02 | 2004-03-03 | 3M Innovative Properties Company | Plasma projection |
| CN101613183A (en) * | 2009-04-07 | 2009-12-30 | 上海师范大学 | Multi-functional fluorescent glass of long-wave broadband burst of ultraviolel and preparation method thereof |
| CN104310783A (en) * | 2014-10-09 | 2015-01-28 | 东华大学 | Long-afterglow luminescent glass and preparation method thereof |
| CN104876441A (en) * | 2015-04-10 | 2015-09-02 | 东华大学 | Quantum dot glass phosphor powder as well as preparation method and application thereof |
| CN105399335A (en) * | 2015-11-18 | 2016-03-16 | 天津工业大学 | Lanthanum-doped mesoporous bioactive glass, and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| PING HUANG等: "Preparation and luminescence of transparent silica glass-ceramics containing LaF3:Eu3+ nanocrystals", 《MATERIALS LETTERS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116462510A (en) * | 2023-04-10 | 2023-07-21 | 东华大学 | Calcium fluoride-based fluorescent ceramic material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Li et al. | Color control and white light generation of upconversion luminescence by operating dopant concentrations and pump densities in Yb 3+, Er 3+ and Tm 3+ tri-doped Lu 2 O 3 nanocrystals | |
| CN101284733B (en) | Yttrium aluminium garnet and yttria double crystal transparent ceramic and method for making same | |
| Zhang et al. | A novel scheme to acquire enhanced up-conversion emissions of Ho3+ and Yb3+ co-doped Sc2O3 | |
| CN102382654A (en) | Preparation method of up-conversion fluorescent material rare earth doped NaYF4 nanocrystal | |
| CN102994089A (en) | Preparation method of alkaline earth fluoride nanocrystal with ultra small core-shell structure | |
| CN115557787B (en) | Sesquioxide transparent ceramic and preparation method thereof | |
| Yi et al. | The effect of Gd3+ ions on fabrication and luminescence properties of Nd3+-doped (Ca1-xGdx) F2+ x transparent ceramics | |
| Yao et al. | Garnet transparent ceramic film of Y3Al5O12: Eu3+ fabricated through an interface reaction of layered rare-earth hydroxide nanosheets on amorphous alumina | |
| Liu et al. | Fabrication and characterizations of Cr3+‐doped ZnGa2O4 transparent ceramics with persistent luminescence | |
| CN111646703A (en) | Fluoride/oxyfluoride fluorescent glass ceramic and preparation method and application thereof | |
| CN102515549A (en) | Rare earth doping cerium oxide contained nano-crystal glass ceramic and preparation method thereof | |
| Aminaka et al. | Effect of rare-earth oxide additives on transparency and fluorescence of α-SiAlON ceramics | |
| CN111778025A (en) | Erbium-ytterbium co-doped scandium molybdate heat-enhanced up-down conversion luminescent material and preparation method thereof | |
| CN101538739A (en) | Cadmium tungstate crystal and preparation method thereof | |
| CN115232618B (en) | Phase-change induced upconversion green light near-zero thermal quenching fluorescent powder and preparation method thereof | |
| Jiao et al. | Preparation and properties of Nd: YAG ultra-fine powders | |
| CN108504357B (en) | Titanium aluminate based up-conversion luminescent material, preparation method and application | |
| Wang et al. | Sol-gel synthesis and enhanced 1.54 μm emission in Y2O3: Yb3+, Er3+ nanophosphors co-doped with Ce3+ ions | |
| CN107573071B (en) | Monodisperse spherical Y2O3And Al2O3Powder preparation (Y)1-xYbx) Method for preparing AG transparent ceramic | |
| CN115093223A (en) | Thermal enhancement luminescence erbium-ytterbium co-doped scandium zirconium phosphotungstate two-dimensional negative thermal expansion material with moisture resistance and abnormality and preparation method thereof | |
| CN113603475A (en) | Preparation method of trivalent chromium ion doped magnesium aluminate spinel transparent ceramic | |
| CN102503139A (en) | Up-conversion luminescence transparent glass ceramics and preparation method thereof | |
| CN112239352A (en) | Complex phase fluorescent ceramic material and preparation method thereof | |
| Kravtsov et al. | Synthesis and study of the optical and spectral-luminescent properties of LuAG: Ce ceramic | |
| CN110713833A (en) | Rare earth doped up-conversion luminescent material and preparation method thereof |
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 | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20200911 |
|
| WD01 | Invention patent application deemed withdrawn after publication |