CN116218525B - Thermosensitive up-conversion luminescent material and preparation method thereof - Google Patents
Thermosensitive up-conversion luminescent material and preparation method thereof Download PDFInfo
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- CN116218525B CN116218525B CN202310057292.1A CN202310057292A CN116218525B CN 116218525 B CN116218525 B CN 116218525B CN 202310057292 A CN202310057292 A CN 202310057292A CN 116218525 B CN116218525 B CN 116218525B
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- 239000000463 material Substances 0.000 title claims abstract description 104
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 10
- 239000010431 corundum Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 3
- 238000010304 firing Methods 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 239000007858 starting material Substances 0.000 claims 1
- 238000004020 luminiscence type Methods 0.000 abstract description 8
- 230000001105 regulatory effect Effects 0.000 abstract description 6
- 238000003384 imaging method Methods 0.000 abstract description 5
- 238000005245 sintering Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 229910003893 H2WO4 Inorganic materials 0.000 description 2
- 238000005415 bioluminescence Methods 0.000 description 2
- 230000029918 bioluminescence Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 2
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 238000002428 photodynamic therapy 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
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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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
- C09K11/7776—Vanadates; Chromates; Molybdates; Tungstates
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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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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention provides an up-conversion luminescent material and a preparation method thereof, wherein the chemical general formula of the material is A 2‑2x‑2yNd2xMO6; uniformly mixing the raw materials according to the stoichiometric ratio in the chemical formula A 2‑2x‑2yNd2xMO6 to generate a first material; calcining the first material to generate a second material; and grinding the cooled second material to obtain the thermosensitive up-conversion luminescent material. The material of the invention rapidly increases the up-conversion luminescence intensity along with the temperature rise; therefore, the luminous performance can be regulated and controlled by regulating the temperature. The material has the potential of being applied to high-temperature up-conversion imaging, high-temperature and high-sensitivity temperature sensors, laser anti-counterfeiting and other aspects.
Description
Technical Field
The invention relates to the field of material synthesis, in particular to a thermosensitive up-conversion luminescent material and a preparation method thereof.
Background
The up-conversion luminescent material is capable of converting a plurality of low energy long wavelength photons into one high energy short wavelength photon. Based on the characteristics, the rare earth doped up-conversion luminescent material has wide application in the fields of laser anti-counterfeiting, three-dimensional stereoscopic display, high-efficiency solar cells, bioluminescence imaging, solid-state lasers, high-sensitivity temperature sensors and the like.
Among them, neodymium (Nd) -doped up-conversion luminescence is particularly widely used in the fields of bioluminescence imaging and the like. Meanwhile, nd 3+ has a large absorption cross section around 800nm, and thus, some Nd 3+ is used for photodynamic therapy as a material system of sensitizer. For example, in 2016, researchers have designed core-shell luminescent materials using 808nm as an excitation light source and Nd 3+ as a sensitizer, which have an emission intensity 6-fold higher than that of conventional luminescent structures (Advanced Functional Materials,2016, 26 (26): 4778-4785).
However, the current Nd-doped luminescent materials are not temperature-sensitive and are only suitable for a relatively small temperature range.
Disclosure of Invention
The invention provides a thermosensitive up-conversion luminescent material and a preparation method thereof, which are used for overcoming at least one technical problem in the prior art.
According to a first aspect of an embodiment of the present invention, there is provided a thermosensitive up-conversion luminescent material comprising: the chemical general formula of the material is A 2-2x-2yNd2xMO6; wherein A is one or more of Y, lu, ho, dy, M is W or Mo; in the chemical general formula, x is more than 0 and less than or equal to 0.10,0, and y is more than or equal to 0.30.
Optionally, the x=0.005; y=0.18.
According to a second aspect of the embodiment of the present invention, there is provided a method for preparing a thermosensitive up-conversion luminescent material, including: uniformly mixing the raw materials according to the stoichiometric ratio in the chemical formula A 2-2x-2yNd2xMO6 to obtain a first material; calcining the first material to generate a second material; and grinding the cooled second material to obtain the thermosensitive up-conversion luminescent material.
Optionally, the step of calcining the first material to produce a second material includes: the method comprises the steps of firstly carrying out presintering treatment, grinding after the presintering treatment is finished, and calcining the ground powder.
Optionally, the presintering temperature is 400-600 ℃; the presintering time is 2-30 hours.
Optionally, the temperature of the calcination is 1000 ℃ -1400 ℃; the calcination time is 2-10 hours.
Optionally, the granularity of the thermosensitive up-conversion luminescent material is 0.2-100 μm. The thermosensitive up-conversion luminescent material has the texture of fluorescent powder.
Optionally, the raw materials are compounds containing elements in the chemical formula in the forms of oxide, carbonate, oxalate, acetate and hydroxide, and the compounds have the purity of 99.99%.
Optionally, the atmosphere of the calcination treatment is air or pure oxygen.
Optionally, the second material is placed in a ceramic boat or corundum boat and then calcined or presintered.
The invention provides a thermosensitive up-conversion luminescent material and a preparation method thereof, wherein the material takes an A2MO6 type material as a matrix of the luminescent material. On one hand, the phonon energy of the material is relatively low, so that the up-conversion luminescence is relatively strong; on the other hand, the material is an oxide, and is excellent in thermal stability and chemical stability. Along with Nd doping, the material rapidly increases the up-conversion luminescence intensity along with the temperature rise in a larger temperature range; therefore, the luminous performance can be regulated and controlled by regulating the temperature. The material has the potential of being applied to high-temperature up-conversion imaging, high-temperature and high-sensitivity temperature sensors, laser anti-counterfeiting and other aspects. Is one of the innovative points of the embodiments of the present invention.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method for preparing a thermosensitive up-conversion luminescent material according to the present invention;
FIG. 2 is a temperature swing X-ray diffraction (XRD) spectrum of sample Y 1.995Nd0.005WO6 obtained by sintering at 1200 o C in example 2;
FIG. 3 is a Scanning Electron Microscope (SEM) topography of sample Y 1.995Nd0.005WO6 obtained in Experimental example 2;
FIG. 4 is a graph showing luminescence spectra of sample Y 1.995Nd0.005WO6 obtained in example 2 up-converted at different temperatures;
FIG. 5 is a graph showing luminescence spectra of up-conversion at different temperatures of the sample Lu 1.995Nd0.005WO6 obtained in example 3.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only 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 any inventive effort, are intended to be within the scope of the invention.
It should be noted that the terms "comprising" and "having" and any variations thereof in the embodiments of the present invention and the accompanying drawings are intended to cover non-exclusive inclusions. For example, a process, method, and apparatus, article, or apparatus that comprises a list of steps or elements is not limited to only those listed steps or elements but may include other steps or elements not listed or inherent to such process, method, article, or apparatus.
The invention provides a thermosensitive up-conversion luminescent material, which has a chemical general formula of A 2-2x-2yNd2xMO6.
Wherein A is one or more of Y, lu, ho, dy, and M is W or Mo.
Further, x is more than 0 and less than or equal to 0.10,0, y is more than or equal to 0.30, and further x=0.005; y=0.18.
Example 1
The embodiment provides a first preparation method of a thermosensitive up-conversion luminescent material, referring to fig. 1, fig. 1 is a flowchart of a preparation method of a thermosensitive up-conversion luminescent material according to the present invention. As shown in fig. 1, the preparation method of the up-conversion luminescent material comprises the following steps:
and step 101, uniformly mixing the raw materials according to the stoichiometric ratio in the chemical formula A 2-2x-2yNd2xMO6 to obtain a first material.
Wherein the raw materials are selected from compounds containing elements in the chemical formula in the forms of oxides, carbonates, oxalates, acetates and hydroxides, and the compounds have the purity of 99.99%.
Further, high purity oxide H 2WO4 can be selected as a raw material.
And 102, calcining the first material to generate a second material.
In this step, in order to control the particle size of the finally produced material, a pre-firing treatment may be performed before the calcination, and grinding may be performed after the pre-firing treatment is completed, and the ground powder may be calcined.
Further, the presintering temperature is 400-600 ℃; the presintering time is 2-30 hours.
Further, the presintering temperature is 500 ℃; the burn-in time was 6 hours.
Wherein the temperature of the calcination is 1000-1400 ℃; the calcination time is 2-10 hours.
Further, the calcination temperature is 1300 ℃; the calcination time was 6 hours.
The container used for presintering and calcining is a ceramic boat or a corundum boat.
And 103, grinding the cooled second material to obtain the thermosensitive up-conversion luminescent material.
In this step, the granularity of the thermosensitive up-conversion luminescent material is 0.2-100 μm. The thermosensitive up-conversion luminescent material has the texture of fluorescent powder.
The grinding may be performed by mechanical ball milling, and the grinding solvent is alcohol.
Example 2
The embodiment provides a second preparation method of the thermosensitive up-conversion luminescent material, which comprises the following steps:
And step 201, weighing the mass corresponding to Y 2O3,Nd2O3,H2WO4 according to the molar ratio of Y 1.995Nd0.005WO6, and grinding the materials with absolute ethyl alcohol for 2-3 times to uniformly mix the materials, thereby obtaining the first material.
And 202, placing the first material in an oven at 80 ℃ for drying for two hours, placing the first material in a high-temperature furnace for sintering for 2-6 hours under the air atmosphere at 1000-1400 o ℃, and naturally cooling to normal temperature to generate a second material.
In practice, 500 o C may be selected in a high temperature furnace for sintering for 6 hours.
In the implementation, the first material may be placed in a ceramic boat or a corundum boat and then placed in a high-temperature furnace.
And 203, grinding the second material with alcohol for 2-3 times, and drying to obtain a third material.
And 204, placing the third material into a corundum boat, placing the corundum boat into a high-temperature furnace, slowly heating to 1300 ℃ under the air atmosphere, preserving heat for 6 hours, and then naturally cooling to obtain the thermosensitive up-conversion luminescent material.
Example 3
The embodiment provides a third preparation method of the thermosensitive up-conversion luminescent material, which comprises the following steps:
And step 301, weighing the mass corresponding to the Lu 2O3,Nd2O3,H2WO4 according to the molar ratio of the Lu 1.995Nd0.005WO6, and grinding the materials with absolute ethyl alcohol for 2-3 times to uniformly mix the materials, thereby obtaining the first material.
Step 302, placing the first material in an oven at 80 ℃ for drying for two hours, placing the first material in a high-temperature furnace for sintering for 2-6 hours under the air atmosphere at 1000-1400 o ℃, and naturally cooling to normal temperature to generate a second material.
In practice, 500 o C may be selected in a high temperature furnace for sintering for 6 hours.
In the implementation, the first material may be placed in a ceramic boat or a corundum boat and then placed in a high-temperature furnace.
And 303, grinding the second material with alcohol for 2-3 times, and drying to obtain a third material.
And 304, placing the third material into a corundum boat, placing the corundum boat into a high-temperature furnace, slowly heating to 1250 ℃ in air or pure oxygen atmosphere, preserving heat for 6 hours, and then naturally cooling to obtain the thermosensitive up-conversion luminescent material.
In a specific implementation, the second material may be placed in a corundum boat and then placed in a high-temperature furnace.
And 304, placing the third material into a clean container, adding deionized water for centrifugal treatment, reserving the third material at the bottom, adding deionized water again for mixing, and performing centrifugal treatment for more than three times to generate a fourth material.
Step 305, baking the fourth material at 100 o C to generate an up-conversion luminescent material.
Therefore, the invention provides a thermosensitive up-conversion luminescent material and a preparation method thereof, wherein the material takes an A2MO6 type material as a matrix of the luminescent material. On one hand, the phonon energy of the material is relatively low, so that the up-conversion luminescence is relatively strong; on the other hand, the material is an oxide, and is excellent in thermal stability and chemical stability. Along with Nd doping, the material rapidly increases the up-conversion luminescence intensity along with the temperature rise in a larger temperature range; therefore, the luminous performance can be regulated and controlled by regulating the temperature. The material has the potential of being applied to high-temperature up-conversion imaging, high-temperature and high-sensitivity temperature sensors, laser anti-counterfeiting and other aspects.
Those of ordinary skill in the art will appreciate that: the drawings are schematic representations of an embodiment only,
The modules or flows in the figures are not necessarily required to practice the invention.
Finally, it should be noted that: 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 of the 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. The application of the thermosensitive up-conversion luminescent material in the temperature sensor is characterized in that the chemical formula of the material is Y 1.995Nd0.005WO6,Lu1.995Nd0.005WO6.
2. The use according to claim 1, wherein the method of preparing the luminescent material comprises:
uniformly mixing the raw materials according to the stoichiometric ratio in the chemical formula Y 1.995Nd0.005WO6,Lu1.995Nd0.005WO6 to obtain a first material;
calcining the first material to generate a second material;
And grinding the cooled second material to obtain the thermosensitive up-conversion luminescent material.
3. The use of claim 2, wherein the step of calcining the first material to produce a second material comprises: the method comprises the steps of firstly carrying out presintering treatment, grinding after the presintering treatment is finished, and calcining the ground powder.
4. The use according to claim 3, wherein the pre-firing temperature is 400 ℃ to 600 ℃; the presintering time is 2-30 hours.
5. The use according to claim 3, wherein the temperature of calcination after calcination is 1000 ℃ to 1400 ℃; the time is 2-10 hours.
6. The use according to claim 3, wherein the particle size of the heat-sensitive up-conversion luminescent material is 0.2-100 μm and the heat-sensitive up-conversion luminescent material has a phosphor texture.
7. Use according to claim 3, wherein the starting material is a compound containing the element of the general chemical formula in the form of an oxide, carbonate, oxalate, acetate, hydroxide, said compound having a purity of 99.99%.
8. The use according to claim 3, wherein the atmosphere of the calcination treatment is air or pure oxygen.
9. The use according to claim 3, wherein the second material is placed in a ceramic or corundum boat for calcination or presintering treatment.
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| GB2448604B (en) * | 2007-04-18 | 2012-05-02 | Bank Of England | Copy-protected documents |
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| GB2448604B (en) * | 2007-04-18 | 2012-05-02 | Bank Of England | Copy-protected documents |
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| Title |
|---|
| Bi3+ 掺杂对Y2WO6: Nd3+ /Yb3+ 的近红外发光的敏化;王婷等;中国稀土学报;第35卷(第3期);第322-328页 * |
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