CN110643363B - Molybdate up-conversion luminescent material and preparation method and application thereof - Google Patents
Molybdate up-conversion luminescent material and preparation method and application thereof Download PDFInfo
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Abstract
The application discloses a molybdate up-conversion luminescent material and a preparation method and application thereof, and relates to the technical field of luminescent materials2‑2x‑ 2yEr2xYb2yMo3O12Wherein Ln is one or more of Y, Lu, La, Gd and Dy, 0<x+y<1. The application solves the problem that the existing up-conversion luminescent material can not realize the regulation and control of the luminescent performance in real time and in situ, and realizes the random regulation and control of the luminescent intensity of the up-conversion luminescent material through temperature.
Description
Technical Field
The application relates to the technical field of luminescent materials, in particular to a molybdate up-conversion luminescent material and a preparation method and application thereof.
Background
A rare earth doped up-conversion luminescent material is a photoluminescent material that is capable of converting multiple longer wavelength photons (low energy) into shorter wavelength photons (high energy). The nonlinear optical characteristic has unique advantages in many fields and high value, and the application mainly comprises a high-performance blue-green laser, biological cell optical imaging, a high-efficiency solar cell, a temperature sensor, 3D imaging and the like.
In general, rare earth doped up-conversion luminescent materials generally consist of three parts: a host material providing a suitable crystal field for the luminescent centers; activators, which absorb energy and produce luminescence by transition; dopant ions capable of absorbing and efficiently transferring energy to an activator and ultimately improving overall luminous efficiency are referred to as sensitizers. Generally, the upconversion luminescence intensity is determined by luminescence absorption and conversion efficiency. The up-conversion light absorption efficiency is mainly determined by the light scattering cross section of the dopant ions, the transparency of the matrix, and the like. The up-conversion efficiency depends on the rare-earth ion excited state dynamics and the interaction between the rare-earth ion excited state dynamics and the matrix.
At present, the regulation and control of luminescence are mainly realized by regulating the types of doped ions, regulating the concentration of the doped ions, regulating and regulating the crystalline phase, the crystal size, the core-shell structure and the like of a matrix. However, the conventional luminescence regulation and control method cannot realize real-time and in-situ luminescence performance regulation and control.
Disclosure of Invention
The embodiment of the application provides the molybdate up-conversion luminescent material and the preparation method and application thereof, solves the problem that the existing up-conversion luminescent material cannot realize real-time and in-situ luminescent property regulation and control, and realizes that the luminescent intensity of the up-conversion luminescent material is regulated and controlled at will through temperature.
In order to achieve the above purpose, the present application mainly provides the following technical solutions:
in one aspect, embodiments of the present application provide a molybdate up-conversion luminescent material having a chemical formula Ln2-2x- 2yEr2xYb2yMo3O12Wherein Ln is one or more of elements Y, Lu, La, Gd and Dy, 0<x+y<1。
Preferably, 0< x.ltoreq.0.1 and 0< y.ltoreq.0.4.
Preferably, x is 0.02 and y is 0.18.
Preferably, the particle size of the molybdate up-conversion luminescent material is 0.2-100 μm.
In another aspect, an embodiment of the present application provides a method for preparing a molybdate up-conversion luminescent material, including the following steps:
an Ln-containing compound, an Er-containing compound, an Yb-containing compound and a Mo-containing compound are mixed according to the following formula: er: yb: mo ═ 2-2x-2 y: 2 x: 2 y: 3, pre-burning and grinding the mixture after the mixture is uniformly mixed, calcining the ground powder, cooling and grinding the powder to obtain the molybdate up-conversion luminescent material; wherein Ln is one or more of elements Y, Lu, La, Gd and Dy, and 0< x + Y < 1.
Preferably, the chemical formula of the molybdate up-conversion luminescent material is Ln2-2x-2yEr2xYb2yMo3O12。
Preferably, 0< x.ltoreq.0.1 and 0< y.ltoreq.0.4.
Preferably, x is 0.02 and y is 0.18.
Preferably, the Ln-containing compound, Er-containing compound, Yb-containing compound and Mo-containing compound are each selected from the corresponding oxides, carbonates, oxalates, acetates or compounds present in the form of hydroxides.
Preferably, the Ln-containing compound, Er-containing compound and Yb-containing compound are each selected from the corresponding oxides; the Mo-containing compound is MoO3。
Preferably, the purity of the Ln-containing compound, Er-containing compound, Yb-containing compound and Mo-containing compound is 99.99%.
Preferably, the particle size of the molybdate up-conversion luminescent material is 0.2-100 μm.
Preferably, the Ln-containing compound, the Er-containing compound, the Yb-containing compound, and the Mo-containing compound are uniformly mixed by mechanical ball milling or a sol-gel method.
Preferably, the pre-sintering temperature is 400-600 ℃, and the pre-sintering time is 2-30 hours.
Preferably, the containers used for the pre-firing and the calcining are ceramic or corundum boats.
Preferably, the calcining atmosphere is air or pure oxygen, the calcining temperature is 800-1000 ℃, and the calcining time is 2-10 hours.
The embodiment of the application also provides application of the molybdate up-conversion luminescent material in the fields of high-temperature up-conversion imaging, temperature sensors and laser anti-counterfeiting.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
the molybdate up-conversion luminescent material provided by the application is prepared by adding Ln2Mo3O12Being luminescent materialsThe substrate is doped by erbium ytterbium, so that the performance of light attenuation of the conventional up-conversion luminescent material when the temperature is increased is broken, the performance of light enhancement of the material when the temperature is increased is realized, the position of the luminescent peak of the material is not changed along with the change of the luminescent intensity, but the luminescent intensity is rapidly enhanced along with the temperature increase. The luminescent material creates good conditions for regulating and controlling the luminescent performance by regulating the temperature, and 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.
Drawings
FIG. 1 shows a luminescent material Lu obtained in example 1 of the present application2-0.4Er0.04Yb0.36Mo3O12The normal temperature luminescence spectrum of (1);
FIG. 2 shows a luminescent material Lu obtained in example 1 of the present application2-0.4Er0.04Yb0.36Mo3O12Luminescence spectra at different temperatures;
FIG. 3 shows a luminescent material Lu obtained in example 1 of the present application2-0.4Er0.04Yb0.36Mo3O12Graph of luminescence intensity at specific luminescence peaks (524 and 560nm) as a function of temperature;
FIG. 4 shows a luminescent material Y obtained in example 2 of the present application2-0.4Er0.04Yb0.36Mo3O12The normal temperature luminescence spectrum of (1);
FIG. 5 shows a luminescent material Y obtained in example 2 of the present application2-0.4Er0.04Yb0.36Mo3O12Up-converting luminescence spectra at different temperatures;
FIG. 6 shows a luminescent material Y obtained in example 2 of the present application2-0.4Er0.04Yb0.36Mo3O12Spectra of intensity at different luminescence peak positions as a function of temperature.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention thereto.
The embodiment of the application provides molybdenumAn acid salt up-conversion luminescent material with a chemical formula of Ln2-2x- 2yEr2xYb2yMo3O12Wherein Ln is one or more of elements Y, Lu, La, Gd and Dy, 0<x+y<1. Preferably, 0<x≤0.1，0<y is less than or equal to 0.4. More preferably, x is 0.02 and y is 0.18.
The particle size of the molybdate up-conversion luminescent material is 0.2-100 mu m.
The molybdate up-conversion luminescent material provided by the embodiment of the application is prepared by adding Ln2Mo3O12The erbium-ytterbium co-doped erbium-ytterbium doped erbium-ytterbium doped erbium-ytterbium doped erbium-ytterbium doped erbium-ytterbium doped erbium-ytterbium doped erbium-ytterbium doped erbium-ytterbium doped erbium-ytterbium doped erbium-ytterbium doped erbium-ytterbium doped erbium-ytterbium doped erbium-ytterbium doped erbium-doped erbium-doped erbium. The luminescent material creates good conditions for regulating and controlling the luminescent performance by regulating the temperature, and 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.
The embodiment of the application also provides a preparation method of the molybdate up-conversion luminescent material, which comprises the following steps:
an Ln-containing compound, an Er-containing compound, an Yb-containing compound and a Mo-containing compound are mixed according to the following formula: er: yb: mo ═ 2-2x-2 y: 2 x: 2 y: 3, pre-burning and grinding the mixture after the mixture is uniformly mixed, calcining the ground powder, cooling and grinding the powder to obtain the molybdate up-conversion luminescent material; wherein Ln is one or more of elements Y, Lu, La, Gd and Dy, and 0< x + Y < 1.
Preferably, 0< x.ltoreq.0.1, 0< y.ltoreq.0.4. More preferably, x is 0.02 and y is 0.18.
The chemical general formula of the molybdate up-conversion luminescent material is Ln2-2x-2yEr2xYb2yMo3O12。
Wherein the Ln-containing compound, the Er-containing compound, the Yb-containing compound and the Mo-containing compound are selected from the corresponding oxides, carbonates, oxalates, vinegarAcid salts or compounds in the form of hydroxides. Preferably, the Ln-containing compound, the Er-containing compound and the Yb-containing compound are each selected from the corresponding oxides; the Mo-containing compound is MoO3(ii) a And the purities of the raw materials are all 99.99%.
In the preparation method, the Ln-containing compound, the Er-containing compound, the Yb-containing compound and the Mo-containing compound are uniformly mixed by a mechanical ball milling method or a sol-gel method.
In the preparation method, the presintering temperature is 400-600 ℃, and the presintering time is 2-30 hours.
In the preparation method, the containers used for pre-burning and calcining are ceramic boats or corundum boats.
In the preparation method, the calcining atmosphere is air or pure oxygen, the calcining temperature is 800-1000 ℃, and the calcining time is 2-10 hours.
The molybdate up-conversion luminescent material provided by the embodiment of the application can be applied to the fields of high-temperature up-conversion imaging, temperature sensors and laser anti-counterfeiting.
The following examples illustrate the preparation of the molybdate up-conversion phosphor.
Example 1
(1) According to the chemical formula Lu2-0.4Er0.04Yb0.36Mo3O12The stoichiometric ratio of Lu, Er, Yb and Mo is measured2O3，Yb2O3，MoO3And Er2O3The purity of the raw materials is 99.99 percent according to the corresponding mass, and the raw materials are ground for 2 to 3 times by absolute ethyl alcohol to be uniformly mixed;
(2) placing the ground sample in an oven at 80 ℃ for two hours for drying, then placing the sample in a corundum boat, placing the corundum boat with the sample in a high-temperature furnace for presintering, preserving heat for 6 hours at 500 ℃ in air atmosphere, and then naturally cooling to normal temperature;
(3) taking out the sample from the high-temperature furnace, grinding the sample for 2 to 3 times by using alcohol, and drying the sample;
(4) and putting the dried sample into a corundum boat, putting the corundum boat into a high-temperature furnace for calcining, slowly heating to 900 ℃ in the air atmosphere, preserving the temperature for 6 hours, naturally cooling, and grinding to obtain the molybdate up-conversion luminescent material.
The detection shows that the particle size of the prepared molybdate up-conversion luminescent material is 0.2-100 mu m.
The molybdate up-conversion luminescent material prepared in example 1 was subjected to a luminescence property test to obtain luminescence spectra shown in fig. 1, 2 and 3.
FIG. 1 shows a luminescent material Lu2-0.4Er0.04Yb0.36Mo3O12The normal temperature luminescence spectrogram under the excitation of 980nm laser can be seen from figure 1, and the luminescent material Lu is obtained under the normal temperature condition2-0.4Er0.04Yb0.36Mo3O12Emitting green light under the irradiation of near infrared laser;
FIG. 2 shows the luminescent material Lu under different temperature conditions2-0.4Er0.04Yb0.36Mo3O12A luminescence spectrum under 980nm laser excitation; as can be seen from FIG. 2, the luminescent material Lu2-0.4Er0.04Yb0.36Mo3O12Does not change with the increase of temperature, but the luminous intensity increases with the increase of temperature.
FIG. 3 shows a luminescent material Lu2-0.4Er0.04Yb0.36Mo3O12Graph of luminescence intensity at specific luminescence peaks (524 and 560nm) as a function of temperature; as can be seen from FIG. 3, the luminescent material Lu2-0.4Er0.04Yb0.36Mo3O12The luminous enhancement quantity at different luminous peak positions has larger difference, and the luminous intensity with the peak position of 524nm changes most obviously along with the temperature.
As can be seen from the above, the luminescent material Lu2-0.4Er0.04Yb0.36Mo3O12Has the property of light enhancement at the temperature rise which is different from that of the conventional material, the position of the luminescence peak of the material does not change with the change of the luminescence intensity, but the luminescence intensity rapidly increases with the temperature rise. Therefore, the molybdate up-conversion luminescent material prepared in the embodiment can be up-converted at will by temperature controlThe luminous intensity of the luminescent material is changed, and real-time and in-situ regulation and control of the luminous performance are realized.
Example 2
(1) According to the formula Y2-0.4Er0.04Yb0.36Mo3O12In the stoichiometric ratio of Y, Er, Yb and Mo, weighing Y2O3，Yb2O3，MoO3And Er2O3The purity of the raw materials is 99.99 percent according to the corresponding mass, and the raw materials are ground for 2 to 3 times by absolute ethyl alcohol to be uniformly mixed.
(2) And placing the ground sample in an oven at 80 ℃ for two hours for drying, then placing the sample in a corundum boat, placing the corundum boat with the sample in a high-temperature furnace for presintering, preserving the heat for 6 hours at 500 ℃ in the air atmosphere, and then naturally cooling to the normal temperature.
(3) Taking out the sample from the high temperature furnace, grinding for 2-3 times by alcohol, and drying.
(4) And putting the dried sample into a corundum boat, putting the corundum boat into a high-temperature furnace for calcining, slowly heating to 950 ℃ in the air atmosphere, preserving the temperature for 6 hours, naturally cooling, and grinding to obtain the molybdate up-conversion luminescent material.
The detection shows that the particle size of the prepared molybdate up-conversion luminescent material is 0.2-100 mu m.
The molybdate up-conversion luminescent material prepared in example 2 was subjected to a luminescence property test to obtain luminescence spectra shown in fig. 4, 5 and 6.
FIG. 4 shows a luminescent material Y2-0.4Er0.04Yb0.36Mo3O12The normal temperature luminescence spectrogram under 980nm laser excitation can be seen from FIG. 4, and the luminescent material Y is obtained under normal temperature2-0.4Er0.04Yb0.36Mo3O12Emitting green light under the irradiation of near infrared laser;
FIG. 5 shows a luminescent material Y under different temperature conditions2-0.4Er0.04Yb0.36Mo3O12A luminescence spectrum under 980nm laser excitation; as can be seen from FIG. 5, the luminescent material Y2-0.4Er0.04Yb0.36Mo3O12Does not change with the increase of temperature, but the luminous intensity increases with the increase of temperature.
FIG. 6 shows a luminescent material Y2-0.4Er0.04Yb0.36Mo3O12Graph of luminescence intensity at specific luminescence peaks (524 and 560nm) as a function of temperature; as can be seen from FIG. 6, the luminescent material Y2-0.4Er0.04Yb0.36Mo3O12The luminous enhancement quantity at different luminous peak positions has larger difference, and the luminous intensity with the peak position of 524nm changes most obviously along with the temperature.
As can be seen from the above, the luminescent material Y2-0.4Er0.04Yb0.36Mo3O12Has the property of light enhancement at the temperature rise which is different from that of the conventional material, the position of the luminescence peak of the material does not change with the change of the luminescence intensity, but the luminescence intensity rapidly increases with the temperature rise. Therefore, the molybdate up-conversion luminescent material prepared by the embodiment can realize real-time and in-situ luminescent property regulation and control by randomly regulating and controlling the luminescent intensity of the up-conversion luminescent material through temperature.
Experiments prove that the chemical general formula is Ln2-2x-2yEr2xYb2yMo3O12When Ln is one or more of La, Gd and Dy, the molybdate up-conversion luminescent material of (1) also has a property that the position of the luminescence peak of the material does not change with the change of the luminescence intensity, but the luminescence intensity rapidly increases with the increase of the temperature.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (6)
1. A molybdate up-conversion luminescent material is characterized in that the molybdate up-conversion luminescent material is formed by esterificationHas a chemical general formula of Ln2-2x-2yEr2xYb2yMo3O12Wherein Ln is element Y or Lu, 0<x+y<1；
The preparation method of the molybdate up-conversion luminescent material comprises the following steps:
an Ln-containing compound, an Er-containing compound, an Yb-containing compound and a Mo-containing compound are mixed according to the following formula: er: yb: mo = (2-2x-2 y): 2 x: 2 y: 3, pre-burning and grinding the mixture after the mixture is uniformly mixed, calcining the ground powder, cooling and grinding the powder to obtain the molybdate up-conversion luminescent material; wherein Ln is element Y or Lu, 0< x + Y < 1; x =0.02 and y = 0.18.
2. The molybdate up-conversion phosphor of claim 1, wherein the molybdate up-conversion phosphor has a particle size of 0.2 to 100 μm.
3. The molybdate up-conversion luminescent material of claim 1, wherein the Ln-containing compound, the Er-containing compound, the Yb-containing compound, and the Mo-containing compound are each selected from the corresponding oxides, carbonates, oxalates, acetates, or compounds in the form of hydroxides.
4. The molybdate up-conversion luminescent material of claim 3, wherein said Ln-containing compound, Er-containing compound, and Yb-containing compound are each selected from the group consisting of the corresponding oxides; the Mo-containing compound is MoO3。
5. The molybdate up-conversion luminescent material of claim 1, wherein the Ln-containing compound, the Er-containing compound, the Yb-containing compound and the Mo-containing compound are all 99.99% pure.
6. Use of a molybdate up-conversion luminescent material, wherein the molybdate up-conversion luminescent material is used in the fields of high-temperature up-conversion imaging, temperature sensors and laser anti-counterfeiting according to any one of claims 1 to 5.
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| A review on nanostructured glass ceramics for promising application in optical thermometry;Jiasong Zhong et al.;《Journal of Alloys and Compounds》;20180530;第763卷;第34-48页 * |
| M = W, Mo ; Ln = Yb/Er, Yb/Tm) hierarchical microcrystals: Hydrothermal synthesis and up-conversion luminescence.《Optical Materials》.2013,第36卷第602-607页. * |
| Y2W3O12和Yb2W3O12的制备及其负热膨胀性能;黄远辉等;《中国钨业》;20081231;第23卷(第5期);第26-29页 * |
| You Zhou et al..Self-assembled RE2(MO4)3:Ln3+ (RE = Y, La, Gd, Lu * |
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