阅读说明：本技术 一种温度敏感发光材料及其制备方法 (Temperature-sensitive luminescent material and preparation method thereof ) 是由 张粟 李成宇 张晓伟 庞然 姜丽宏 李达 张洪杰 于 2021-09-27 设计创作，主要内容包括：本发明提供了一种温度敏感发光材料,分子式为：A-(2-x)Sm-(x)O-(3)·yTa-(2)O-(5)·zNb-(2)O-(5)；其中,x＝0.001～0.2,y＝0～0.9,z＝0.001～1；A为Gd、Y、Lu与Sc中的一种或多种。本发明提供的温度敏感发光材料以铌钽酸盐复合氧化物为基质,以稀土Sm离子为激活剂。所合成的发光材料能够被紫外光源以及可见光蓝光光源有效激发,在77～500K温度范围内具有优异的光学测温特性,显示出可调的多色发射以及良好的稳定性,且无毒无害,无放射性,不会对人体和环境产生危害。同时,其制备工艺简单,生产效率高,易研磨,便于工业化生产,具有良好的工业应用前景。(The invention provides a temperature-sensitive luminescent material, which has the molecular formula: a. the 2‑x Sm x O 3 ·yTa 2 O 5 ·zNb 2 O 5 (ii) a Wherein x is 0.001-0.2, y is 0-0.9, and z is 0.001-1; a is one or more of Gd, Y, Lu and Sc. The temperature-sensitive luminescent material provided by the invention takes niobium tantalate composite oxide as a matrix and takes rare earth Sm ions as an activator. The synthesized luminescent material can be effectively excited by an ultraviolet light source and a visible light blue light source, has excellent optical temperature measurement characteristics within the temperature range of 77-500K, shows adjustable multicolor emission and good stability, is non-toxic, harmless and non-radioactive, and does not harm human bodies and the environment. Meanwhile, the preparation method is simple in preparation process, high in production efficiency, easy to grind, convenient for industrial production and good in industrial application prospect.)

1. A temperature-sensitive luminescent material, characterized by the molecular formula:

A_2-xSm_xO₃·yTa₂O₅·zNb₂O₅；

wherein x is 0.001-0.2, y is 0-0.9, and z is 0.001-1;

a is one or more of Gd, Y, Lu and Sc.

2. The temperature-sensitive luminescent material according to claim 1, wherein the molecular formula is:

Y_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅；Y_2-0.01Sm_0.01O₃·0.7Ta₂O₅·0.3Nb₂O₅；

Y_2-0.01Sm_0.01O₃·0.8Ta₂O₅·0.2Nb₂O₅；Y_2-0.01Sm_0.01O₃·0.9Ta₂O₅·0.1Nb₂O₅；

Y_2-0.02Sm_0.02O₃·0.7Ta₂O₅·0.3Nb₂O₅；Y_2-0.03Sm_0.03O₃·0.8Ta₂O₅·0.2Nb₂O₅；

Y_2-0.03Sm_0.03O₃·0.7Ta₂O₅·0.3Nb₂O₅；Y_2-0.03Sm_0.03O₃·0.9Ta₂O₅·0.1Nb₂O₅；

Y_2-0.04Sm_0.04O₃·0.7Ta₂O₅·0.3Nb₂O₅；Lu_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅；

Sc_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅；Gd_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅。

3. a method for preparing a temperature-sensitive luminescent material, comprising:

s1) mixing the A source compound, the samarium source compound, the tantalum source compound and the niobium source compound to obtain a mixture;

s2) roasting the mixture to obtain the temperature-sensitive luminescent material.

4. The method according to claim 3, wherein the atmosphere of the firing is air, nitrogen, argon or oxygen;

the roasting temperature is 1000-1600 ℃; the roasting time is 0.5-24 hours.

5. The method according to claim 3, wherein the A source compound is selected from one or more of an oxide, a chloride, a carbonate, silver nitrate, an oxalate, a citrate and an acetate of A.

6. A method of producing samarium in accordance with claim 3 wherein the samarium source compound is selected from one or more of samarium oxide, chloride, carbonate and nitrate.

7. The method according to claim 3, wherein the tantalum source compound is one or more selected from the group consisting of simple metal elements, oxides, chlorides, hydroxides, and nitrates of tantalum.

8. The method according to claim 3, wherein the niobium source compound is one or more selected from the group consisting of elemental metal, oxide, hydroxide and nitrate of niobium.

9. The method of claim 3, comprising:

A) mixing the A source compound, the samarium source compound, the tantalum source compound and the niobium source compound, and calcining for the first time under a protective atmosphere to obtain a primary product;

B) and carrying out secondary roasting on the primary product under a protective atmosphere to obtain the temperature-sensitive luminescent material.

10. Use of the temperature-sensitive luminescent material according to any one of claims 1 to 2 or the temperature-sensitive luminescent material prepared by the preparation method according to any one of claims 3 to 9 in an optical temperature sensor.

Technical Field

The invention relates to the technical field of photoluminescence materials, in particular to a temperature-sensitive luminescent material and a preparation method thereof.

Background

A photoluminescent material is a material that can generate an electronic transition under the excitation of energy of external light radiation such as ultraviolet light, visible light, infrared light, or the like, thereby generating a light emission phenomenon. It undergoes roughly three main processes of absorption, energy transfer and light emission, all of which are susceptible to temperature. The latest research results show that the temperature-sensitive luminescent material has important application value in the fields of temperature sensing, temperature indication and measurement.

The rare earth ion activated photoluminescence material has important application in the fields of solid state illumination, display, laser crystal, optical fiber communication and the like. However, the luminescence property of rare earth ions is susceptible to temperature, and different temperatures can cause the spectrum of the material to change significantly. The property can be used as a temperature sensing material and can be used in the fields of temperature detection, temperature indication and the like. The temperature detection by using the light emitting mode has many advantages, such as electromagnetic interference resistance and radio frequency interference resistance, can work in severe environments such as high temperature and radiation, and has high sensitivity and resolution, safety, no toxicity and wide application range.

At present, few research reports on temperature-sensitive luminescent materials exist, along with the progress of optical temperature sensing technology and the expansion of application fields, the temperature-sensitive luminescent materials with excellent performance are still very deficient, and the development of the temperature-sensitive luminescent materials has important application significance.

Disclosure of Invention

In view of the above, the technical problem to be solved by the present invention is to provide a temperature-sensitive luminescent material and a preparation method thereof, which is sensitive to temperature response.

In order to solve the technical problems, the invention provides a temperature-sensitive luminescent material, which has the molecular formula:

A_2-xSm_xO₃·yTa₂O₅·zNb₂O₅；

wherein x is 0.001-0.2, preferably 0.005-0.1, more preferably 0.005-0.05, still more preferably 0.005-0.04, and most preferably 0.01-0.03; in some embodiments provided herein, the x is preferably 0.02; in other embodiments provided herein, x is preferably 0.01, 0.03, or 0.04.

y is 0-0.9, preferably 0.5-0.9, more preferably 0.7-0.9; in some embodiments provided herein, y is preferably 0.8; in other embodiments provided herein, y is preferably 0.9 or 0.7.

z is 0.001-1, preferably 0.05-0.5, more preferably 0.1-0.3; in some embodiments provided herein, y is preferably 0.2; in other embodiments provided herein, y is preferably 0.1 or 0.3.

A is one or more of Gd, Y, Lu and Sc; more preferably Y.

In some embodiments of the present invention, the temperature-sensitive luminescent material has a formula of:

Y_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅；Y_2-0.01Sm_0.01O₃·0.7Ta₂O₅·0.3Nb₂O₅；

Y_2-0.01Sm_0.01O₃·0.8Ta₂O₅·0.2Nb₂O₅；Y_2-0.01Sm_0.01O₃·0.9Ta₂O₅·0.1Nb₂O₅；

Y_2-0.02Sm_0.02O₃·0.7Ta₂O₅·0.3Nb₂O₅；Y_2-0.03Sm_0.03O₃·0.8Ta₂O₅·0.2Nb₂O₅；

Y_2-0.03Sm_0.03O₃·0.7Ta₂O₅·0.3Nb₂O₅；Y_2-0.03Sm_0.03O₃·0.9Ta₂O₅·0.1Nb₂O₅；

Y_2-0.04Sm_0.04O₃·0.7Ta₂O₅·0.3Nb₂O₅；Lu_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅；

Sc_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅；Gd_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅。

the temperature sensitive range of the temperature sensitive luminescent material provided by the invention is 77K-500K.

Niobate and tantalate as substrate materials have outstanding properties of high thermal stability, high environmental stability, low toxicity, low phonon energy and the like. Mixing NbO₄ ^3-The radical doped in tantalate can also become effective luminescent center to raise the luminous efficiency. The temperature sensitive luminescent material provided by the invention is represented by Y₂O₃、Ta₂O₅And Nb₂O₅Sm as a matrix³⁺As an activator, a composite oxide phosphor is obtained which can be used as a temperature-sensitive luminescent material, A_2-xSm_xO₃·yTa₂O₅·zNb₂O₅. By A_2-xSm_xO₃·yTa₂O₅·zNb₂O₅The luminous intensity changes with the temperature and is based on NbO₄ ^3-Group Sm³⁺The luminescent material has sensitive response of the luminous intensity to temperature, good relative sensitivity, large color gamut variation, chemical and physical stability, and is suitable for high-precision optical temperature sensors; meanwhile, the temperature-sensitive luminescent material has the advantages of simple preparation process, high production efficiency, easy grinding, no toxic metal, convenience for industrial production and no harm to human bodies and environment.

The invention also provides a preparation method of the temperature-sensitive luminescent material, which comprises the following steps:

s1) mixing the A source compound, the samarium source compound, the tantalum source compound and the niobium source compound to obtain a mixture;

s2) roasting the mixture to obtain the temperature-sensitive luminescent material.

In the preferred embodiment of the present invention, the atmosphere for calcination is air, nitrogen, argon or oxygen.

Preferably, the roasting temperature is 1000-1600 ℃; the roasting time is 0.5-24 hours.

The a source compound is a compound containing an a element well known to those skilled in the art, and is not particularly limited, and is preferably one or more of an oxide, a chloride, a carbonate, silver nitrate, an oxalate, a citrate, and an acetate of a. For example, where A is Y, the A source can be yttria Y₂O₃Yttrium nitrate Y (NO)₃)₃·6H₂O, and the like.

In the present invention, Sm is an activator ion, and the samarium source compound is a samarium source compound known to those skilled in the art, and is not particularly limited, and preferably, the samarium source compound is one or more selected from samarium oxide, chloride, carbonate and nitrate, and most preferably Sm oxide₂O₃。

The tantalum source compound is not particularly limited as long as it is a compound containing Ta element well known to those skilled in the art, and it is preferable in the present invention that the tantalum source compound is selected from one or more of simple metal, oxide, chloride, hydroxide and nitrate of tantalum, and more preferably, Ta oxide, Ta₂O₅。

The Nb source compound is not particularly limited as long as it is a Nb-containing compound known to those skilled in the art, and preferably, the Nb source compound is one or more selected from the group consisting of a metal simple substance, an oxide, a hydroxide and a nitrate of niobium, and more preferably, an oxide of Nb, Nb₂O₅。

In the present invention, the molar ratio of the a source compound, the samarium source compound, the tantalum source compound, and the niobium source compound is preferably (0.8 to 0.999): (0.001-0.20): (0-0.99): (0.001-1), more preferably (0.8-0.999): (0.001-0.20): (0.7-0.99): (0.01-0.30).

Preferably, the preparation method specifically comprises the following steps:

A) mixing the A source compound, the samarium source compound, the tantalum source compound and the niobium source compound, and calcining for the first time under a protective atmosphere to obtain a primary product;

B) and carrying out secondary roasting on the primary product under a protective atmosphere to obtain the temperature-sensitive luminescent material.

In the invention, preferably, the A source compound, the samarium source compound and the tantalum source compound are mixed with the niobium source compound.

After mixing, grinding is preferably carried out, and then primary calcination is carried out under a protective atmosphere; the protective atmosphere is not particularly limited as long as it is known to those skilled in the art, and air is preferred in the present invention; the temperature of the primary calcination is preferably 1100-1600 ℃, more preferably 1250-1500 ℃, and further preferably 1350 ℃; the time of the primary calcination is preferably 5-20 h, more preferably 10-20 h, and still more preferably 16 h.

After primary calcination, preferably cooling and grinding to obtain a primary product; the grinding apparatus of the present invention is not particularly limited, and may be a crushing mill and a grinding machine well known to those skilled in the art.

Carrying out secondary roasting on the primary product under a protective atmosphere; the protective atmosphere is not particularly limited as long as it is known to those skilled in the art, and in the present invention, the secondary baking is performed in a certain atmosphere. In the present invention, the atmosphere is preferably nitrogen, oxygen, argon and air, most preferably air; the temperature of the secondary roasting is preferably 1100-1600 ℃, more preferably 1250-1500 ℃, and further preferably 1350 ℃; the secondary roasting time is preferably 5-20 hours, more preferably 8-15 hours, and further preferably 10 hours. The apparatus used in the primary calcination and the secondary calcination is not particularly limited, and a high temperature furnace known to those skilled in the art may be used. In the invention, the primary calcination promotes the formation of a crystal phase, so that the product has primary luminescence property, and the secondary calcination can ensure that the crystal phase is more complete and the luminescence property is enhanced, so that high-efficiency fluorescence is emitted.

And after secondary roasting, preferably cooling and grinding, obtaining the temperature-sensitive luminescent material.

The luminous intensity of the temperature-sensitive luminescent material provided by the invention is sensitive to temperature response, and meanwhile, the temperature-sensitive luminescent material has large color gamut variation and chemical and physical stability, and is suitable for high-precision optical temperature sensors.

Based on the above, the invention provides the application of the temperature-sensitive luminescent material or the temperature-sensitive luminescent material prepared by the preparation method in an optical temperature sensor.

Compared with the prior art, the invention provides a temperature-sensitive luminescent material, which has the molecular formula: a. the_2-xSm_xO₃·yTa₂O₅·zNb₂O₅(ii) a Wherein x is 0.001-0.2, y is 0-0.9, and z is 0.001-1; a is one or more of Gd, Y, Lu and Sc.

The temperature-sensitive luminescent material provided by the invention takes niobium tantalate composite oxide as a matrix and takes rare earth Sm ions as an activator. The synthesized luminescent material can be effectively excited by an ultraviolet light source and a visible light blue light source, has excellent optical temperature measurement characteristics within the temperature range of 77-500K, shows adjustable multicolor emission and good stability, is non-toxic, harmless and non-radioactive, and does not harm human bodies and the environment. Meanwhile, the preparation method is simple in preparation process, high in production efficiency, easy to grind, convenient for industrial production and good in industrial application prospect.

Drawings

FIG. 1 is a graph of an emission spectrum of a temperature-sensitive luminescent material obtained in example 1 of the present invention under 230nm excitation;

FIG. 2 is a graph of an emission spectrum and a corresponding excitation spectrum of a temperature-sensitive luminescent material obtained in example 1 of the present invention under the excitation of 262nm ultraviolet light;

FIG. 3 is a graph showing an emission spectrum and a corresponding excitation spectrum of a temperature-sensitive luminescent material obtained in example 1 of the present invention under excitation by 405nm violet light;

FIG. 4 is a chart of an emission spectrum of a temperature-sensitive luminescent material obtained in example 4 of the present invention under the excitation of 262nm ultraviolet light;

FIG. 5 is a chart of an emission spectrum of a temperature-sensitive luminescent material obtained in example 7 of the present invention under the excitation of 262nm ultraviolet light;

fig. 6 is a graph of emission spectra of the temperature-sensitive luminescent material obtained in example 1 of the present invention under the excitation of 255nm ultraviolet light at different temperatures.

Detailed Description

In order to further illustrate the present invention, the following will describe the temperature-sensitive luminescent material and the preparation method thereof in detail with reference to the examples.

The reagents used in the following examples are all commercially available.

Example 1 x 0.02, y 0.8, and z 0.2

Get Y₂O₃、Sm₂O₃、Ta₂O₅、Nb₂O₅And mixing the components according to a molar ratio of 0.99:0.01:0.8:0.2, and fully and uniformly grinding to obtain a mixture. Putting the mixture into a corundum crucible, putting the corundum crucible filled with the mixture into a high-temperature furnace, calcining for 16h at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10h at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain the temperature-sensitive luminescent material Y_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅。

The excitation spectrum and the emission spectrum of the temperature-sensitive luminescent material obtained in example 1 were analyzed, and the results are shown in fig. 1 to 3. Wherein, fig. 1 is an emission spectrum of the temperature-sensitive luminescent material provided in embodiment 1 of the present invention under excitation of 230nm, as can be seen from fig. 2, the temperature-sensitive luminescent material can be effectively excited by ultraviolet light of 262nm, the emission spectrum thereof is composed of broadband emission and linear emission, and the broadband emission peak is located near 400nmAscribed to NbO₄ ^3-Has a linear emission peak of Sm³⁺The characteristic emission of (1); fig. 3 shows an emission spectrum of the temperature-sensitive luminescent material provided in embodiment 1 of the present invention after excitation of 405nm blue light, and as can be seen from fig. 3, the luminescent color of the temperature-sensitive luminescent material is orange red, which is classified as Sm³⁺4f → 4f transition of the ion. FIG. 6 shows the emission spectra of the sample of example 1 at different temperatures. The test results showed that the maximum relative sensitivity obtained in example 1 was 1.151%.

Example 2 x 0.02, y 0.8, z 0.2

Taking Y (NO)₃)₃、Sm₂O₃、Ta₂O₅、Nb₂O₅Mixing according to the molar ratio of 1.98:0.01:0.8:0.2, and fully and uniformly grinding to obtain a mixture. Putting the mixture into a corundum crucible, putting the corundum crucible filled with the mixture into a high-temperature furnace, calcining for 16h at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10h at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain the temperature-sensitive luminescent material Y_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅。

The temperature-sensitive luminescent material obtained in example 2 was subjected to excitation spectrum and emission spectrum tests. The temperature-sensitive luminescent material can be effectively excited by ultraviolet light and blue light. The emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 2 of the invention consists of broadband emission and linear emission under the excitation of ultraviolet light, the broadband emission peak is positioned near 400nm and belongs to charge transfer of NbO43-, and the linear emission peak is Sm³⁺The characteristic emission of (1); the emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 2 of the invention after being excited by 405nm blue light is orange red, and the luminescent color of the temperature-sensitive luminescent material belongs to Sm³⁺4f → 4f transition of the ion.

Example 3 x 0.02, y 0.8, z 0.2

Get Y₂(CO₃)₃、Sm₂O₃、Ta₂O₅、Nb₂O₅Mixing according to a molar ratio of 0.99:0.01:0.8:0.2, putting the mixture into a corundum crucible, putting the corundum crucible filled with the mixture into a high-temperature furnace, calcining for 16 hours at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10h at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain the temperature-sensitive luminescent material Y_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅。

The temperature-sensitive luminescent material obtained in example 3 was subjected to excitation spectrum and emission spectrum tests. The temperature-sensitive luminescent material can be effectively excited by ultraviolet light and blue light. The emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 3 of the invention consists of broadband emission and linear emission under the excitation of ultraviolet light, and the broadband emission peak is positioned near 400nm and belongs to NbO₄ ^3-Has a linear emission peak of Sm³⁺The characteristic emission of (1); the emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 3 of the invention after excitation of 405nm blue light is orange red, and the luminescent color of the temperature-sensitive luminescent material belongs to Sm³⁺4f → 4f transition of the ion.

Example 4 x 0.01, y 0.7, z 0.3

Get Y₂O₃、Sm₂O₃、Ta₂O₅、Nb₂O₅Mixing according to a molar ratio of 0.995:0.005:0.7:0.3, putting the mixture into a corundum crucible, putting the corundum crucible filled with the mixture into a high-temperature furnace, calcining at 1350 ℃ for 16h in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucible, placing the corundum crucible into a high-temperature furnace, calcining the corundum crucible at 1350 ℃ for 10 hours in the presence of air, and naturally cooling the corundum crucible to room temperatureTaking out, crushing and grinding uniformly to obtain the temperature sensitive luminescent material Y_2-0.01Sm_0.01O₃·0.7Ta₂O₅·0.3Nb₂O₅。

FIG. 4 is an emission spectrum of a temperature-sensitive luminescent material excited by 262nm ultraviolet light according to embodiment 4 of the present invention, where the emission spectrum includes a broadband emission peak near 400nm and a linear emission, and the broadband emission peak is attributed to NbO₄ ^3-Has a linear emission peak of Sm³⁺The emission intensity is less than that of the example 1 under the excitation of 262nm ultraviolet light; the emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 4 of the invention after excitation of 405nm blue light is orange red, and the luminescent color of the temperature-sensitive luminescent material belongs to Sm³⁺4f → 4f transition of the ion.

Example 5 x 0.01, y 0.8, z 0.2

Get Y₂O₃、Sm₂O₃、Ta₂O₅、Nb₂O₅Mixing according to a molar ratio of 0.995:0.005:0.8:0.2, putting the mixture into a corundum crucible, putting the corundum crucible filled with the mixture into a high-temperature furnace, calcining at 1350 ℃ for 16h in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10h at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain the temperature-sensitive luminescent material Y_2-0.01Sm_0.01O₃·0.8Ta₂O₅·0.2Nb₂O₅。

The temperature-sensitive luminescent material obtained in example 5 was subjected to excitation spectrum and emission spectrum tests. The temperature sensitive luminescent material can be effectively excited by ultraviolet light and purple light. The temperature-sensitive luminescent material provided by embodiment 5 of the invention has an emission spectrum consisting of broadband emission and linear emission under the excitation of ultraviolet light, wherein a broadband emission peak is positioned near 400nm and belongs to NbO₄ ^3-Has a linear emission peak of Sm³⁺Is characterized in thatPerforming emission; the emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 5 of the invention after excitation of 405nm blue light is orange red, and the luminescent color of the temperature-sensitive luminescent material belongs to Sm³⁺4f → 4f transition of the ion.

Example 6 x 0.01, y 0.9, and z 0.1

Get Y₂O₃、Sm₂O₃、Ta₂O₅、Nb₂O₅Mixing according to a molar ratio of 0.995:0.005:0.9:0.1, putting the mixture into a corundum crucible, putting the corundum crucible filled with the mixture into a high-temperature furnace, calcining at 1350 ℃ for 16h in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10h at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain the temperature-sensitive luminescent material Y_2-0.01Sm_0.01O₃·0.9Ta₂O₅·0.1Nb₂O₅。

The temperature-sensitive luminescent material obtained in example 6 was subjected to excitation spectrum and emission spectrum tests. The temperature sensitive luminescent material can be effectively excited by ultraviolet light and purple light. The temperature-sensitive luminescent material provided by embodiment 6 of the invention has an emission spectrum consisting of broadband emission and linear emission under the excitation of ultraviolet light, wherein a broadband emission peak is positioned near 400nm and belongs to NbO₄ ^3-Has a linear emission peak of Sm³⁺The characteristic emission of (1); the emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 6 of the invention after excitation of 405nm blue light is orange red, and the luminescent color of the temperature-sensitive luminescent material belongs to Sm³⁺4f → 4f transition of the ion.

Example 7 x 0.02, y 0.7, and z 0.3

Get Y₂O₃、Sm₂O₃、Ta₂O₅、Nb₂O₅Mixing according to a molar ratio of 0.99:0.01:0.7:0.3, placing the mixture into a corundum crucible, and placing the corundum crucible filled with the mixture into a corundum crucibleCalcining in a warm furnace at 1350 ℃ for 16h in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10h at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain the temperature-sensitive luminescent material Y_2-0.02Sm_0.02O₃·0.7Ta₂O₅·0.3Nb₂O₅。

FIG. 5 is an emission spectrum of a temperature-sensitive luminescent material excited by 262nm ultraviolet light according to embodiment 7 of the present invention, where the emission spectrum includes a broadband emission peak near 400nm and a linear emission, and the broadband emission peak is attributed to NbO₄ ^3-Has a linear emission peak of Sm³⁺The characteristic emission of (1); the emission spectrum of the temperature-sensitive luminescent material provided by embodiment 7 of the invention after excitation by 405nm violet light is orange red, and the luminescent color of the temperature-sensitive luminescent material belongs to Sm³⁺4f → 4f transition of the ion.

Example 8 x 0.03, y 0.8, and z 0.2

Get Y₂O₃、Sm₂O₃、Ta₂O₅、Nb₂O₅Mixing according to a molar ratio of 0.985:0.015:0.8:0.2, putting the mixture into a corundum crucible, putting the corundum crucible filled with the mixture into a high-temperature furnace, calcining for 16 hours at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10h at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain the temperature-sensitive luminescent material Y_2-0.03Sm_0.03O₃·0.8Ta₂O₅·0.2Nb₂O₅。

The temperature-sensitive luminescent material obtained in example 8 was subjected to excitation spectroscopy and emission spectroscopy, and the temperature-sensitive luminescent material was tested to be effectively excited by ultraviolet light and blue light. The temperature-sensitive luminescent material provided in embodiment 8 of the present invention is exposed to ultraviolet lightUnder the excitation of light, the emission spectrum of the light-emitting diode consists of broadband emission and linear emission, the broadband emission peak is positioned near 400nm and is attributed to NbO₄ ^3-Has a linear emission peak of Sm³⁺The characteristic emission of (1); the emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 8 of the invention after excitation of 405nm violet light is orange red, and the luminescent color of the temperature-sensitive luminescent material belongs to Sm³⁺4f → 4f transition of the ion.

Example 9 x 0.03, y 0.7, and z 0.3

Get Y₂O₃、Sm₂O₃、Ta₂O₅、Nb₂O₅Mixing according to a molar ratio of 0.985:0.015:0.7:0.3, putting the mixture into a corundum crucible, putting the corundum crucible filled with the mixture into a high-temperature furnace, calcining for 16 hours at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10h at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain the temperature-sensitive luminescent material Y_2-0.03Sm_0.03O₃·0.7Ta₂O₅·0.3Nb₂O₅。

The emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 9 of the invention consists of broadband emission and linear emission under the excitation of ultraviolet light, and the broadband emission peak is positioned near 400nm and belongs to NbO₄ ^3-Has a linear emission peak of Sm³⁺The characteristic emission of (1); the emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 9 of the invention after excitation by 405nm violet light is orange red, and the luminescent color of the temperature-sensitive luminescent material belongs to Sm³⁺4f → 4f transition of the ion.

Example 10 x 0.03, y 0.9, and z 0.1

Get Y₂O₃、Sm₂O₃、Ta₂O₅、Nb₂O₅Mixing according to a molar ratio of 0.985:0.015:0.9:0.1, placing the mixture into a corundum crucible, and adding the mixture into the corundum cruciblePlacing the corundum crucible filled with the mixture into a high-temperature furnace, calcining for 16h at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10h at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain the temperature-sensitive luminescent material Y_2-0.03Sm_0.03O₃·0.9Ta₂O₅·0.1Nb₂O₅。

The temperature-sensitive luminescent material obtained in example 10 was subjected to excitation spectrum and emission spectrum tests. The temperature sensitive luminescent material can be effectively excited by ultraviolet light and purple light. The emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 10 of the invention consists of broadband emission and linear emission under the excitation of ultraviolet light, and the broadband emission peak is positioned near 400nm and belongs to NbO₄ ^3-Has a linear emission peak of Sm³⁺The characteristic emission of (1); the emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 10 of the invention after excitation of 405nm violet light is orange red, and the luminescent color of the temperature-sensitive luminescent material belongs to Sm³⁺4f → 4f transition of the ion.

Example 11 x-0.04, y-0.7, and z-0.3

Get Y₂O₃、Sm₂O₃、Ta₂O₅、Nb₂O₅Mixing according to a molar ratio of 0.98:0.02:0.7:0.3, putting the mixture into a corundum crucible, putting the corundum crucible filled with the mixture into a high-temperature furnace, calcining for 16 hours at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10h at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain the temperature-sensitive luminescent material Y_2-0.04Sm_0.04O₃·0.7Ta₂O₅·0.3Nb₂O₅。

Temperature sensitive luminescence obtained in example 11And (3) carrying out excitation spectrum and emission spectrum tests on the material. The temperature sensitive luminescent material can be effectively excited by ultraviolet light and purple light. The emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 11 of the invention consists of broadband emission and linear emission under the excitation of ultraviolet light, and the broadband emission peak is positioned near 400nm and belongs to NbO₄ ^3-Has a linear emission peak of Sm³⁺The characteristic emission of (1); the emission spectrum of the temperature-sensitive luminescent material provided in embodiment 11 of the present invention after excitation by 405nm violet light is orange red, which is classified as Sm³⁺4f → 4f transition of the ion.

Example 12 x 0.02, y 0.8, and z 0.2

Taking Lu₂O₃、Sm₂O₃、Ta₂O₅、Nb₂O₅Mixing according to a molar ratio of 0.99:0.01:0.8:0.2, putting the mixture into a corundum crucible, putting the corundum crucible filled with the mixture into a high-temperature furnace, calcining for 16 hours at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining the corundum crucible for 10 hours at 1350 ℃ in the presence of air, naturally cooling the corundum crucible to room temperature, taking out the corundum crucible, crushing and grinding the corundum crucible uniformly to obtain the temperature-sensitive luminescent material Lu_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅。

The temperature-sensitive luminescent material obtained in example 12 was subjected to excitation spectrum and emission spectrum tests. The temperature-sensitive luminescent material can be effectively excited by ultraviolet light and blue light. The emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 12 of the invention consists of broadband emission and linear emission under the excitation of ultraviolet light, and the broadband emission peak is positioned near 400nm and belongs to NbO₄ ^3-Has a linear emission peak of Sm³⁺The characteristic emission of (1); the emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 12 of the invention after excitation by 405nm violet light is orange red, and the luminescent color of the temperature-sensitive luminescent material belongs to Sm³⁺4f → 4f transition of the ion.

Example 13 x-0.02, y-0.8, and z-0.2

Taking Sc₂O₃、Sm₂O₃、Ta₂O₅、Nb₂O₅Mixing according to a molar ratio of 0.99:0.01:0.8:0.2, putting the mixture into a corundum crucible, putting the corundum crucible filled with the mixture into a high-temperature furnace, calcining for 16 hours at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining the corundum crucible for 10 hours at 1350 ℃ in the presence of air, naturally cooling the corundum crucible to room temperature, taking out the corundum crucible, crushing and grinding the corundum crucible uniformly to obtain the temperature-sensitive luminescent material Sc_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅。

The temperature-sensitive luminescent material obtained in example 13 was subjected to excitation spectrum and emission spectrum measurement. The temperature-sensitive luminescent material can be effectively excited by ultraviolet light and blue light. The emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 13 of the invention consists of broadband emission and linear emission under the excitation of ultraviolet light, and the broadband emission peak is positioned near 400nm and belongs to NbO₄ ^3-Has a linear emission peak of Sm³⁺The characteristic emission of (1); the emission spectrum of the temperature-sensitive luminescent material provided by embodiment 13 of the present invention after excitation by 405nm violet light is orange red, which is classified as Sm³⁺4f → 4f transition of the ion.

Example 14 x 0.02, y 0.8, and z 0.2

Taking Gd₂O₃、Sm₂O₃、Ta₂O₅、Nb₂O₅Mixing according to a molar ratio of 0.99:0.01:0.8:0.2, putting the mixture into a corundum crucible, putting the corundum crucible filled with the mixture into a high-temperature furnace, calcining for 16 hours at 1350 ℃ in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain a powdery primary product; placing the primary product into a corundum crucibleThen placing the mixture into a high-temperature furnace, calcining the mixture for 10 hours at 1350 ℃ in the presence of air, naturally cooling the mixture to room temperature, taking out the mixture, crushing and grinding the mixture uniformly to obtain the temperature-sensitive luminescent material Gd_2-0.02Sm_0.02O₃·0.8Ta₂O₅·0.2Nb₂O₅。

The temperature-sensitive luminescent material obtained in example 14 was subjected to excitation spectrum and emission spectrum measurement. The temperature sensitive luminescent material can be effectively excited by ultraviolet light and purple light. The emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 14 of the invention consists of broadband emission and linear emission under the excitation of ultraviolet light, and the broadband emission peak is positioned near 400nm and belongs to NbO₄ ^3-Has a linear emission peak of Sm³⁺The characteristic emission of (1); the emission spectrum of the temperature-sensitive luminescent material provided by the embodiment 14 of the invention after excitation by 405nm violet light is orange red, and the luminescent color of the temperature-sensitive luminescent material belongs to Sm³⁺4f → 4f transition of the ion.

The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.