CN113698933B - Temperature sensitive luminescent material and preparation method thereof - Google Patents
Temperature sensitive luminescent material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a temperature sensitive luminescent material, which has the molecular formula: a is that 2‑x Sm x O 3 ·yTa 2 O 5 ·zNb 2 O 5 The method comprises the steps of carrying out a first treatment on the surface of the Wherein x=0.001 to 0.2, y=0 to 0.9, and z=0.001 to 1; a is one or more of Gd, Y, lu and Sc. The temperature sensitive luminescent material provided by the invention uses niobium tantalate composite oxide as a matrix and 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 in a temperature range of 77-500K, shows adjustable multicolor emission and good stability, is nontoxic and harmless, has no radioactivity, and does not harm human bodies and the environment. Meanwhile, the preparation process is simple, the production efficiency is high, the grinding is easy, the industrial production is convenient, and the preparation process has good industrial application prospect.
Description
Technical Field
The invention relates to the technical field of photoluminescent materials, in particular to a temperature-sensitive luminescent material and a preparation method thereof.
Background
Photoluminescent material is a material capable of undergoing an electronic transition under the excitation of energy from external light radiation such as ultraviolet light, visible light, or infrared light, to produce 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 photoluminescent material activated by rare earth ions has important application in the fields of solid state lighting, display, laser crystal, optical fiber communication and the like. However, the luminescence properties of rare earth ions are susceptible to temperature, and different temperatures can cause significant changes in the spectrum of the material. 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 utilizing the luminescence mode has a plurality of advantages, such as electromagnetic and radio frequency interference resistance, can work under severe environments such as high temperature, radiation and the like, has high sensitivity and resolution, is safe and nontoxic, and has wide application range.
At present, the research reports of temperature sensitive luminescent materials are not many, and 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 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 invention is to provide a temperature-sensitive luminescent material and a preparation method thereof, and the temperature response is sensitive.
In order to solve the technical problems, the invention provides a temperature sensitive luminescent material, which has the following molecular formula:
A 2-x Sm x O 3 ·yTa 2 O 5 ·zNb 2 O 5 ；
wherein x=0.001 to 0.2, preferably 0.005.ltoreq.x.ltoreq.0.1, more preferably 0.005.ltoreq.x.ltoreq.0.05, still more preferably 0.005.ltoreq.x.ltoreq.0.04, most preferably 0.01.ltoreq.x.ltoreq.0.03; in some embodiments provided herein, the x is preferably 0.02; in other embodiments provided by the present invention, the x is preferably 0.01, 0.03 or 0.04.
y=0 to 0.9, preferably 0.5.ltoreq.y.ltoreq.0.9, more preferably 0.7.ltoreq.y.ltoreq.0.9; in some embodiments provided herein, the y is preferably 0.8; in other embodiments provided by the present invention, the y is preferably 0.9 or 0.7.
z=0.001 to 1, preferably 0.05.ltoreq.y.ltoreq.0.5, more preferably 0.1.ltoreq.y.ltoreq.0.3; in some embodiments provided herein, the y is preferably 0.2; in other embodiments provided by the present invention, the 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 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 ；Y 2-0.01 Sm 0.01 O 3 ·0.7Ta 2 O 5 ·0.3Nb 2 O 5 ；
Y 2-0.01 Sm 0.01 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 ；Y 2-0.01 Sm 0.01 O 3 ·0.9Ta 2 O 5 ·0.1Nb 2 O 5 ；
Y 2-0.02 Sm 0.02 O 3 ·0.7Ta 2 O 5 ·0.3Nb 2 O 5 ；Y 2-0.03 Sm 0.03 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 ；
Y 2-0.03 Sm 0.03 O 3 ·0.7Ta 2 O 5 ·0.3Nb 2 O 5 ；Y 2-0.03 Sm 0.03 O 3 ·0.9Ta 2 O 5 ·0.1Nb 2 O 5 ；
Y 2-0.04 Sm 0.04 O 3 ·0.7Ta 2 O 5 ·0.3Nb 2 O 5 ；Lu 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 ；
Sc 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 ；Gd 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 。
the temperature sensitive range of the temperature sensitive luminescent material provided by the invention is 77K-500K.
Niobate and tantalate have outstanding properties such as high thermal stability, high environmental stability, low toxicity, low phonon energy, etc. as matrix materials. To NbO 4 3- The group doped in tantalate can also become an effective luminescence center, and the luminescence efficiency is improved. The temperature sensitive luminescent material provided by the invention adopts Y 2 O 3 、Ta 2 O 5 With Nb 2 O 5 Sm as matrix 3+ As an activator, a composite oxide fluorescent powder A which can be used as a temperature sensitive luminescent material is obtained 2-x Sm x O 3 ·yTa 2 O 5 ·zNb 2 O 5 . Through A 2-x Sm x O 3 ·yTa 2 O 5 ·zNb 2 O 5 Light emission intensity changes with temperature and is based on NbO 4 3- Radicals and Sm 3+ The different thermal quenching performance and characteristic emission among ions can realize the sensitivity of the luminous intensity of the luminous material to the temperature response, has good relative sensitivity, has larger color gamut, 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, convenient industrialized 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 an A source compound, a samarium source compound, a tantalum source compound and a niobium source compound to obtain a mixture;
s2) roasting the mixture to obtain the temperature sensitive luminescent material.
Preferably, the roasting atmosphere 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, which is well known to those skilled in the art, and is not particularly limited, and is preferably one or more of an oxide, chloride, carbonate, silver nitrate, oxalate, citrate, and acetate of a. For example, when A is Y, the A source may be yttrium oxide Y 2 O 3 Yttrium nitrate Y (NO) 3 ) 3 ·6H 2 O, etc.
Sm is an activator ion in the invention, and the samarium source compoundThe compound may be a samarium source compound known to those skilled in the art, and is not particularly limited, and the samarium source compound is preferably selected from one or more of samarium oxide, chloride, carbonate and nitrate, and is most preferably Sm oxide Sm 2 O 3 。
The tantalum source compound is a compound containing Ta element known to those skilled in the art, and is not particularly limited, and the tantalum source compound is preferably selected from one or more of elemental metals, oxides, chlorides, hydroxides and nitrates of tantalum, more preferably, ta oxide 2 O 5 。
The Nb source compound is a compound containing Nb element known to those skilled in the art, and is not particularly limited, and the Nb source compound is preferably one or more selected from the group consisting of elemental metal, oxide, hydroxide and nitrate of niobium, more preferably Nb oxide 2 O 5 。
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 to 0.999): (0.001-0.20): (0.7-0.99): (0.01-0.30).
The preparation method of the invention preferably comprises the following steps:
a) Mixing an A source compound, a samarium source compound, a tantalum source compound and a niobium source compound, and performing primary calcination in a protective atmosphere to obtain a primary product;
b) And (3) carrying out secondary roasting on the primary product in a protective atmosphere to obtain the temperature sensitive luminescent material.
In the present invention, the A source compound, samarium source compound, tantalum source compound and niobium source compound are preferably mixed first.
After mixing, grinding is preferably carried out firstly, and then primary calcination is carried out under a protective atmosphere; the protective atmosphere is a protective atmosphere well known to those skilled in the art, and is not particularly limited, and is preferably air in the present invention; the temperature of the primary calcination is preferably 1100-1600 ℃, more preferably 1250-1500 ℃, and still more preferably 1350 ℃; the time of the primary calcination is preferably 5 to 20 hours, more preferably 10 to 20 hours, still more preferably 16 hours.
After primary calcination, the primary product is obtained preferably after cooling and grinding; the grinding apparatus of the present invention is not particularly limited, and may be any of crushing and grinding machines known to those skilled in the art.
Carrying out secondary roasting on the primary product in a protective atmosphere; the protective atmosphere is not particularly limited as long as it is a protective atmosphere well known to those skilled in the art, and in the present invention, the secondary baking process 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 still more preferably 1350 ℃; the time for the secondary calcination is preferably 5 to 20 hours, more preferably 8 to 15 hours, still more preferably 10 hours. The apparatus used for 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 the crystal phase, so that the product has the primary luminescence property, the secondary calcination can enable the phase of the crystal to be more complete and enhance the luminescence property, and high-efficiency fluorescence is emitted.
After the secondary roasting, the temperature sensitive luminescent material is obtained preferably after cooling and grinding.
The temperature sensitive luminescent material provided by the invention has the advantages of sensitive luminescent intensity to temperature response, larger color gamut variation, chemical and physical stability, and suitability 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 following molecular formula: a is that 2-x Sm x O 3 ·yTa 2 O 5 ·zNb 2 O 5 The method comprises the steps of carrying out a first treatment on the surface of the Wherein x=0.001 to 0.2 and y=0 to the upper portion thereof0.9, z=0.001 to 1; a is one or more of Gd, Y, lu and Sc.
The temperature sensitive luminescent material provided by the invention uses niobium tantalate composite oxide as a matrix and 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 in a temperature range of 77-500K, shows adjustable multicolor emission and good stability, is nontoxic and harmless, has no radioactivity, and does not harm human bodies and the environment. Meanwhile, the preparation process is simple, the production efficiency is high, the grinding is easy, the industrial production is convenient, and the preparation process has good industrial application prospect.
Drawings
FIG. 1 is a graph showing the emission spectrum of the temperature sensitive luminescent material obtained in example 1 of the present invention under excitation at 230 nm;
FIG. 2 is a graph showing the emission spectrum and the corresponding excitation spectrum of the temperature sensitive luminescent material obtained in example 1 of the present invention under 262nm ultraviolet excitation;
FIG. 3 is a graph showing the emission spectrum and the corresponding excitation spectrum of the temperature sensitive luminescent material obtained in example 1 of the present invention under 405nm excitation by ultraviolet light;
FIG. 4 is a graph showing the emission spectrum of the temperature sensitive luminescent material obtained in example 4 of the present invention under 262nm ultraviolet excitation;
FIG. 5 is a graph showing the emission spectrum of the temperature sensitive luminescent material of example 7 of the present invention under 262nm ultraviolet excitation;
FIG. 6 is a graph showing the emission spectra of the temperature sensitive luminescent material obtained in example 1 of the present invention at different temperatures under 255nm ultraviolet excitation.
Detailed Description
In order to further illustrate the present invention, the temperature-sensitive luminescent material and the preparation method thereof provided by the present invention are described in detail below with reference to examples.
The reagents used in the examples below are all commercially available.
Example 1 x =0.02, y=0.8, z=0.2
Taking Y 2 O 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to the molar ratio of 0.99:0.01:0.8:0.2, and fully and uniformly grinding to obtain a mixture. Placing the mixture into a corundum crucible, placing 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 initial product; placing the initial product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10 hours 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 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 。
The temperature sensitive luminescent material obtained in example 1 was subjected to excitation spectrum and emission spectrum, and the results are shown in FIGS. 1 to 3. In which FIG. 1 shows the emission spectrum of the temperature sensitive luminescent material provided in embodiment 1 of the present invention under 230nm excitation, as can be seen from FIG. 2, the temperature sensitive luminescent material can be effectively excited by 262nm ultraviolet light, the emission spectrum thereof is composed of broadband emission and linear emission, the broadband emission peak is located near 400nm and belongs to NbO 4 3- Is of Sm 3+ Is characterized by emission of (a); FIG. 3 shows the emission spectrum of the temperature sensitive luminescent material according to example 1 of the present invention after excitation with 405nm blue light, wherein the luminescent color of the temperature sensitive luminescent material is orange red, which belongs to Sm as shown in FIG. 3 3+ The ion transitions from 4f to 4 f. Fig. 6 shows the emission spectra of the samples of example 1 at different temperatures. The test results showed that the maximum relative sensitivity obtained in example 1 was 1.151%.
Example x =0.02, y=0.8, z=0.2
Taking Y (NO) 3 ) 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to the molar ratio of 1.98:0.01:0.8:0.2, and fully and uniformly grinding to obtain a mixture. Placing the mixture into a corundum crucible, placing the corundum crucible filled with the mixture into a high-temperature furnace, calcining at 1350 ℃ for 16h in the presence of air, and naturally cooling to a roomTaking out, crushing and grinding uniformly to obtain a powdery initial product; placing the initial product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10 hours 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 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 。
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 temperature-sensitive luminescent material provided in embodiment 2 of the invention has an emission spectrum consisting of broadband emission and linear emission under ultraviolet excitation, the broadband emission peak is located near 400nm and is responsible for charge migration of NbO43-, and the linear emission peak is Sm 3+ Is characterized by emission of (a); the temperature-sensitive luminescent material provided in embodiment 2 of the invention has an emission spectrum after excitation of 405nm blue light, and the luminescent color of the temperature-sensitive luminescent material is orange red and belongs to Sm 3+ The ion transitions from 4f to 4 f.
Example 3 x =0.02, y=0.8, z=0.2
Taking Y 2 (CO 3 ) 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to a molar ratio of 0.99:0.01:0.8:0.2, placing the mixture into a corundum crucible, placing 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 initial product; placing the initial product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10 hours 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 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 。
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 invention is trueThe temperature-sensitive luminescent material provided in example 3 has an emission spectrum consisting of broadband emission and linear emission under ultraviolet excitation, the broadband emission peak being located near 400nm and attributed to NbO 4 3- Is of Sm 3+ Is characterized by emission of (a); the temperature-sensitive luminescent material provided in embodiment 3 of the invention has an emission spectrum after excitation of 405nm blue light, and the luminescent color of the temperature-sensitive luminescent material is orange red and belongs to Sm 3+ The ion transitions from 4f to 4 f.
Example 4 x =0.01, y=0.7, z=0.3
Taking Y 2 O 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to a molar ratio of 0.995:0.005:0.7:0.3, placing the mixture into a corundum crucible, placing 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 initial product; placing the initial product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10 hours 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 2-0.01 Sm 0.01 O 3 ·0.7Ta 2 O 5 ·0.3Nb 2 O 5 。
FIG. 4 shows the emission spectrum of the temperature sensitive luminescent material of example 4 under 262nm ultraviolet excitation, which comprises broadband emission and linear emission, the broadband emission peak is located near 400nm, belonging to NbO 4 3- Is of Sm 3+ Is less than the luminescence intensity of example 1 under 262nm uv excitation; the temperature-sensitive luminescent material provided in embodiment 4 of the invention has an emission spectrum after excitation of 405nm blue light, and the luminescent color of the temperature-sensitive luminescent material is orange red and belongs to Sm 3+ The ion transitions from 4f to 4 f.
Example 5 x =0.01, y=0.8, z=0.2
Taking Y 2 O 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to a molar ratio of 0.995:0.005:0.8:0.2, placing the mixture into a corundum crucible, placing 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 initial product; placing the initial product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10 hours 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 2-0.01 Sm 0.01 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 。
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 in embodiment 5 of the invention has an emission spectrum composed of broadband emission and linear emission under ultraviolet excitation, the broadband emission peak is located near 400nm and belongs to NbO 4 3- Is of Sm 3+ Is characterized by emission of (a); the temperature-sensitive luminescent material provided in embodiment 5 of the invention has an emission spectrum after excitation of 405nm blue light, and the luminescent color of the temperature-sensitive luminescent material is orange red and belongs to Sm 3+ The ion transitions from 4f to 4 f.
Example x =0.01, y=0.9, z=0.1
Taking Y 2 O 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to a molar ratio of 0.995:0.005:0.9:0.1, placing the mixture into a corundum crucible, placing 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 initial product; placing the initial product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10 hours 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 2-0.01 Sm 0.01 O 3 ·0.9Ta 2 O 5 ·0.1Nb 2 O 5 。
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 in embodiment 6 of the invention has an emission spectrum composed of broadband emission and linear emission under ultraviolet excitation, the broadband emission peak is located near 400nm and belongs to NbO 4 3- Is of Sm 3+ Is characterized by emission of (a); the temperature-sensitive luminescent material provided in embodiment 6 of the invention has an emission spectrum after excitation of 405nm blue light, and the luminescent color of the temperature-sensitive luminescent material is orange red and belongs to Sm 3+ The ion transitions from 4f to 4 f.
Example x =0.02, y=0.7, z=0.3
Taking Y 2 O 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to a molar ratio of 0.99:0.01:0.7:0.3, placing the mixture into a corundum crucible, placing 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 initial product; placing the initial product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10 hours 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 2-0.02 Sm 0.02 O 3 ·0.7Ta 2 O 5 ·0.3Nb 2 O 5 。
FIG. 5 shows the emission spectrum of the temperature sensitive luminescent material of example 7 under 262nm ultraviolet excitation, which comprises broadband emission and linear emission, the broadband emission peak is located near 400nm, belonging to NbO 4 3- Is of Sm 3+ Is characterized by emission of (a); the temperature-sensitive luminescent material provided in embodiment 7 of the invention has an emission spectrum after excitation of 405nm violet light, and the luminescent color of the temperature-sensitive luminescent material is orange red and belongs to Sm 3+ The ion transitions from 4f to 4 f.
Example x =0.03, y=0.8, z=0.2
Taking Y 2 O 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to a molar ratio of 0.985:0.015:0.8:0.2, placing the mixture into a corundum crucible, placing 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 initial product; placing the initial product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10 hours 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 2-0.03 Sm 0.03 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 。
The temperature sensitive luminescent material obtained in example 8 can be effectively excited by ultraviolet light and blue light by performing excitation spectrum and emission spectrum test. The temperature sensitive luminescent material provided in embodiment 8 of the invention has an emission spectrum composed of broadband emission and linear emission under ultraviolet excitation, the broadband emission peak is located near 400nm and belongs to NbO 4 3- Is of Sm 3+ Is characterized by emission of (a); the temperature-sensitive luminescent material provided in embodiment 8 of the invention has an emission spectrum after excitation of 405nm violet light, and the luminescent color of the temperature-sensitive luminescent material is orange red and belongs to Sm 3+ The ion transitions from 4f to 4 f.
Example 9 x =0.03, y=0.7, z=0.3
Taking Y 2 O 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to a molar ratio of 0.985:0.015:0.7:0.3, placing the mixture into a corundum crucible, placing 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 initial product; placing the primary product into a corundum crucible, and thenCalcining in a high temperature furnace at 1350 deg.C for 10 hr in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding to obtain temperature sensitive luminescent material Y 2-0.03 Sm 0.03 O 3 ·0.7Ta 2 O 5 ·0.3Nb 2 O 5 。
The temperature sensitive luminescent material provided in embodiment 9 of the invention has an emission spectrum composed of broadband emission and linear emission under ultraviolet excitation, the broadband emission peak is located near 400nm and belongs to NbO 4 3- Is of Sm 3+ Is characterized by emission of (a); the temperature-sensitive luminescent material provided in embodiment 9 of the invention has an emission spectrum after excitation of 405nm violet light, and the luminescent color of the temperature-sensitive luminescent material is orange red and belongs to Sm 3+ The ion transitions from 4f to 4 f.
Example x =0.03, y=0.9, z=0.1
Taking Y 2 O 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to a molar ratio of 0.985:0.015:0.9:0.1, placing the mixture into a corundum crucible, placing 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 initial product; placing the initial product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10 hours 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 2-0.03 Sm 0.03 O 3 ·0.9Ta 2 O 5 ·0.1Nb 2 O 5 。
The temperature sensitive luminescent material obtained in example 10 was subjected to excitation spectrum and emission spectrum test. The temperature sensitive luminescent material can be effectively excited by ultraviolet light and purple light. The temperature sensitive luminescent material provided in embodiment 10 of the invention has an emission spectrum composed of broadband emission and linear emission under ultraviolet excitation, the broadband emission peak is located near 400nm and belongs to NbO 4 3- Is of Sm 3+ Characteristic hair of (a)Shooting; the temperature sensitive luminescent material provided in embodiment 10 of the invention has an emission spectrum after excitation of 405nm violet light, and the luminescent color of the temperature sensitive luminescent material is orange red and belongs to Sm 3+ The ion transitions from 4f to 4 f.
Example 11 x =0.04, y=0.7, z=0.3
Taking Y 2 O 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to a molar ratio of 0.98:0.02:0.7:0.3, placing the mixture into a corundum crucible, placing 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 initial product; placing the initial product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10 hours 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 2-0.04 Sm 0.04 O 3 ·0.7Ta 2 O 5 ·0.3Nb 2 O 5 。
The temperature sensitive luminescent material obtained in example 11 was subjected to excitation spectrum and emission spectrum test. The temperature sensitive luminescent material can be effectively excited by ultraviolet light and purple light. The temperature-sensitive luminescent material provided in embodiment 11 of the invention has an emission spectrum composed of broadband emission and linear emission under ultraviolet excitation, the broadband emission peak is located near 400nm and belongs to NbO 4 3- Is of Sm 3+ Is characterized by emission of (a); the temperature-sensitive luminescent material provided in embodiment 11 of the invention has an emission spectrum after excitation of 405nm violet light, and the luminescent color of the temperature-sensitive luminescent material is orange red and belongs to Sm 3+ The ion transitions from 4f to 4 f.
Example 12 x =0.02, y=0.8, z=0.2
Lu is taken 2 O 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to the molar ratio of 0.99:0.01:0.8:0.2, placing the mixture into a corundum crucible, and placing the corundum crucible filled with the mixture into the corundum crucibleCalcining in a high temperature 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 initial product; placing the initial product into a corundum crucible, then placing into a high-temperature furnace, calcining at 1350 ℃ for 10 hours in the presence of air, naturally cooling to room temperature, taking out, crushing and grinding uniformly to obtain the temperature sensitive luminescent material Lu 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 。
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 temperature sensitive luminescent material provided in embodiment 12 of the invention has an emission spectrum composed of broadband emission and linear emission under ultraviolet excitation, the broadband emission peak is located near 400nm and belongs to NbO 4 3- Is of Sm 3+ Is characterized by emission of (a); the temperature-sensitive luminescent material provided in embodiment 12 of the invention has an emission spectrum after excitation of 405nm violet light, and the luminescent color of the temperature-sensitive luminescent material is orange red and belongs to Sm 3+ The ion transitions from 4f to 4 f.
Example 13 x =0.02, y=0.8, z=0.2
Sc is taken 2 O 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to a molar ratio of 0.99:0.01:0.8:0.2, placing the mixture into a corundum crucible, placing 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 initial product; placing the initial product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10 hours 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 Sc 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 。
Excitation Spectrum and emission of the temperature-sensitive luminescent Material obtained in example 13And (5) spectrum testing. The temperature sensitive luminescent material can be effectively excited by ultraviolet light and blue light. The temperature-sensitive luminescent material provided in embodiment 13 of the invention has an emission spectrum composed of broadband emission and linear emission under ultraviolet excitation, the broadband emission peak is located near 400nm and belongs to NbO 4 3- Is of Sm 3+ Is characterized by emission of (a); the temperature-sensitive luminescent material provided in embodiment 13 of the invention has an emission spectrum after excitation of 405nm violet light, and the luminescent color of the temperature-sensitive luminescent material is orange red and belongs to Sm 3+ The ion transitions from 4f to 4 f.
Example 14 x =0.02, y=0.8, z=0.2
Gd taking 2 O 3 、Sm 2 O 3 、Ta 2 O 5 、Nb 2 O 5 Mixing according to a molar ratio of 0.99:0.01:0.8:0.2, placing the mixture into a corundum crucible, placing 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 initial product; placing the initial product into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, calcining for 10 hours 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 Gd 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 。
The temperature sensitive luminescent material obtained in example 14 was subjected to excitation spectrum and emission spectrum test. The temperature sensitive luminescent material can be effectively excited by ultraviolet light and purple light. The temperature sensitive luminescent material provided in embodiment 14 of the invention has an emission spectrum composed of broadband emission and linear emission under ultraviolet excitation, the broadband emission peak is located near 400nm and belongs to NbO 4 3- Is of Sm 3+ Is characterized by emission of (a); the temperature-sensitive luminescent material provided in embodiment 14 of the invention has an emission spectrum after excitation of 405nm violet light, and the luminescent color of the temperature-sensitive luminescent material is orange red and belongs to Sm 3+ The ion transitions from 4f to 4 f.
The above description of the embodiments is only for aiding in the understanding of the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
Claims (9)
1. An application of a temperature sensitive luminescent material in an optical temperature sensor, which is characterized in that the molecular formula of the temperature sensitive luminescent material is as follows:
A 2-x Sm x O 3 ·yTa 2 O 5 ·zNb 2 O 5 ；
wherein x=0.001-0.2, y=0.7-0.9, and z is more than 0.1 and less than or equal to 0.3;
a is one or more of Gd, lu and Sc.
2. The use according to claim 1, wherein the temperature sensitive luminescent material has the formula:
Y 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 ；Y 2-0.01 Sm 0.01 O 3 ·0.7Ta 2 O 5 ·0.3Nb 2 O 5 ；
Y 2-0.01 Sm 0.01 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 ；Y 2-0.01 Sm 0.01 O 3 ·0.9Ta 2 O 5 ·0.1Nb 2 O 5 ；
Y 2-0.02 Sm 0.02 O 3 ·0.7Ta 2 O 5 ·0.3Nb 2 O 5 ；Y 2-0.03 Sm 0.03 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 ；
Y 2-0.03 Sm 0.03 O 3 ·0.7Ta 2 O 5 ·0.3Nb 2 O 5 ；Y 2-0.03 Sm 0.03 O 3 ·0.9Ta 2 O 5 ·0.1Nb 2 O 5 ；
Y 2-0.04 Sm 0.04 O 3 ·0.7Ta 2 O 5 ·0.3Nb 2 O 5 ；Lu 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 ；
Sc 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 ；Gd 2-0.02 Sm 0.02 O 3 ·0.8Ta 2 O 5 ·0.2Nb 2 O 5 。
3. the use according to claim 1, wherein the method for preparing the temperature sensitive luminescent material comprises:
s1) mixing an A source compound, a samarium source compound, a tantalum source compound and a niobium source compound to obtain a mixture;
s2) roasting the mixture to obtain the temperature sensitive luminescent material.
4. Use according to claim 3, wherein the firing atmosphere is air, nitrogen, argon or oxygen;
the roasting temperature is 1000-1600 ℃; the roasting time is 0.5-24 hours.
5. The use according to claim 3, wherein the a source compound is selected from one or more of the group consisting of oxides, chlorides, carbonates, silver nitrate, oxalates, citrates and acetates of a.
6. The use according to claim 3, wherein the samarium source compound is selected from one or more of the group consisting of samarium oxide, chloride, carbonate and nitrate.
7. The use according to claim 3, wherein the tantalum source compound is selected from one or more of elemental metals, oxides, chlorides, hydroxides and nitrates of tantalum.
8. The use according to claim 3, wherein the niobium source compound is selected from one or more of elemental niobium metal, oxides, hydroxides and nitrates.
9. A use according to claim 3, comprising:
a) Mixing an A source compound, a samarium source compound, a tantalum source compound and a niobium source compound, and performing primary calcination in a protective atmosphere to obtain a primary product;
b) And (3) carrying out secondary roasting on the primary product in a protective atmosphere to obtain the temperature sensitive luminescent material.
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