CN111073642A - Novel self-calibration fluorescent temperature probe material and preparation method and application thereof - Google Patents

Novel self-calibration fluorescent temperature probe material and preparation method and application thereof Download PDF

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CN111073642A
CN111073642A CN201911338701.5A CN201911338701A CN111073642A CN 111073642 A CN111073642 A CN 111073642A CN 201911338701 A CN201911338701 A CN 201911338701A CN 111073642 A CN111073642 A CN 111073642A
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temperature
probe material
gdtao
fluorescence emission
intensity ratio
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CN111073642B (en
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高妍
关钧华
温大尉
王波
宋伟东
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Wuyi University
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    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7767—Chalcogenides
    • C09K11/7769—Oxides
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
    • G01K11/32—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using changes in transmittance, scattering or luminescence in optical fibres

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  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The invention relates to a novel self-calibration fluorescent temperature probe material, a preparation method and application thereof, wherein the chemical formula of the probe material is Pr3+：GdTaO4The material can be synthesized by a simple high-temperature solid phase method. Under the excitation of ultraviolet light, three emission peaks at 489nm, 613nm and 657nm can be generated, and the fluorescence intensity ratio I is613/I489And I613/I657And the temperature respectively satisfy certain functional relations, and the temperature monitoring device can be used for temperature monitoring. Because the temperature probe material adopts the double fluorescence intensity ratios to detect the temperature, the temperature probe material has good self-calibration characteristic, effectively solves the problem of temperature measurement sensitivity difference of the single fluorescence intensity ratio temperature probe material in different temperature intervals, and has wide application prospect.

Description

Novel self-calibration fluorescent temperature probe material and preparation method and application thereof
Technical Field
The invention relates to a novel self-calibration fluorescent temperature probe material, a preparation method and application thereof, belonging to the fields of non-contact temperature detection technology, rare earth luminescent materials and the like.
Background
Accurate measurement of temperature is of great importance for exploring many important physical phenomena and application studies of new materials. The traditional contact temperature measurement utilizes heat exchange to realize a heat balance piece, and the application range of the traditional contact temperature measurement is greatly limited due to the fact that the traditional contact temperature measurement needs to be in direct contact with an object to be measured.
The non-contact temperature measuring tool does not need to be in contact with an object to be measured, and has very important value in remote temperature measurement. For some corrosive liquids, the traditional thermocouple is easy to corrode in the measuring process, so that measuring errors are caused; for precision devices or cultural relics, the contact measurement can damage the precision devices or the cultural relics to a certain extent; for some biological tissues, the contact thermometry tool cannot realize accurate measurement of the temperature inside the tissue.
The temperature detection technology based on the fluorescence intensity ratio of the luminescent material has the advantages of high spatial resolution, quick response, capability of being used for remote measurement and the like, and can meet the requirements of more accurate and complex measurement. Therefore, the fluorescent temperature probe material which has high spatial resolution and quick response and can be used for remote measurement has good application prospect.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a novel self-calibration fluorescence temperature probe material, a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: a novel self-calibration fluorescent temperature probe material has a chemical formula of Pr3+：GdTaO4。
In a preferred embodiment of the probe material of the present invention, the probe material is a monoclinic phase GdTaO4The matrix is doped with 1 percent of Pr3+Ions.
As a preferred embodiment of the probe material, the probe material shows fluorescence emission peaks with wavelengths of 489nm, 613nm and 657nm respectively under the excitation of 265nm ultraviolet light.
As a preferred embodiment of the probe material of the present invention, the fluorescence emission intensity ratio at 613nm and 489nm is exponential with the reciprocal temperature.
As a preferred embodiment of the probe material of the present invention, the fluorescence emission intensity ratio between 613nm and 657nm is exponential with the reciprocal temperature.
In a second aspect, the present invention provides a method for preparing the probe material, including the following steps: uniformly mixing gadolinium oxide, tantalum pentoxide, praseodymium oxide and boric acid, fully grinding, and calcining at high temperature to obtain the novel self-calibration fluorescent temperature probe material.
As a preferred embodiment of the method for preparing the probe material of the present invention, the molar mass ratio of the gadolinium oxide, the tantalum pentoxide, and the praseodymium oxide is 1: 0.0033, wherein the mass percent of the boric acid in the raw material is 5%.
In a preferred embodiment of the method for preparing the probe material of the present invention, the grinding time is 20 min.
As a preferred embodiment of the preparation method of the probe material, the high-temperature calcination temperature is 1350 ℃ and the time is 2 h.
In a third aspect, the invention provides the use of the probe material, Pr is irradiated with 265nm ultraviolet light3+：GdTaO4The temperature of the monitored object was detected by measuring the fluorescence emission intensity ratio of the material at 613nm and 489nm and the fluorescence emission intensity ratio at 613nm and 657 nm.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a novel self-calibration fluorescent temperature probe material which comprises the following components in parts by weight: pr (Pr) of3+：GdTaO4The material generates three main emission peaks under the excitation of 265nm ultraviolet light, the wavelengths of the emission peaks are 489nm (blue), 613nm (red) and 657nm (red), wherein the emission peaks at 489nm and 657nm are respectively derived from Pr3+Ion(s)3P0Energy level to ground state and lower excited state3F2Radiative transition of energy level, emission peak at 489nm derived from Pr3+Ion(s)1D2Radiative transitions of energy levels to the ground state. The relative intensities of the three emission peaks vary at different test temperatures, in particular the fluorescence intensity ratio I613/I489And I613/I657And the temperature respectively satisfy certain functional relations, and the temperature monitoring device can be used for temperature monitoring. The temperature probe material has good self-calibration characteristic because the fluorescence intensity ratio is not influenced by external environmental factors such as fluctuation of an excitation light source and the like, and the accuracy of the temperature probe material is further improved by adopting the double fluorescence intensity ratio to monitor the temperature.
Drawings
FIG. 1 shows Pr3+:GdTaO4XRD powder diffraction pattern of (a).
FIG. 2 shows Pr3+:GdTaO4The temperature-variable emission spectrum of (1).
FIG. 3 shows fluorescence intensity ratio I613/I489Exponential dependence on the reciprocal of the temperature.
FIG. 4 shows fluorescence intensity ratio I613/I657Exponential dependence on the reciprocal of the temperature.
FIG. 5 shows fluorescence intensity ratio I613/I489And I613/I657Sensitivity profile to temperature.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
Example 1 Pr3+:GdTaO4Synthesis of phosphor
Raw materials: gadolinium oxide (Gd)2O3)362.5mg tantalum pentoxide (Ta)2O5)441.9mg of praseodymium oxide (Pr)6O11)3.4mg of boric acid (H)3BO3)40.4mg
Uniformly mixing the weighed raw materials in an agate mortar, fully grinding for 20min, putting into a corundum crucible, putting into a box furnace, and calcining at 1350 ℃ for 2h to obtain Pr3+:GdTaO4And (3) fluorescent powder.
Pr synthesized by high-temperature solid phase method3+:GdTaO4The XRD powder diffraction pattern of the compound is shown in figure 1, wherein PDF 24-0441 is a standard card of the phase in a JADE database.
Example 2 Pr3+:GdTaO4Application of fluorescent powder
The phosphor was irradiated with ultraviolet light of wavelength 265nm to generate three main emission peaks with wavelengths of 489nm, 613nm, and 657nm, respectively, and the emission spectra of the phosphor at different temperatures were monitored, as shown in fig. 2. Deriving I from the emission spectrum613/I489And I613/I657Respectively, are exponentially related to the reciprocal of the temperature, as shown in fig. 3 and 4, respectively, wherein I613、I489、I657The intensity of the emission peak at the wavelength can be used for calibrating the temperature of the monitored object.
Irradiating Pr with 265nm ultraviolet light3+:GdTaO4Fluorescent powder, measuring Pr by FLS980 fluorescence spectrometer3+:GdTaO4The variable temperature emission spectrum of (1), calculating I613/I489And I613/I657The values are compared in the index maps given in fig. 3 and 4, respectively, and the temperature of the monitored object can be calibrated.
By means of I613/I489Measuring the temperature, and obtaining the maximum sensitivity of 3.9 multiplied by 10 when the monitored temperature is 480K-3K-1By means of I613/I657The temperature measurement is carried out, and the maximum sensitivity is obtained when the temperature is monitored to 480K and is 3.2 multiplied by 10-3K-1As shown in fig. 5. Notably, I is utilized around room temperature613/I657High sensitivity of measuring temperature and high temperature section utilization I613/I489The sensitivity of the measured temperature is high, and the sensitivity can be mutually compensated, so that the problem of temperature measurement sensitivity difference of the temperature probe material with single fluorescence intensity ratio in different temperature ranges can be effectively solved by adopting the temperature detection method with double fluorescence intensity ratios, and the method has wide application prospect.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. A novel self-calibration fluorescent temperature probe material is characterized in that the chemical formula of the probe material is Pr3+：GdTaO4。
2. The probe material of claim 1, wherein the probe material is GdTaO in a monoclinic phase4The matrix is doped with 1 percent of Pr3+Ions.
3. The probe material of claim 1, wherein the probe material exhibits fluorescence emission peaks at 489nm, 613nm, and 657nm, respectively, under excitation of 265nm ultraviolet light.
4. The probe material of claim 3, wherein the ratio of fluorescence emission intensities at 613nm and 489nm is exponential with the reciprocal temperature.
5. The probe material of claim 3, wherein the ratio of fluorescence emission intensities at 613nm and 657nm is exponential with the reciprocal temperature.
6. The method for preparing a probe material according to any one of claims 1 to 5, comprising the steps of: uniformly mixing gadolinium oxide, tantalum pentoxide, praseodymium oxide and boric acid, fully grinding, and calcining at high temperature to obtain the novel self-calibration fluorescent temperature probe material.
7. The method for preparing the probe material according to claim 6, wherein the molar mass ratio of the gadolinium oxide to the tantalum pentoxide to the praseodymium oxide is 1: 0.0033, wherein the mass percent of the boric acid in the raw material is 5%.
8. The method of claim 6, wherein the grinding time is 20 min.
9. The method of claim 6, wherein the high temperature calcination is carried out at 1350 ℃ for 2 hours.
10. Use of the probe material according to any one of claims 1 to 5, wherein Pr is irradiated with 265nm ultraviolet light3+：GdTaO4The temperature of the monitored object was detected by measuring the fluorescence emission intensity ratio of the material at 613nm and 489nm and the fluorescence emission intensity ratio at 613nm and 657 nm.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113390529A (en) * 2021-06-10 2021-09-14 松山湖材料实验室 Fluorescent temperature measurement method suitable for ultra-wide temperature measurement range
CN113447134A (en) * 2021-06-25 2021-09-28 松山湖材料实验室 Temperature measuring device and temperature measuring method suitable for special environment
CN114479853A (en) * 2022-01-11 2022-05-13 五邑大学 Optical temperature sensing material and application thereof
DE102021133467A1 (en) 2021-12-16 2023-06-22 Endress+Hauser Conducta Gmbh+Co. Kg Calibration standard, sensor arrangement and use

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CN104726100A (en) * 2015-03-31 2015-06-24 中国科学院福建物质结构研究所 Fluorescent temperature probe material used for temperature detection and preparation method for fluorescent temperature probe material
CN106635008A (en) * 2016-09-29 2017-05-10 中国科学院福建物质结构研究所 High-sensitivity fluorescent temperature sensitive material as well as preparation method and application thereof
CN108456524A (en) * 2018-04-17 2018-08-28 东北电力大学 A kind of fluorescent material and preparation method thereof and method for measuring temperature

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CN104726100A (en) * 2015-03-31 2015-06-24 中国科学院福建物质结构研究所 Fluorescent temperature probe material used for temperature detection and preparation method for fluorescent temperature probe material
CN106635008A (en) * 2016-09-29 2017-05-10 中国科学院福建物质结构研究所 High-sensitivity fluorescent temperature sensitive material as well as preparation method and application thereof
CN108456524A (en) * 2018-04-17 2018-08-28 东北电力大学 A kind of fluorescent material and preparation method thereof and method for measuring temperature

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113390529A (en) * 2021-06-10 2021-09-14 松山湖材料实验室 Fluorescent temperature measurement method suitable for ultra-wide temperature measurement range
CN113390529B (en) * 2021-06-10 2023-10-27 松山湖材料实验室 Fluorescence temperature measurement method suitable for ultra-wide temperature measurement range
CN113447134A (en) * 2021-06-25 2021-09-28 松山湖材料实验室 Temperature measuring device and temperature measuring method suitable for special environment
CN113447134B (en) * 2021-06-25 2022-09-02 松山湖材料实验室 Temperature measuring device and temperature measuring method suitable for special environment
DE102021133467A1 (en) 2021-12-16 2023-06-22 Endress+Hauser Conducta Gmbh+Co. Kg Calibration standard, sensor arrangement and use
CN114479853A (en) * 2022-01-11 2022-05-13 五邑大学 Optical temperature sensing material and application thereof

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