CN108840571B - Double-crystal-phase glass ceramic for fluorescent temperature probe and preparation method thereof - Google Patents
Double-crystal-phase glass ceramic for fluorescent temperature probe and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
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- 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
- G01K11/20—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using thermoluminescent materials
Abstract
The invention provides a CsPbBr-containing material capable of realizing efficient temperature detection3And EuPO4Glass ceramics with crystalline phase and preparation technology thereof. The glass component and the percentage (mol%) of the glass ceramic are as follows: 10-60 mol% P2O5；0‑40mol％SiO2；0‑40mol％Al2O3；0‑30mol％Cs2CO3；0‑30mol％PbBr2；0‑30mol％SrCO3；5‑30mol％NaBr；5‑30mol％EuCl3The total mole amount of the above components is 100 mol%. The invention also provides a preparation technology of the glass ceramic. Under the irradiation of ultraviolet light with the wavelength of 393 nanometers, Eu3+Red light emission band at 611nm with CsPbBr3The fluorescence intensity ratio of the green light emission band at 516nm changes obviously with temperature, and temperature detection in a certain temperature range can be realized. CsPbBr in the temperature range of 303-483K3/EuPO4The maximum absolute sensitivity of the biphase glass ceramic reaches 0.082K‑1The highest relative sensitivity reaches 1.8 percent K‑1. Moreover, the material has good thermal stability and can be recycled for many times. Thus, CsPbBr was shown3/EuPO4The biphase glass ceramic is a fluorescent temperature probe material capable of realizing high-efficiency temperature detection.
Description
Technical Field
The invention relates to the field of solid luminescent materials, in particular to a bicrystal phase glass ceramic capable of being applied to a fluorescent temperature probe and a preparation process thereof.
Background
Temperature is the most basic thermodynamic parameter, which plays an important role in industrial and scientific applications. The traditional temperature measurement method needs to be in contact with an object to be measured, and typically comprises a thermometer, a thermocouple and the like. However, the contact type temperature measurement can change the actual temperature of the object, which is easy to cause inaccurate temperature measurement. In addition, the effect of testing small-sized objects and fast moving objects is not satisfactory. Recently, fluorescent materials having higher fluorescence intensity than temperature-based probe materials have received much attention, and such fluorescent materials are non-contact type, have high measurement accuracy and spatial resolution, and can be used in harsh environments. The ideal fluorescent intensity ratio-based fluorescent probe needs two distinguishable emission peaks, high sensitivity and excellent thermal stability.
Most research has focused on rare earth fluorescence intensity ratio-based fluorescence temperature probes, which mainly utilize the abundant energy levels of rare earths. Conventionally, the thermal coupling energy level pair of a single rare earth (Er, Tm, Ho), which is commonly used as a fluorescence intensity ratio-based fluorescent probe, moves electrons in an opposite direction in the arrangement of the thermal coupling energy level with a change in temperature. However, the small energy gap difference in the thermal coupling energy level pair easily causes the overlapping of two monitoring emission peaks, thereby causing inaccurate temperature measurement. To address this problem, dual emission center rare earth/rare earth doped materials have been reported as fluorescent temperature probe materials. However, the low absorption cross section and weak fluorescence intensity of rare earth 4f-4f are determined by the characteristics of the astronomical forbidden band. In addition, rare earths are relatively expensive.
Therefore, people aim at semiconductor nanocrystal temperature measuring materials which have large absorption cross sections, high fluorescence quantum fields, high light stability and adjustable emission bands. These excellent properties make them suitable as fluorescent temperature probe materials. However, semiconductor nanocrystals are unstable and susceptible to other environmental factors (such as PH), which are detrimental to temperature detection.
Currently, most fluorescent materials based on fluorescence intensity ratio are phosphors and crystals. However, the phosphor is easy to scatter, which causes inaccurate temperature measurement; the preparation process of the crystal is complicated, and needs to consume a large amount of time and high cost. In recent years, the glass ceramic-based fluorescent temperature measuring material has attracted attention, not only has simple preparation technology and easy mass production, but also can be processed into various shapes, has excellent thermal stability and can be recycled. The excellent properties make it have potential application prospect in the field of fluorescent temperature probes.
The invention provides a dual-phase glass ceramic for high-sensitivity temperature detection and a preparation method thereof. CsPbBr under 393 nanometer ultraviolet excitation3/EuPO4The dual-phase glass ceramic exhibits CsPbBr3And Eu3+The main peaks of the fluorescent emission band are respectively positioned in a green light emission band at 516 nanometers and a red light emission band at 593 nanometers, 611 nanometers and 700 nanometers. Measuring the variable temperature emission spectrum in the temperature range of 303K-483K, and adopting Eu3+Middle 611nm and CsPbBr3The fluorescence intensity ratio of two peaks at 516nm is used as a temperature detection signal, the change of the fluorescence intensity ratio of the two peaks is very obvious, and the highest absolute sensitivity of the material reaches 0.082K-1The highest relative sensitivity reaches 1.8 percent K-1Higher than most of the reported fluorescent temperature probe materials. The novel CsPbBr3/EuPO4The biphase glass ceramic is a fluorescent temperature probe material with excellent performance.
Disclosure of Invention
The invention relates to CsPbBr3/EuPO4The preparation of the dual-phase glass ceramic aims at preparing a glass ceramic-based fluorescent temperature probe material which has high sensitivity and excellent thermal stability, can be excited by ultraviolet and is used for temperature detection.
The invention also provides the CsPbBr3/EuPO4The preparation method of the biphase glass ceramic comprises the steps of reasonably designing precursor glass components, adopting a melt quenching technology, preparing the required glass ceramic through self-crystallization, and in the cooling process, CsPbBr3And EuPO4Crystal grains are simultaneously precipitated in the glass matrix to form CsPbBr3/EuPO4A dual phase glass-ceramic. The material can be excited by violet light, and the highest absolute sensitivity reaches 0.082K-1The highest relative sensitivity reaches 1.8 percent K-1The temperature detection can be effectively performed.
CsPbBr3/EuPO4The preparation method of the dual-phase glass ceramic comprises the following steps:
(1) the design of a precursor glass substrate comprises the following components:
10-60mol％P2O5；0-40mol％SiO2；0-40mol％Al2O3；0-30mol％Cs2CO3；0-30mol％PbBr2；0-30mol％SrCO3；5-30mol％NaBr；5-30mol％EuCl3the total mole amount of the above components is 100 mol%.
According to the invention, the preferred contents of the components are as follows:
P2O5preferably 20 to 50 mol%;
SiO2preferably 5 to 30 mol%;
Al2O3preferably 5 to 30 mol%;
Cs2CO3preferably 5 to 25 mol%;
PbBr2preferably 5 to 25 mol%;
SrCO3preferably 5 to 25 mol%;
NaBr is preferably 5-25 mol%;
EuCl3preferably 10 to 25 mol%;
(2) will P2O5、SiO2、Al2O3、Cs2CO3、PbBr2、SrCO3、NaBr、EuCl3Weighing powder raw materials according to a certain component ratio, mixing the powder raw materials in an agate ball-milling tank, fully grinding the powder raw materials uniformly, placing the mixture in an alumina crucible, heating the mixture, preserving the heat for a period of time to melt the mixture, then quickly pouring the molten liquid into a mould to form the mixture, obtaining blocky glass ceramics through self-crystallization, finally placing the obtained glass ceramics into a resistance furnace to anneal so as to eliminate internal stress, cooling the glass ceramics along with the furnace, and cutting the glass ceramics into blocks;
according to the invention, in step (2), heating is carried out in a resistance furnace to 1300 ℃ at 900-. The temperature is maintained for 1 to 4 hours, preferably 1 to 3 hours, to melt the powder raw material.
According to the invention, in step (2), the glass melt is taken out and quickly poured into a mold for forming, so as to obtain the block-shaped glass ceramic.
According to the present invention, in the step (2), the annealing temperature is 200-400 ℃.
According to the invention, in the step (2), the temperature rise rate is controlled to be 1-10 ℃/min, preferably 2-5 ℃/min during the temperature rise process.
In the invention, by adopting the material components and the preparation process, CsPbBr embedded in the glass matrix can be obtained3/EuPO4A glass-ceramic of crystalline grains.
The invention also relates to application of the glass ceramic, which is characterized in that the glass ceramic fluorescent temperature probe is applied to temperature detection.
CsPbBr under 393 nanometer ultraviolet excitation3/EuPO4The dual-phase glass ceramic exhibits CsPbBr3And Eu3+The main peaks of the fluorescent emission band are respectively positioned in a green light emission band at 516 nanometers and a strong red light emission band at 593 nanometers, 611 nanometers and 700 nanometers. By using Eu3+Middle 611nm and CsPbBr3The ratio of the fluorescence intensities of the two peaks at 516nm was used as a temperature detection signal. The fluorescence intensity ratio of the two changes very obviously in the temperature range of 303K to 483K. CsPbBr3The fluorescence intensity of (1) is reduced very significantly, whereas Eu3+Only slightly reduced in emission intensity. The fluorescence intensity ratio at different temperatures is subjected to exponential fitting, and the highest absolute sensitivity reaches 0.082K-1The highest relative sensitivity reaches 1.8 percent K-1And the performance is superior to most of the reported fluorescence temperature probe materials. The temperature of the environment can be obtained by measuring the fluorescence intensity ratio of the two. Meanwhile, the color is changed from green to red along with the change of the temperature, so that the remote observation is facilitated. In addition to this, CsPbBr3/EuPO4The dual phase glass-ceramic was confirmed to have excellent thermal stability. These results indicate that CsPbBr3/EuPO4The biphase glass ceramic is an ideal fluorescent temperature probe material and has wide application prospect in the field of temperature detection.
Drawings
FIG. 1: CsPbBr3/EuPO4X-ray diffraction pattern of the dual phase glass-ceramic.
FIG. 2: CsPbBr3/EuPO4Scanning electron microscope image of the biphase glass ceramic.
FIG. 3: CsPbBr3/EuPO4The excitation spectrum of the two-phase glass ceramic has a monitoring wavelength of 516nm and 611 nm.
FIG. 4: CsPbBr under 393nm excitation3/EuPO4Emission spectrum of the duplex glass-ceramic.
FIG. 5: CsPbBr3/EuPO4The temperature change of the variable-temperature emission spectrum of the double-phase glass ceramic is 303K-483K, and the excitation is 393 nm.
FIG. 6: CsPbBr3(516nm) and Eu3+Ionic Eu3+：5D0→7F1(593nm)，5D0→7F2(611nm)，5D0→7F4(700nm) transition emission intensity histogram.
FIG. 7: FIR ratio of emission intensity obtained by experimental measured value and fitting611/516Graph with temperature.
FIG. 8: and calculating the obtained absolute sensitivity and relative sensitivity and corresponding fitting curves.
Detailed Description
Example 1: pure P2O5、SiO2、Al2O3、Cs2CO3、PbBr2、SrCO3、NaBr、EuCl3Powder of 30P2O5；20SiO2；10Al2O3；10Cs2CO3；10PbBr2；5SrCO3；5NaBr；10EuCl3Weighing the components according to the molar ratio, mixing the components in an agate ball-milling tank, fully grinding the mixture uniformly, putting the mixture in an alumina crucible, putting the alumina crucible in a resistance furnace, heating the mixture to 1000 ℃, keeping the temperature for 2 hours to melt the mixture, then quickly pouring the molten liquid into a mold for molding, obtaining block-shaped glass ceramics in a self-crystallization mode, finally putting the obtained glass ceramics in the resistance furnace, annealing the glass ceramics at 200 ℃ to eliminate internal stress, cooling the glass ceramics along with the furnace, cutting the glass ceramics into blocks to obtain CsPbBr3/EuPO4A twinned phase glass-ceramic.
X-ray diffraction data show that C is precipitated in the glass matrixsPbBr3And EuPO4Crystalline phase (as shown in fig. 1). Scanning electron micrographs show CsPbBr3And EuPO4The distribution of the crystalline phases in the glass matrix (as shown in fig. 2). The samples were surface polished and their room temperature excitation and emission were measured using an FLS920 fluorescence spectrometer. In monitoring Eu3+Detection of the excitation spectrum emitted by the ion 611nm corresponds to Eu3+-O2-Charge transport and Eu3+: 4f → 4f absorption transition (the wavelength with the highest intensity is at 393 nanometers) excitation band (as shown in FIG. 3). In monitoring CsPbBr3At 516nm, the corresponding CsPbBr is detected3The excitation band of the transition (as shown in figure 4). At 393nm excitation the emission spectrum appears corresponding to Eu3+:5D0→7FJ(J ═ 1,2,3,4) strong red emission of the transition (central wavelengths correspond to 593 nm,611nm, 652 nm, 700nm, respectively). Under the excitation of ultraviolet light with the wavelength of 393 nanometers, the variable temperature emission spectrum of the ultraviolet light is measured, and the temperature change range is 303K to 483K. CsPbBr was observed3The fluorescence intensity of (1) is reduced very significantly, whereas Eu3+Only slightly reduced in emission intensity (as shown in fig. 5). In CsPbBr3And Eu3+This can be further confirmed in ion transition emission intensity histograms (as shown in figure 6). Eu (Eu)3+Middle 611nm and CsPbBr3The ratio of the fluorescence intensities of the two peaks at 516nm was significant with temperature (as shown in FIG. 7). The fluorescence intensity ratio of the two is used as a temperature detection signal, and the highest absolute sensitivity reaches 0.082K-1The highest relative sensitivity reaches 1.8 percent K-1(as shown in fig. 8).
Example 2: pure P2O5、SiO2、Al2O3、Cs2CO3、PbBr2、EuCl3Powder of 20P2O5；20SiO2；10Al2O3；20Cs2CO3；20PbBr2；10EuCl3The mixture ratio (mol ratio) is weighed, mixed in an agate ball-milling tank, fully and uniformly ground, placed in an alumina crucible, placed in a resistance furnace and heated to 1300 ℃, and then the mixture is maintainedHeating for 2 hr to melt, pouring the molten liquid into mold to form, self-crystallizing to obtain glass ceramic block, annealing at 200 deg.c in a resistance furnace to eliminate internal stress, cooling, and cutting into CsPbBr3/EuPO4A twinned phase glass-ceramic. Testing the variable-temperature emission spectrum of the dual-crystal-phase glass ceramic and utilizing Eu3+Middle 611nm and CsPbBr3The fluorescence intensity ratio of two peaks at 516nm is used as a temperature detection signal, and the highest absolute sensitivity reaches 0.064K-1The highest relative sensitivity reaches 1.5 percent K-1。
Example 3: pure P2O5、Al2O3、Cs2CO3、PbBr2、NaBr、EuCl3Powder of 40P2O5；5Al2O3；15Cs2CO3；10PbBr2；10NaBr；20EuCl3Weighing the components according to the molar ratio, mixing the components in an agate ball-milling tank, fully grinding the mixture uniformly, putting the mixture in an alumina crucible, putting the alumina crucible in a resistance furnace, heating the mixture to 900 ℃, preserving the heat for 4 hours to melt the mixture, then quickly pouring the molten liquid into a mold for molding, obtaining block-shaped glass ceramics in a self-crystallization mode, finally putting the obtained glass ceramics in the resistance furnace, annealing the glass ceramics at 300 ℃ to eliminate the internal stress, cooling the glass ceramics along with the furnace, cutting the glass ceramics into blocks to obtain CsPbBr3/EuPO4A twinned phase glass-ceramic. Testing the variable-temperature emission spectrum of the dual-crystal-phase glass ceramic and utilizing Eu3+Middle 611nm and CsPbBr3The fluorescence intensity ratio of two peaks at 516nm is used as a temperature detection signal, and the highest absolute sensitivity reaches 0.036K-1The highest relative sensitivity reaches 1.2 percent K-1。
Example 4: pure P2O5、SiO2、Cs2CO3、PbBr2、NaBr、SrCO3、EuCl3Powder of 10P2O5；40SiO2；20Cs2CO3；10PbBr2；10NaBr；5SrCO3；5EuCl3Weighing the components according to the molar ratio, mixing the components in an agate ball-milling tank, fully grinding the mixture uniformly, putting the mixture in an alumina crucible, putting the alumina crucible in a resistance furnace, heating the mixture to 1400 ℃, preserving the heat for 4 hours to enable the mixture to be molten, then quickly pouring the molten liquid into a mold to be molded, obtaining block-shaped glass ceramics in a self-crystallization mode, finally putting the obtained glass ceramics in the resistance furnace, annealing the glass ceramics at 400 ℃ to eliminate internal stress, cooling the glass ceramics along with the furnace, cutting the glass ceramics into blocks to obtain CsPbBr3/EuPO4A twinned phase glass-ceramic. Testing the variable-temperature emission spectrum of the dual-crystal-phase glass ceramic and utilizing Eu3+Middle 611nm and CsPbBr3The fluorescence intensity ratio of two peaks at 516nm is used as a temperature detection signal, and the highest absolute sensitivity reaches 0.022K-1The highest relative sensitivity reaches 0.8 percent K-1。
Claims (4)
1. CsPbBr-containing material3/EuPO4A dual-crystalline phase glass-ceramic having a glass matrix with a glass component content as follows:
10-60mol％P2O5；0-40mol％SiO2；0-40mol％Al2O3；0-30mol％Cs2CO3；
0-30mol％PbBr2；0-30mol％SrCO3；5-30mol％NaBr；5-30mol％EuCl3the total mole amount of the above components is 100 mol%.
2. The CsPbBr-containing material according to claim 13/EuPO4A dual-crystalline phase glass-ceramic characterized by: the glass component of the glass matrix is preferably as follows:
20-50％mol％P2O5；5-30mol％SiO2；5-30mol％Al2O3；5-25mol％Cs2CO3；
5-25mol％PbBr2；5-25mol％SrCO3；5-25mol％NaBr；10-25mol％EuCl3。
3. a composition according to claim 1, comprisingCsPbBr3/EuPO4A dual crystalline phase glass-ceramic characterized by a microstructure characterized by CsPbBr3/EuPO4The microcrystals are uniformly embedded in the glass matrix.
4. A CsPbBr-containing material as defined in any one of claims 1 to 33/EuPO4The application of glass ceramic containing double crystal phases is characterized in that the glass ceramic containing CsPbBr is irradiated by ultraviolet light with the wavelength of 393nm3/EuPO4Glass-ceramics with a dual crystal phase, the temperature of which is increased from 303K to 483K, CsPbBr of the material3The green light emission intensity is reduced very obviously, Eu3+The red emission intensity of the fluorescent material is only slightly reduced, and the fluorescence is changed from green to red, CsPbBr3At 516nm and Eu3+：5D0→7F2The fluorescence intensity ratio emitted at 611nm changes obviously with temperature, and the ambient temperature can be measured by using the fluorescence intensity ratio of the two as a temperature detection signal.
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| CN109553303A (en) * | 2018-12-21 | 2019-04-02 | 温州大学 | A kind of CsPb (1-x) SnXBr3 quantum dot microcrystal glass material |
| CN110642515B (en) * | 2019-09-29 | 2022-02-01 | 昆明理工大学 | Preparation method and application of all-inorganic perovskite quantum dot glass |
| CN111732341B (en) * | 2020-07-03 | 2022-05-31 | 福建师范大学 | Double-crystal-phase microcrystalline glass material and preparation method thereof |
| CN112322287B (en) * | 2020-10-16 | 2022-11-08 | 厦门华厦学院 | Temperature sensing material and preparation method and application thereof |
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