CN114656964B - Self-calibration fluorescent temperature measurement material and preparation method thereof - Google Patents
Self-calibration fluorescent temperature measurement material and preparation method thereof Download PDFInfo
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- 238000009529 body temperature measurement Methods 0.000 title claims abstract description 37
- 239000000463 material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 230000005284 excitation Effects 0.000 claims abstract description 3
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000004570 mortar (masonry) Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 8
- 229910052593 corundum Inorganic materials 0.000 claims description 8
- 239000010431 corundum Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 229910003443 lutetium oxide Inorganic materials 0.000 claims description 6
- MPARYNQUYZOBJM-UHFFFAOYSA-N oxo(oxolutetiooxy)lutetium Chemical compound O=[Lu]O[Lu]=O MPARYNQUYZOBJM-UHFFFAOYSA-N 0.000 claims description 6
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 6
- 229940075624 ytterbium oxide Drugs 0.000 claims description 6
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 5
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 3
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims 1
- 230000008878 coupling Effects 0.000 abstract description 20
- 238000010168 coupling process Methods 0.000 abstract description 20
- 238000005859 coupling reaction Methods 0.000 abstract description 20
- 230000035945 sensitivity Effects 0.000 abstract description 12
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 9
- -1 rare earth ions Chemical class 0.000 abstract description 6
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 3
- 150000002910 rare earth metals Chemical class 0.000 abstract description 3
- DLWVQSOQDMSDHN-UHFFFAOYSA-N [Lu].[Li] Chemical compound [Lu].[Li] DLWVQSOQDMSDHN-UHFFFAOYSA-N 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- DFGKGUXTPFWHIX-UHFFFAOYSA-N 6-[2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]acetyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)C1=CC2=C(NC(O2)=O)C=C1 DFGKGUXTPFWHIX-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000004861 thermometry Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
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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
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- Chemical & Material Sciences (AREA)
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- Engineering & Computer Science (AREA)
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention belongs to the field of fluorescence temperature sensing, and discloses a self-calibration fluorescence temperature measurement material and a preparation method thereof. The invention aims to provide an efficient fluorescent temperature measurement matrix material, which is doped with rare earth ions Er together 3+ /Tm 3+ /Yb 3+ When the self-calibration fluorescence intensity ratio temperature measurement is realized by utilizing the thermal coupling energy level pair and the non-thermal coupling energy level pair from different rare earth ions, and the highest sensitivity is not limited by Boltzmann distribution. Under the excitation of near infrared laser, the rare earth doped lutetium lithium molybdate has small emission peak overlapping of corresponding temperature measuring energy level, can keep higher relative sensitivity in different temperature areas, and is beneficial to realizing the fluorescent temperature measurement application of high sensitivity, high precision and extremely wide temperature areas.
Description
Technical Field
The invention belongs to the field of fluorescence temperature sensing, and particularly relates to a self-calibration fluorescence temperature measuring material with high sensitivity and a preparation method thereof.
Background
Accurate real-time temperature monitoring plays an important role in ensuring product quality, saving energy, promoting production and the like. Compared with the traditional thermocouple and infrared radiation temperature measurement, the fluorescence temperature measurement technology has the characteristics of non-contact temperature measurement, large-scale imaging, wide dynamic range, high response speed, high precision and the like, and therefore, has the advantages of high temperature measurement fieldHas wide application prospect. The fluorescence temperature measurement is to monitor physical quantities such as luminous intensity, fluorescence lifetime, emission bandwidth, peak position movement, polarization property, fluorescence intensity ratio and the like by utilizing the dependency relationship between luminous characteristics and temperature, so as to obtain corresponding temperature conditions. The Fluorescence Intensity Ratio (FIR) temperature measurement has self-calibration characteristic, is not interfered by external environment, and is realized by a pair of thermal coupling energy levels of rare earth ions. However, the thermal coupling energy level difference DeltaE is limited to the range of 200-2000cm by Boltzmann distribution based on the fluorescence intensity ratio temperature measurement of the thermal coupling energy level -1 Between which the theoretical highest relative sensitivity Sr (sr=Δe/kT is determined 2 ) Should not exceed 2878/T 2 The application of fluorescence temperature measurement with high sensitivity is restricted.
In order to further improve the temperature measurement performance, fluorescence temperature measurement is considered to be carried out on different temperature areas by utilizing a thermal coupling energy level pair and a non-thermal coupling energy level pair. Most of rare earth ions are non-thermal coupling energy levels, so that the selection of the non-thermal coupling energy level pairs is richer, the non-thermal coupling energy levels of different ions are not limited by Boltzmann distribution to the greatest extent, and the non-thermal coupling energy levels of different ions also show certain temperature dependence characteristics, which are mostly caused by the difference of thermal quenching or the energy transfer process. Therefore, the fluorescence temperature measurement is carried out by utilizing the non-thermal coupling energy level pairs from different ions, so that the sensitivity is further improved, the temperature measurement precision is ensured, the temperature measurement error is reduced, and the high-performance fluorescence intensity ratio temperature measurement is realized.
Disclosure of Invention
The invention aims to provide an efficient fluorescent temperature measurement matrix material, which is doped with rare earth ions Er together 3+ /Tm 3 + /Yb 3+ When the temperature measurement device is used, the high-sensitivity fluorescence intensity ratio temperature measurement can be realized by utilizing the thermal coupling energy level pair and the non-thermal coupling energy level pair from different rare earth ions.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a self-calibrating fluorescent temperature measurement material, the chemical formula of the self-calibrating fluorescent temperature measurement material is: liLu 0.93-x-y (MoO 4 ) 2 :xEr 3+ ,yTm 3+ ,0.07Yb 3+ Wherein x is more than or equal to 0.002 and less than or equal to 0.01,0, and y is more than or equal to 0.02; the saidx and y each represent Er 3+ 、Tm 3+ Substitution of Lu 3+ Molar content of (2).
A preparation method of a self-calibration fluorescent temperature measurement material comprises the following steps:
1) According to the chemical formula LiLu 0.93-x-y (MoO 4 ) 2 :xEr 3+ ,yTm 3+ ,0.07Yb 3+ The stoichiometric ratio of each element is respectively measured to be lithium-containing compound, lutetium oxide, molybdenum-containing compound, erbium oxide, thulium oxide and ytterbium oxide;
2) Placing the powder weighed in the step 1) into an agate mortar, adding a small amount of absolute ethyl alcohol, and grinding to uniformly mix the powder to obtain a mixture;
3) Placing the mixture obtained in the step 2) in a corundum crucible, then placing the corundum crucible in a muffle furnace, sintering at a high temperature, and cooling to room temperature;
4) And 3) grinding the solid sample obtained in the step 3) in an agate mortar to obtain a target product.
Preferably, the above preparation method, the lithium-containing compound is selected from lithium carbonate or lithium oxide.
Preferably, the above preparation method, the molybdenum-containing compound is selected from molybdenum trioxide or molybdenum trioxide.
Preferably, in the above preparation method, in step 2), the grinding time is 30 to 60 minutes.
Preferably, in the above preparation method, in step 3), the atmosphere of high-temperature sintering is an air atmosphere.
Preferably, in the above preparation method, in step 3), the high temperature sintering is performed at 900-1100 ℃, the temperature rising rate is 3-5 ℃/min, and the calcination time is 3-6 h.
Preferably, in the above preparation method, in step 4), the grinding time is 5 to 10min.
The beneficial effects of the invention are as follows:
according to the invention, lutetium lithium molybdate is used as a matrix material, and the material is stable in physical and chemical properties, simple in preparation process, high-temperature-resistant and environment-friendly. When co-doping Er 3+ /Tm 3+ /Yb 3+ When excited by near infrared 972nm laser, the emission peaks overlap relativelyThe fluorescent temperature measurement device is small, the signal discrimination of fluorescent temperature measurement can be improved, and the temperature measurement error is reduced; respectively utilize Er 3+ 、Tm 3+ The thermal coupling energy level pair and the non-thermal coupling energy level pair can realize high-sensitivity and high-precision temperature measurement in different temperature areas.
Drawings
FIG. 1 is an XRD pattern of the fluorescent thermometry materials prepared in example 1 and example 2.
FIG. 2 is an upconversion temperature change spectrum of the fluorescent temperature measuring material under near infrared excitation in example 5.
FIG. 3 is a graph of Er according to example 5 3+ : 2 H 11/2 / 4 S 3/2 Thermal coupling energy level versus calculated fluorescence thermometry sensitivity versus temperature.
FIG. 4 is Er in example 5 3+ /Tm 3+ The fluorescence intensity ratio of the non-thermally coupled energy level pairs is plotted against temperature T.
Detailed Description
Example 1
The chemical formula of the fluorescent temperature measuring material of the embodiment is LiLu 0.915 (MoO 4 ) 2 :0.005Er 3+ ,0.01Tm 3+ ,0.07Yb 3+ The preparation method comprises the following steps:
respectively weighing 0.0739g of lithium carbonate, 0.3641g of lutetium oxide, 0.5758g of molybdenum trioxide, 0.0019g of erbium oxide, 0.0039g of thulium oxide and 0.0276g of ytterbium oxide; placing the weighed powder into an agate mortar, adding 1ml of absolute ethyl alcohol, grinding clockwise for 30min to uniformly mix, transferring into a corundum crucible, placing the crucible into a high-temperature muffle furnace, heating at a heating rate of 3 ℃/min, heating to 900 ℃ and calcining for 4h, and cooling to room temperature along with the furnace; and (3) grinding the obtained solid sample in an agate mortar for 5min to obtain the fluorescent temperature measuring material of the target product.
Subjecting the sample to phase analysis to obtain XRD patterns as shown in Tm in FIG. 1 3+ : as shown in the 1% graph, compared with a standard pdf card (JPCDS No. 23-1192), diffraction peak positions and diffraction intensities are in one-to-one correspondence, and the pure-phase rare earth doped fluorescent temperature measurement material is proved to be synthesized.
Example 2
The chemical formula of the fluorescent temperature measuring material of the embodiment is LiLu 0.905 (MoO 4 ) 2 :0.005Er 3+ ,0.02Tm 3+ ,0.07Yb 3+ The preparation method comprises the following steps:
respectively weighing 0.0739g of lithium carbonate, 0.3601g of lutetium oxide, 0.5758g of molybdenum trioxide, 0.0019g of erbium oxide, 0.0077g of thulium oxide and 0.0276g of ytterbium oxide; placing the weighed powder into an agate mortar, adding 2ml of absolute ethyl alcohol, grinding clockwise for 40min to uniformly mix, transferring into a corundum crucible, placing the crucible into a high-temperature muffle furnace, heating at a heating rate of 5 ℃/min, heating to 900 ℃ and calcining for 4h, and cooling to room temperature along with the furnace; and (3) grinding the obtained solid sample in an agate mortar for 10min to obtain the fluorescent temperature measuring material of the target product.
Subjecting the sample to phase analysis to obtain XRD patterns as shown in Tm in FIG. 1 3+ : as shown in the 2% graph, compared with a standard pdf card (JPCDS No. 23-1192), diffraction peak positions and diffraction intensities are in one-to-one correspondence, and the pure-phase rare earth doped fluorescent temperature measurement material is proved to be synthesized.
Example 3
The chemical formula of the fluorescent temperature measuring material of the embodiment is LiLu 0.91 (MoO 4 ) 2 :0.01Er 3+ ,0.01Tm 3+ ,0.07Yb 3+ The preparation method comprises the following steps:
respectively weighing 0.0739g of lithium carbonate, 0.3621g of lutetium oxide, 0.4798g of molybdenum trioxide, 0.0038g of erbium oxide, 0.0039g of thulium oxide and 0.0276g of ytterbium oxide; placing the weighed powder into an agate mortar, adding 1ml of absolute ethyl alcohol, grinding clockwise for 35min to uniformly mix the powder, transferring the powder into a corundum crucible, placing the crucible into a high-temperature muffle furnace, heating the crucible at a heating rate of 3 ℃/min, heating the crucible to 1100 ℃ and calcining the crucible for 3h, and cooling the crucible to room temperature along with the furnace; and (3) grinding the obtained solid sample in an agate mortar for 15min to obtain the fluorescent temperature measuring material of the target product.
Example 4
The chemical formula of the fluorescent temperature measuring material of the embodiment is LiLu 0.916 (MoO 4 ) 2 :0.004Er 3+ ,0.01Tm 3+ ,0.07Yb 3+ The preparation method comprises the following steps:
respectively weighing 0.0299g of lithium oxide, 0.3645g of lutetium oxide, 0.5758g of molybdenum trioxide, 0.0015g of erbium oxide, 0.0039g of thulium oxide and 0.0276g of ytterbium oxide; placing the weighed powder into an agate mortar, adding 2ml of absolute ethyl alcohol, grinding clockwise for 45min to uniformly mix the powder, transferring the powder into a corundum crucible, placing the crucible into a high-temperature muffle furnace, heating the crucible to 1000 ℃ at a heating rate of 4 ℃/min, calcining the crucible for 4h, and cooling the crucible to room temperature along with the furnace; and (3) grinding the obtained solid sample in an agate mortar for 10min to obtain the fluorescent temperature measuring material of the target product.
Example 5
The fluorescent temperature measurement material prepared in the embodiment 1 is placed in a testing device, near infrared laser with the central wavelength of 972nm is used as a pumping light source, the optical path is adjusted, the optical path is excited, an up-conversion temperature-changing spectrum is obtained within the range of 300.3-563K and is shown as a graph in fig. 2, and sensitivity calculation is carried out by using a thermal coupling energy level pair and a non-thermal coupling energy level pair respectively. FIG. 3 shows Er-based 3+ : 2 H 11/2 / 4 S 3/2 The sensitivity of thermal coupling energy level calculation is changed along with the temperature, and Er is found out 3+ The relative sensitivity of (2) reaches a maximum at a temperature of 563K, the maximum being 4.54X 10 -3 K -1 . FIG. 4 shows Er 3+ : 2 H 11/2 And Tm 3+ : 1 G 4 The fluorescence intensity ratio of the non-thermally coupled energy level pairs is fitted as a function of the temperature T, and the highest relative sensitivity is calculated to be reached at 463K at a value of 9.9X10 -2 K -1 。
Claims (3)
1. The self-calibration fluorescent temperature measurement material is characterized by having a chemical formula as follows: liLu 0.93-x-y (MoO 4 ) 2 :xEr 3+ , yTm 3+ , 0.07Yb 3+ The method comprises the steps of carrying out a first treatment on the surface of the Wherein x=0.005, y=0.01; or x=0.005, y=0.02; or x=0.01, y=0.01; or x=0.004, y=0.01; under the excitation of near infrared 972 and nm laser, the up-conversion temperature change spectrum is measured in the range of 300.3-563-K;
the preparation method of the self-calibration fluorescent temperature measurement material comprises the following steps:
1) According to the chemical formula LiLu 0.93-x-y (MoO 4 ) 2 :xEr 3+ , yTm 3+ , 0.07Yb 3+ The stoichiometric ratio of each element is respectively measured to be lithium-containing compound, lutetium oxide, molybdenum-containing compound, erbium oxide, thulium oxide and ytterbium oxide;
2) Placing the powder weighed in the step 1) into an agate mortar, adding a small amount of absolute ethyl alcohol, and grinding for 30-60 min to uniformly mix the powder to obtain a mixture;
3) Placing the mixture obtained in the step 2) in a corundum crucible, then placing the corundum crucible in a muffle furnace, carrying out high-temperature calcination for 3-6 hours in an air atmosphere at a heating rate of 3-5 ℃/min, and cooling to room temperature;
4) And (3) grinding the solid sample obtained in the step (3) in an agate mortar for 5-10 min to obtain a target product.
2. A self-calibrating fluorescent temperature measurement material according to claim 1, wherein: the lithium-containing compound is selected from lithium carbonate or lithium oxide.
3. A self-calibrating fluorescent temperature measurement material according to claim 1, wherein: the molybdenum-containing compound is selected from molybdenum trioxide or molybdenum trioxide.
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Linlin Li et al..Synthesis and luminescent properties of high brightness MRE(MoO4)2:Eu3+ (M=Li,Na,K * |
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