CN114874770A - Fluorescent material for optical temperature sensing and preparation method thereof - Google Patents
Fluorescent material for optical temperature sensing and preparation method thereof Download PDFInfo
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- CN114874770A CN114874770A CN202210517288.4A CN202210517288A CN114874770A CN 114874770 A CN114874770 A CN 114874770A CN 202210517288 A CN202210517288 A CN 202210517288A CN 114874770 A CN114874770 A CN 114874770A
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- temperature sensing
- europium
- strontium
- aluminum
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- 239000000463 material Substances 0.000 title claims abstract description 47
- 230000003287 optical effect Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 230000035945 sensitivity Effects 0.000 claims abstract description 15
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 7
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 5
- 229910001940 europium oxide Inorganic materials 0.000 claims description 5
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- PPQREHKVAOVYBT-UHFFFAOYSA-H dialuminum;tricarbonate Chemical compound [Al+3].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O PPQREHKVAOVYBT-UHFFFAOYSA-H 0.000 claims description 4
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 4
- UBXAKNTVXQMEAG-UHFFFAOYSA-L strontium sulfate Chemical compound [Sr+2].[O-]S([O-])(=O)=O UBXAKNTVXQMEAG-UHFFFAOYSA-L 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 238000004020 luminiscence type Methods 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- 229940009827 aluminum acetate Drugs 0.000 claims description 2
- 229940118662 aluminum carbonate Drugs 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- PVDYMOCCGHXJAK-UHFFFAOYSA-H europium(3+);oxalate Chemical compound [Eu+3].[Eu+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O PVDYMOCCGHXJAK-UHFFFAOYSA-H 0.000 claims description 2
- KJNZTHUWRRLWOA-UHFFFAOYSA-K europium(3+);phosphate Chemical compound [Eu+3].[O-]P([O-])([O-])=O KJNZTHUWRRLWOA-UHFFFAOYSA-K 0.000 claims description 2
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 claims description 2
- NNMXSTWQJRPBJZ-UHFFFAOYSA-K europium(iii) chloride Chemical compound Cl[Eu](Cl)Cl NNMXSTWQJRPBJZ-UHFFFAOYSA-K 0.000 claims description 2
- WLYAEQLCCOGBPV-UHFFFAOYSA-N europium;sulfuric acid Chemical compound [Eu].OS(O)(=O)=O WLYAEQLCCOGBPV-UHFFFAOYSA-N 0.000 claims description 2
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 2
- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 claims description 2
- 229910001866 strontium hydroxide Inorganic materials 0.000 claims description 2
- UHCGLDSRFKGERO-UHFFFAOYSA-N strontium peroxide Chemical compound [Sr+2].[O-][O-] UHCGLDSRFKGERO-UHFFFAOYSA-N 0.000 claims description 2
- VTBSJEPGLHXIIS-UHFFFAOYSA-L strontium;sulfite Chemical compound [Sr+2].[O-]S([O-])=O VTBSJEPGLHXIIS-UHFFFAOYSA-L 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 1
- -1 europium ion Chemical class 0.000 abstract description 8
- 239000011540 sensing material Substances 0.000 abstract 2
- 230000004913 activation Effects 0.000 abstract 1
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000009529 body temperature measurement Methods 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910003668 SrAl Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- 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
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7734—Aluminates
-
- 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)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses an optical temperature sensing material based on mixed valence europium ion activation and a preparation method thereof. The chemical general formula of the optical temperature sensing material is Sr (1‑x) Eu x Al 2 O 4 Wherein x is more than or equal to 0.001 and less than or equal to 0.3, the preparation method of the material is a high-temperature solid phase method, namely, the raw materials are uniformly mixed according to the stoichiometric ratio, a sintered product is obtained after high-temperature calcination is carried out under normal pressure and air atmosphere, and the sintered product is further ground and screened to obtain the material. The material can be excited by ultraviolet light and simultaneously shows characteristic emission of divalent europium ions and trivalent europium ions, and main emission peaks are respectively positioned at 519nm and 619 nm. The material has obvious luminescent temperature dependence characteristic, and the absolute temperature sensitivity can reach 0.067K ‑1 The relative temperature sensitivity can reach 1.5 percent K ‑1 And has wide application prospect in the field of optical temperature sensing.
Description
Technical Field
The invention relates to a fluorescent material for optical temperature sensing and a preparation method thereof, belonging to the technical field of fluorescent materials and preparation thereof.
Background
Temperature plays an important role in biomedicine, industrial production and human daily life as a basic physical quantity of thermodynamics. Conventional thermal contact thermometers, such as liquid filled glass thermometers, thermocouples, thermal resistors, etc., have been the primary temperature measuring devices for recent decades. Contact thermometers based on the principle of thermal equilibrium between a sensor and an object typically require convective heat transfer to effect a temperature measurement, which may result in a change in the local temperature of the measured object during the measurement process. Moreover, these thermometers are not easily miniaturized and therefore cannot be used for temperature measurement of batteries, minute electronic components, fast moving objects, and the like. In addition, they also fail to meet temperature control and measurement requirements under extreme conditions such as corrosive environments and electromagnetic interference environments. Therefore, the development of the non-contact temperature sensor with high response speed and high temperature sensitivity has important practical significance. Non-contact optical temperature sensing technology is an effective method for temperature measurement under extreme conditions, micro-scale environments and other special circumstances. Remote temperature monitoring can be achieved by monitoring changes in various temperature-sensitive optical parameters including luminous intensity, fluorescence lifetime, emission bandwidth and peak position.
Disclosure of Invention
The invention provides a mixed-valence europium ion activated fluorescent material and a preparation method thereof based on a Fluorescence Intensity Ratio (FIR) principle and the self-reduction characteristic of europium ions. The material can be excited by ultraviolet light, has emission peaks in a blue light wave band and a red light wave band, has good distinguishability and temperature sensitivity, and can be used in the field of optical temperature sensing.
The detailed scheme of the invention is as follows:
the chemical general formula of the fluorescent material for optical temperature sensing is Sr (1-x) Eu x Al 2 O 4 Wherein x is more than or equal to 0.001 and less than or equal to 0.3.
The invention relates to a preparation method of a fluorescent material for optical temperature sensing, which comprises the following specific steps:
(1) weighing compound raw materials containing each element according to the stoichiometric ratio of each element in the chemical general formula of the fluorescent material;
(2) mixing the raw materials in the step (1), and then ball-milling the mixture in a ball mill until the mixture is uniform;
(3) placing the raw material mixture subjected to ball milling in the step (2) in a corundum crucible;
(4) placing the corundum crucible in the step (3) in a muffle furnace, and calcining in the atmosphere of normal pressure and air;
(5) and (5) further performing ball milling and screening on the sintered product obtained in the step (4) to obtain the fluorescent material.
Further, the raw material containing strontium element in step (1) is at least one of strontium oxide, strontium peroxide, strontium hydroxide, strontium sulfate, strontium sulfite, strontium carbonate and strontium nitrate, preferably strontium oxide.
Further, the preparation method of the fluorescent material for optical temperature sensing described in step (1) is characterized by: the raw material containing aluminum element is at least one of aluminum oxide, aluminum hydroxide, aluminum sulfate, aluminum nitrate, aluminum acetate, aluminum chloride and basic aluminum carbonate, and preferably is aluminum oxide.
Further, the preparation method of the fluorescent material for optical temperature sensing described in step (1) is characterized in that: the raw material containing europium element is at least one of europium oxide, europium chloride, europium sulfate, europium nitrate, europium oxalate and europium phosphate, and preferably europium oxide.
Further, the raw material purity in the step (1) is Chemical Purity (CP) or above grade.
Further, the ball milling time in the step (2) is 120 to 480 minutes.
Further, the calcination temperature in the step (4) is 1350 to 1550 ℃, and the holding time is 2 to 18 hours.
Further, the fluorescent material in step (5) can be excited by deep ultraviolet or near ultraviolet, and the main emission peak is located in green and red light bands.
Further, the fluorescent material described in step (5) has good luminescence temperature dependence characteristics, and a temperature sensitivity standard curve can be established based on the luminescence temperature dependence characteristics, and the temperature sensitivity of the material can be calculated.
The main advantages of the invention are:
(1) the fluorescent material for optical temperature sensing is prepared in the atmosphere of air and normal pressure, the preparation process is simple, the reaction process is safe and controllable, and the industrial production is favorably realized;
(2) the fluorescent material for optical temperature sensing provided by the invention can be excited by ultraviolet light, simultaneously shows characteristic emission of divalent europium ions and trivalent europium ions, and has emission peaks respectively positioned in a green light waveband of 519nm and a red light waveband of 619nm, so that the fluorescent material has good distinguishability;
(3) the fluorescent material for optical temperature sensing provided by the invention has good luminous temperature dependence characteristic and higher temperature sensitivity, and has wide application prospect in the field of optical temperature sensing.
Drawings
FIG. 1 shows a phosphor Sr for optical temperature sensing according to the present invention 0.98 Al 2 O 4 :0.02Eu 2+/3+ XRD spectrum of (1);
FIG. 2 shows a phosphor Sr for optical temperature sensing according to the present invention 0.98 Al 2 O 4 :0.02Eu 2+/3+ XPS spectra of (a);
FIG. 3 shows the phosphor Sr for optical temperature sensing according to the present invention 0.98 Al 2 O 4 :0.02Eu 2+/3+ Absolute sensitivity (S) of a ) And relative sensitivity (S) r ) A curve;
FIG. 4 shows a phosphor Sr for optical temperature sensing according to the present invention 0.98 Al 2 O 4 :0.02Eu 2+/3+ CIE color coordinates of (c).
Detailed Description
In order that the invention may be more readily understood, reference will now be made in detail to the following examples.
Example 1
Preparation of fluorescent material Sr for optical temperature sensing 0.98 Al 2 O 4 :0.02Eu 2+/3+ The method comprises the following specific steps:
strontium oxide, aluminum oxide and europium oxide are used as raw materials, the raw materials are weighed and mixed according to the stoichiometric ratio of the strontium, the aluminum and the europium in the chemical formula of 0.98:2:0.02, and the mixed raw materials are subjected to ball milling for 120 minutes. And transferring the raw materials subjected to the full ball milling into a corundum crucible, placing the crucible into a muffle furnace, sintering for 4 hours at 1350 ℃ under normal pressure and air atmosphere, and naturally cooling to room temperature to obtain a sintered product. Ball-milling the sintered product for 120 minutes, and sieving the ball-milled product with a 200-mesh sieveObtaining Sr after separation 0.98 Al 2 O 4 :0.02Eu 2+/3+ A fluorescent material.
Sr in this example 0.98 Al 2 O 4 :0.02Eu 2+/3+ The XRD spectrum of the fluorescent material is shown in figure 1. The XRD diffraction peak of the prepared fluorescent material is well matched with the standard card JCPDS34-379, namely the prepared Sr 0.98 Al 2 O 4 :0.02Eu 2+/3+ The phase composition of the fluorescent material is SrAl 2 O 4 A single pure phase.
Sr in this example 0.98 Al 2 O 4 :0.02Eu 2+/3+ The XPS spectrum of the fluorescent material is shown in FIG. 2. The characteristic binding energy peaks in the figure at 1124.9eV and 1134.6eV correspond to the 3d of divalent and trivalent europium, respectively 5/2 Electronic configuration, namely divalent europium and trivalent europium ions exist in the fluorescent material at the same time.
Sr in this example 0.98 Al 2 O 4 :0.02Eu 2+/3+ Absolute sensitivity (S) of fluorescent materials a ) And relative sensitivity (S) r ) The curves are shown in FIG. 3. The absolute temperature sensitivity of the fluorescent material can reach 0.067K at most -1 The sensitivity to the relative temperature can reach 1.5 percent K at most -1 。
The CIE color coordinates of the Sr0.98Al2O4:0.02Eu2+/3+ fluorescent material related to the embodiment are shown in figure 4. Under the excitation of 365nm wavelength ultraviolet light, as the test temperature is increased from 298K to 473K, the luminescent color of the fluorescent material is changed from yellow-green light to white light, the corresponding color coordinate is changed from (0.2973,0.4473) to (0.3287,0.2527), and the correlated color temperature is reduced from 6562K to 5684K.
The foregoing examples are provided for the purpose of illustration and description of the invention only and are not intended as a limitation thereon.
Claims (8)
1. A fluorescent material for optical temperature sensing, characterized by: the chemical general formula of the fluorescent material is Sr (1-x) Eu x Al 2 O 4 Wherein x is more than or equal to 0.001 and less than or equal to 0.3.
2. A fluorescent material for optical temperature sensing according to claim 1, characterized in that: the fluorescent material can be excited by deep ultraviolet or near ultraviolet light, and the main emission peak is positioned in the green light and red light wave bands.
3. A fluorescent material for optical temperature sensing according to claim 1, characterized in that: based on the good luminescence temperature dependence of the material, a temperature sensitivity standard curve can be established, and the temperature sensitivity of the material can be calculated.
4. A method of preparing a fluorescent material for optical temperature sensing according to claim 1, 2 or 3, characterized in that: weighing compound raw materials containing each element according to the stoichiometric ratio of each element in the chemical general formula, carrying out ball milling and mixing to be uniform, calcining in normal pressure and air atmosphere, and further carrying out ball milling and screening on the sintered product to obtain the material.
5. The method for preparing a fluorescent material for optical temperature sensing according to claim 4, wherein: the raw material containing strontium element is at least one of strontium oxide, strontium peroxide, strontium hydroxide, strontium sulfate, strontium sulfite, strontium carbonate and strontium nitrate, preferably strontium oxide.
6. The method for preparing a fluorescent material for optical temperature sensing according to claim 4, wherein: the raw material containing aluminum element is at least one of aluminum oxide, aluminum hydroxide, aluminum sulfate, aluminum nitrate, aluminum acetate, aluminum chloride and basic aluminum carbonate, and preferably aluminum oxide.
7. The method for preparing a fluorescent material for optical temperature sensing according to claim 4, wherein: the raw material containing europium element is at least one of europium oxide, europium chloride, europium sulfate, europium nitrate, europium oxalate and europium phosphate, and preferably europium oxide.
8. The method for preparing a fluorescent material for optical temperature sensing according to claim 4, wherein: the calcination temperature is 1350-1550 ℃, and the heat preservation sintering time is 2-18 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115612488A (en) * | 2022-10-17 | 2023-01-17 | 上海交通大学 | High-temperature application off-line temperature measurement fluorescent powder for aircraft engine and the like, and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112745836A (en) * | 2021-03-04 | 2021-05-04 | 沈阳大学 | Eu (Eu)2+、Eu3+Ion co-activated optical temperature sensing material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112745836A (en) * | 2021-03-04 | 2021-05-04 | 沈阳大学 | Eu (Eu)2+、Eu3+Ion co-activated optical temperature sensing material and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| 伏振兴; 刘碧蕊: "SrAl2O4∶Eu荧光粉中Eu的价态分析与发光特性研究", 宁夏师范学院学报 * |
| 王梓垚;: "Eu2+/Eu3+共掺SrAl2O4直接白光荧光粉的发光性能研究", 第三届中国国际复合材料科技大会摘要集-分会场51-56 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115612488A (en) * | 2022-10-17 | 2023-01-17 | 上海交通大学 | High-temperature application off-line temperature measurement fluorescent powder for aircraft engine and the like, and preparation method and application thereof |
| CN115612488B (en) * | 2022-10-17 | 2024-04-12 | 上海交通大学 | Offline temperature measurement fluorescent powder for high-temperature application of aero-engine and preparation method and application thereof |
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