CN117191213A - Trivalent Pr ion doped molybdate optical temperature measurement material and preparation method thereof - Google Patents
Trivalent Pr ion doped molybdate optical temperature measurement material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 70
- 230000003287 optical effect Effects 0.000 title claims abstract description 65
- 238000009529 body temperature measurement Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 150000002500 ions Chemical class 0.000 title abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 52
- 238000000227 grinding Methods 0.000 claims abstract description 26
- 239000002243 precursor Substances 0.000 claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 20
- 239000000126 substance Substances 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 17
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 11
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 150000001875 compounds Chemical class 0.000 claims description 45
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 15
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 claims description 13
- 229910003447 praseodymium oxide Inorganic materials 0.000 claims description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 12
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 12
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 12
- 238000011068 loading method Methods 0.000 claims description 12
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 12
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 12
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 10
- 229910052712 strontium Inorganic materials 0.000 claims description 10
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 10
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 9
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 8
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 7
- 239000011575 calcium Substances 0.000 claims description 7
- 229910052791 calcium Inorganic materials 0.000 claims description 7
- 229910001938 gadolinium oxide Inorganic materials 0.000 claims description 7
- 229940075613 gadolinium oxide Drugs 0.000 claims description 7
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 7
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 6
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 6
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 239000011733 molybdenum Substances 0.000 claims description 6
- -1 rare earth ion Chemical class 0.000 claims description 6
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 4
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 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
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 4
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910017569 La2(CO3)3 Inorganic materials 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- QXDMQSPYEZFLGF-UHFFFAOYSA-L calcium oxalate Chemical compound [Ca+2].[O-]C(=O)C([O-])=O QXDMQSPYEZFLGF-UHFFFAOYSA-L 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 claims description 2
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 claims description 2
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 claims description 2
- 229960001633 lanthanum carbonate Drugs 0.000 claims description 2
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 2
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 2
- WFLYOQCSIHENTM-UHFFFAOYSA-N molybdenum(4+) tetranitrate Chemical compound [N+](=O)([O-])[O-].[Mo+4].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] WFLYOQCSIHENTM-UHFFFAOYSA-N 0.000 claims description 2
- CZDSWLXAULJYPZ-UHFFFAOYSA-J molybdenum(4+);dicarbonate Chemical compound [Mo+4].[O-]C([O-])=O.[O-]C([O-])=O CZDSWLXAULJYPZ-UHFFFAOYSA-J 0.000 claims description 2
- YWECOPREQNXXBZ-UHFFFAOYSA-N praseodymium(3+);trinitrate Chemical compound [Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YWECOPREQNXXBZ-UHFFFAOYSA-N 0.000 claims description 2
- QVOIJBIQBYRBCF-UHFFFAOYSA-H yttrium(3+);tricarbonate Chemical compound [Y+3].[Y+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O QVOIJBIQBYRBCF-UHFFFAOYSA-H 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 14
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 21
- 238000010438 heat treatment Methods 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 17
- 238000001816 cooling Methods 0.000 description 12
- 230000005284 excitation Effects 0.000 description 12
- 238000000634 powder X-ray diffraction Methods 0.000 description 12
- 229910052593 corundum Inorganic materials 0.000 description 10
- 239000010431 corundum Substances 0.000 description 10
- 239000011159 matrix material Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 238000000295 emission spectrum Methods 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 238000004861 thermometry Methods 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- 229910052693 Europium Inorganic materials 0.000 description 4
- 230000008878 coupling Effects 0.000 description 4
- 238000010168 coupling process Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- 238000002189 fluorescence spectrum Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000011540 sensing material Substances 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000001506 fluorescence spectroscopy Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
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- 230000007704 transition Effects 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
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- 239000011858 nanopowder Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Luminescent Compositions (AREA)
Abstract
The invention discloses a trivalent Pr ion doped molybdate optical temperature measurement material and a preparation method thereof. The optical temperature measuring material provided by the invention has high relative sensitivity, is a red luminescent material, has a scheelite structure, and has a chemical general formula of LiCa a Sr 1‑a M 1‑x (MoO 4 ) 3 :xPr 3+ Wherein a is more than or equal to 0 and less than or equal to 1, and 1at%<x<15at%, M is Y, gd or La. The preparation method comprises weighing raw materials according to the chemical formula, adding absolute ethanol into agate mortar, grinding to obtain reaction precursor; placing the precursor in an alumina crucible, and presintering in an air atmosphere; and then grinding and mixing again, and calcining under the air atmosphere to obtain the material. The invention adopts the high-temperature solid phase method to prepare the sampleThe particle size is fine, no agglomeration exists, the preparation process is simple and safe, the cost of raw materials is low, and the industrial production is easy to realize.
Description
Technical Field
The invention relates to an optical temperature-measuring luminescent material and a preparation method thereof; in particular to Pr 3+ Doped molybdate optical temperature measuring materialThe preparation method belongs to the technical field of optical temperature measurement.
Background
As is well known, temperature is a very important physical parameter, and accurate measurement of temperature plays a vital role in numerous fields such as industrial production, scientific research, biomedical and the like. According to the statistics of Grand View Research, the temperature sensor for measuring the temperature accounts for about 80% of the global sensor market. The most widely used traditional temperature measuring means are thermocouples and thermal resistance temperature measurement. The traditional temperature sensors are low in cost, stable and reliable, but are all used for measuring temperature in a contact mode, and the traditional temperature sensors are required to be fully contacted with an object to be measured, and then the final temperature value can be given after the thermal balance is achieved. There are problems in that the response time is long, the accuracy is low, and only contact measurement can be performed.
Rare earth elements have the characteristics of special electronic structure, rich energy level and the like, and are the luminous centers of a plurality of optical materials. Furthermore, it has been found that certain optical properties of rare earth ions change with ambient temperature, so rare earth doped luminescent materials can also be used for temperature measurement. The non-contact optical temperature measurement technology based on the rare earth doped luminescent material has the advantages of non-contact, quick response, high sensitivity and the like, and can be used for temperature measurement in extreme occasions, such as strong electric fields and/or strong corrosive environments, and is also suitable for temperature measurement in small-scale systems, such as measurement in micro electronic elements and microbial cells. Among the optical temperature measurement techniques, the fluorescence intensity ratio temperature measurement technique is considered as the most potential optical temperature measurement technique, which uses the relationship between the fluorescence intensity ratio between two thermally coupled energy levels of rare earth ions and the temperature change for temperature measurement. The sensitivity of the optical temperature measuring type thermometer is one of the most important performance indexes, and the relative sensitivity of the thermal coupling energy level type temperature sensing material is determined by the energy level of the thermal coupling energy level, so that the exploration of the optical temperature measuring material with larger thermal coupling energy level spacing has important significance for improving the performance of the optical temperature measuring type thermometer.
The energy interval between the thermal coupling energy levels is generally 200-2000cm -1 At present, the technologyMature Er 3+ The relative sensitivity of the doped fluorescent temperature sensing material is always wander at 1% K -1 Up and down, this severely restricts the application of the optical thermometric thermometer. Pr (Pr) 3+ A kind of electronic device 3 P 0 And (3) with 1 D 2 Is a pair of non-thermally coupled energy levels with a relatively large energy level (about 3900 cm) -1 ) And the thermal quenching tendencies of the different energy levels have significant differences. Meanwhile, the energy level emitted light belongs to the visible light wave band, is easy to distinguish and measure, and can pass Pr 3+ Of ions 1 D 2 Emission peak intensity and transition 3 P 0 And comparing the intensity of the transmitted peak of the transition, and obtaining two groups of FIR values. The two groups of FIR values can represent the temperature change, and the two groups of results can mutually verify, so that the accuracy of temperature measurement can be effectively improved, and self calibration can be realized. Pr therefore 3+ The luminescent center as an optical temperature sensing material has its unique advantages.
In addition to selecting a suitable luminescent center, the properties of the host material also affect the optical properties of the temperature sensing material, so that a suitable material should be selected as a luminescent host before the optical material is prepared. The more common matrix materials include oxide matrix, fluoride matrix, tungstate matrix, molybdate matrix, etc. Pr reported at present 3+ The relative sensitivity of doped optical thermometry materials has yet to be improved, e.g. (Na, li, K) Pr (PO) 3 ) 4 The relative sensitivity of (C) is 0.60%/K -1 (J.Lumin.,2018,201:372-383)，BaNb 2 O 6 :Pr 3+ The relative sensitivity of (C) is 0.61%/K -1 (J.Alloy Compd.,2020,821:153342-1-12),La 2 MgTiO 6 :Pr 3+ The relative sensitivity of (C) is 1.28%/K -1 (J. Mater. Chem. C,2017,5 (41): 10737-10745). Therefore, the selection of a proper luminous matrix for preparing an optical temperature measuring material with high relative sensitivity and high temperature repetition rate has important significance.
Disclosure of Invention
The purpose of the invention is that: aiming at the defects of the prior art, a Pr is provided 3+ Novel doped molybdateAn optical temperature measuring material and a preparation method thereof.
In order to achieve the above object, the present invention provides Pr 3+ The doped molybdate optical temperature measuring material is a red luminescent material, and the chemical composition formula is as follows: liCa a Sr 1-a M 1-x (MoO 4 ) 3 :xPr 3+ Wherein a is more than or equal to 0 and less than or equal to 1, and 1at%<x<15at%, M is at least one of Y, gd and La; the luminous center is rare earth ion Pr 3+ 。
The invention also provides Pr of the above 3+ The preparation method of the doped molybdate optical temperature measurement material comprises the steps of taking a lithium-containing compound, a calcium-containing compound, a strontium-containing compound, an yttrium-containing compound, a gadolinium-containing compound, a lanthanum-containing compound and a molybdenum-containing compound as raw materials, and preparing Pr by adopting a high-temperature solid-phase method 3+ Doped molybdate optical temperature measuring luminescent material.
Preferably, said Pr 3+ The preparation method of the doped molybdate optical temperature measurement material comprises the following steps:
step 1: liCa according to chemical composition a Sr 1-a M 1-x (MoO 4 ) 3 :xPr 3+ Wherein a is more than or equal to 0 and less than or equal to 1, and 1at%<x<15at%, M is at least one of Y, gd and La, and is selected from lithium-containing compound raw materials, calcium-containing compound raw materials, strontium-containing compound raw materials, gadolinium-containing compound raw materials, yttrium-containing compound raw materials, lanthanum-containing compound raw materials, praseodymium-containing compound raw materials and molybdenum-containing compound raw materials respectively; accurately weighing raw materials according to the stoichiometric ratio of each substance in the chemical composition formula, and grinding in an agate mortar to uniformly mix the raw materials to obtain a precursor;
step 2: and (3) placing the precursor into an alumina crucible, capping, placing into a muffle furnace, presintering in an air atmosphere, and naturally cooling to room temperature after presintering.
Step 3: taking out the sample obtained after pre-sintering, grinding the sample in an agate mortar, mixing, loading the mixture into an alumina crucible again, covering, placing the alumina crucible into a muffle furnace, calcining in air atmosphere, naturally cooling to room temperature, and taking the sampleGrinding the mixture into powder in an agate crucible after the mixture is discharged to obtain Pr 3+ Doped molybdate optical temperature measurement material.
Preferably, in the step 1, the lithium-containing compound raw material is at least one of lithium oxide, lithium nitrate, lithium carbonate, lithium hydroxide and lithium oxalate; the raw materials of the calcium-containing compound are at least one of calcium oxide, calcium nitrate, calcium carbonate, calcium hydroxide and calcium oxalate; the strontium-containing compound raw material is at least one of strontium oxide, strontium nitrate and strontium carbonate; the yttrium-containing compound raw material is at least one of yttrium oxide, yttrium nitrate and yttrium carbonate; the gadolinium-containing compound raw material is at least one of gadolinium oxide and gadolinium nitrate; the lanthanum-containing compound raw material is at least one of lanthanum oxide, lanthanum nitrate and lanthanum carbonate; the molybdenum-containing compound raw material is at least one of molybdenum oxide, molybdenum nitrate and molybdenum carbonate; the praseodymium-containing compound raw material is at least one of praseodymium oxide and praseodymium nitrate.
More preferably, the yttrium-containing compound raw material is yttrium oxide, the gadolinium-containing compound raw material is gadolinium oxide, the lanthanum-containing compound raw material is lanthanum oxide, the praseodymium-containing compound raw material is praseodymium oxide, and the molybdenum-containing compound raw material is molybdenum trioxide.
Preferably, the precursor in the step 1 is prepared to have an amount of calcium element and strontium element which is 1% -8% in excess of the molar amount required for the chemical composition formula.
Preferably, the temperature of the pre-sintering in the step 2 is 600-650 ℃, the heat preservation time is 3-4 hours, and the pre-sintering is cooled to room temperature along with the furnace.
Preferably, the calcining temperature in the step 3 is 800-950 ℃, the heat preservation time is 8-10 hours, and the mixture is cooled to room temperature along with the furnace.
The invention also provides Pr of the above 3+ The doped molybdate optical temperature measuring material is applied to the preparation of a temperature sensor and the temperature measurement.
The invention selects alkali metal rare earth dimolybdate with scheelite (body-centered tetragonal phase) structure as the luminescent matrix, which has excellent physical and chemical properties and good high temperature stability, in the luminescent matrix, trivalent Pr system ion doping is carried out, rare earth ion Pr 3+ The inventive LiCa exhibits high excitation and emission efficiency in the scheelite structured molybdate matrix a Sr 1-a M 1-x (MoO 4 ) 3 :xPr 3+ The optical temperature measuring material emits red light of about 650nm under the excitation of 250-350 nm ultraviolet and 440-510nm blue light, and the relative temperature sensitivity is greater than 1%/K -1 Wherein LiSrY (MoO) 4 ) 3 ：8％Pr 3+ The relative sensitivity of (2) is 2.75%/K -1 . Therefore, the LiCa provided by the invention a Sr 1-a M 1-x (MoO 4 ) 3 :xPr 3+ The optical temperature measuring material has the excellent performances of wide excitation area, high relative sensitivity, good temperature resolution, good repeatability and the like; in addition, the LiCa provided by the invention a Sr 1-a M 1-x (MoO 4 ) 3 :xPr 3+ The optical temperature measuring material has the advantages of low cost of raw materials, simple and feasible preparation process, low requirement on equipment and the like.
Compared with the prior art, the invention has the following beneficial effects:
(1) Pr of the invention 3+ The molybdate optical temperature measuring material is doped, so that the selectivity of the optical temperature measuring material to a substrate is greatly expanded, and the development space of the optical temperature measuring material is increased; pr (Pr) 3+ The molybdate-doped optical temperature measurement material is prepared by adopting a high-temperature solid phase method, has the advantages of simple and feasible preparation operation, low equipment requirement, easy control of reaction conditions and the like, and is easy for industrial production.
(2) The emission range of the optical temperature measurement luminescent material is in the red visible light range, can be effectively excited by ultraviolet and blue light absorption areas, and has stable property in air and is not easy to deliquesce.
(3) The optical temperature-measuring luminescent material has the advantages of high temperature sensitivity of luminescent characteristics, rapid fluorescence decay and rapid light response.
Drawings
FIG. 1 is an x-ray diffraction pattern of the optical thermometry luminescent materials of examples 1-5.
FIG. 2 is an excitation pattern of the optical thermometry luminescent materials of examples 1 to 5.
FIG. 3 is an emission spectrum of the optical thermometry luminescent material of examples 1-5.
FIG. 4 is a spectrum of life of the optical thermometry luminescent material of examples 1 to 5.
FIG. 5 is a graph showing the relative sensitivity of the optical thermometry luminescent materials of examples 1-5 with temperature.
Fig. 6 is a comparison of emission spectra of the optical thermometry luminescent materials of comparative example 1 and example 1.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Example 1:
pr (Pr) 3+ The doped molybdate optical temperature measurement luminescent material is in powder, and has the following molecular formula: liCaY (MoO) 4 ) 3 ：12％Pr 3+ . The preparation method comprises the following steps: according to the molecular formula metering ratio, lithium carbonate, calcium carbonate, yttrium oxide, molybdenum oxide and praseodymium oxide with the purity of over 99.9 percent are taken as raw materials, and the specific mass of the lithium carbonate, the calcium carbonate, the yttrium oxide, the molybdenum oxide and the praseodymium oxide are 0.1188g, 0.3229g, 0.3351g, 1.3885g and 0.0657g respectively. Adding 1% -8% of calcium with molar excess on the basis of the calculated proportion of the original chemical formula, grinding and uniformly mixing the precursor by an agate mortar to obtain a precursor, adding a proper amount of absolute ethyl alcohol into the agate mortar for grinding uniformly, loading the precursor into a corundum crucible, heating to 600 ℃ at a heating rate of 120 ℃/h in an air atmosphere, preserving heat and calcining for 3 hours, cooling to room temperature along with a furnace, placing a sample into the agate mortar, grinding uniformly by the absolute ethyl alcohol, loading the sample into the corundum crucible, heating to 800 ℃ at a heating rate of 120 ℃/h in the air atmosphere, preserving heat and calcining for 8 hours, cooling to room temperature along with the furnace, and crushing and grinding the obtained calcined product to obtain Pr 3+ Doped LiCoY (MoO) 4 ) 3 ：12％Pr 3+ Optical temperature measuring luminescent material. The X-ray powder diffraction (XRD) results showed that the obtained phosphor was in a pure phase (as shown in fig. 1). Fluorescence spectroscopy test results showed that the optimal excitation was 451nm (as shown in FIG. 2) and the optimal emission was 653nm (as shown in FIG. 3). Fluorescent life test knotAs a result, the fluorescence lifetime of the sample was 116.5ns (as shown in FIG. 4), which is the sample with the shortest lifetime in the example. Testing relative sensitivity, taking 25K as a recording point, measuring emission spectra of eight temperatures from 298K-473K, recording intensities of 653nm and 607nm emission peaks of each temperature point respectively, fitting in Origin at 653nm/607nm ratio point, calculating relative sensitivity of the sample at 473K to 2.04%/K by fitting formula -1 (as shown in fig. 5).
Example 2:
pr (Pr) 3+ The doped molybdate optical temperature measurement luminescent material is in powder, and has the following molecular formula: liCaGd (MoO) 4 ) 3 ：11％Pr 3+ . The preparation method comprises the following steps: according to the molecular formula metering ratio, lithium carbonate, calcium carbonate, gadolinium oxide, molybdenum oxide and praseodymium oxide with the purity of over 99.9 percent are taken as raw materials, and the specific mass of the lithium carbonate, the calcium carbonate, the gadolinium oxide, the molybdenum oxide and the praseodymium oxide are respectively 0.1083g, 0.2934g, 0.4729g, 1.2658g and 0.0549g. Adding 1% -8% of calcium with molar excess on the basis of the calculated proportion of the original chemical formula, grinding and uniformly mixing the precursor by an agate mortar to obtain a precursor, adding a proper amount of absolute ethyl alcohol into the agate mortar for grinding uniformly, loading the precursor into a corundum crucible, heating to 600 ℃ at a heating rate of 120 ℃/h in an air atmosphere, preserving heat and calcining for 3 hours, cooling to room temperature along with a furnace, placing a sample into the agate mortar, grinding uniformly by the absolute ethyl alcohol, loading the sample into the corundum crucible, heating to 800 ℃ at a heating rate of 120 ℃/h in the air atmosphere, preserving heat and calcining for 8 hours, cooling to room temperature along with the furnace, and crushing and grinding the obtained calcined product to obtain Pr 3+ Doped LiCaGd (MoO) 4 ) 3 ：11％Pr 3+ Optical temperature measuring luminescent material. The X-ray powder diffraction (XRD) results showed that the obtained phosphor was in a pure phase (as shown in fig. 1). Fluorescence spectroscopy test results showed that the optimal excitation was 451nm (as shown in FIG. 2) and the optimal emission was 653nm (as shown in FIG. 3). The fluorescence lifetime test results showed that the fluorescence lifetime of this sample was 148.3ns (as shown in fig. 4). Testing of relative sensitivity, measuring eight temperatures from 298K-473K with 25K as a recording pointThe intensity of the emission peak of each temperature point 651nm and 605nm is recorded respectively, the points with the ratio of 651nm/605nm are fitted in Origin, and the relative sensitivity of the sample at 473K can reach 1.57%/K by calculating the fitting formula -1 (as shown in fig. 5).
Example 3:
pr (Pr) 3+ The doped molybdate optical temperature measurement luminescent material is in powder, and has the following molecular formula: liSrY (MoO) 4 ) 3 ：8％Pr 3+ . The preparation method comprises the following steps: according to the molecular formula metering ratio, lithium carbonate, strontium carbonate, yttrium oxide, molybdenum oxide and praseodymium oxide with the purity of over 99.9 percent are taken as raw materials, and the specific mass of the lithium carbonate, strontium carbonate, yttrium oxide, molybdenum oxide and praseodymium oxide is respectively 0.1107g, 0.4424g, 0.3113g, 1.2939g and 0.0408g. Adding 1% -8% of strontium with molar excess on the basis of the original chemical formula calculation proportion, grinding and uniformly mixing the precursor by an agate mortar to obtain a precursor, adding a proper amount of absolute ethyl alcohol into the agate mortar for grinding uniformly, loading the precursor into a corundum crucible, heating to 650 ℃ at a heating rate of 120 ℃/h in an air atmosphere, preserving heat and calcining for 4 hours, cooling to room temperature along with a furnace, placing a sample into the agate mortar, grinding uniformly with absolute ethyl alcohol, loading the sample into the corundum crucible, heating to 900 ℃ at a heating rate of 120 ℃/h in the air atmosphere, preserving heat and calcining for 10 hours, cooling to room temperature along with the furnace, crushing and grinding the obtained calcined product to obtain Pr 3+ Doped LiSrY (MoO) 4 ) 3 ：8％Pr 3+ Optical temperature measuring luminescent material. The X-ray powder diffraction (XRD) results showed that the obtained phosphor was in a pure phase (as shown in fig. 1). The fluorescence spectrum test results show that the optimal excitation is 451nm (shown in figure 2) and the optimal emission is 651nm (shown in figure 3). The fluorescence lifetime test results show that the fluorescence lifetime of the sample is 318.1ns (as shown in fig. 4). Testing relative sensitivity, taking 25K as a recording point, measuring emission spectra of eight temperatures from 298K-473K, recording intensities of 651nm and 605nm emission peaks of each temperature point respectively, fitting in Origin at 651nm/605nm ratio point, calculating the sample at 473K by fitting formulaThe relative sensitivity of the product can reach 2.75 percent/K -1 (as shown in FIG. 5), which is the sample with the highest relative sensitivity in the examples.
Example 4:
pr (Pr) 3+ The doped molybdate optical temperature measurement luminescent material is in powder, and has the following molecular formula: liSrGd (MoO) 4)3 ：10％Pr 3+ . The preparation method comprises the following steps: according to the molecular formula metering ratio, lithium carbonate, strontium carbonate, gadolinium oxide, molybdenum oxide and praseodymium oxide with the purity of over 99.9 percent are taken as raw materials, and the specific mass of the lithium carbonate, strontium carbonate, gadolinium oxide, molybdenum oxide and praseodymium oxide is 0.1012g, 0.4045g, 0.4469g, 1.1831g and 0.0466g respectively. Adding 1% -8% of strontium with molar excess on the basis of the original chemical formula calculation proportion, grinding and uniformly mixing the precursor by an agate mortar to obtain a precursor, adding a proper amount of absolute ethyl alcohol into the agate mortar for grinding uniformly, loading the precursor into a corundum crucible, heating to 650 ℃ at a heating rate of 120 ℃/h in an air atmosphere, preserving heat and calcining for 4 hours, cooling to room temperature along with a furnace, placing a sample into the agate mortar, grinding uniformly with absolute ethyl alcohol, loading the sample into the corundum crucible, heating to 900 ℃ at a heating rate of 120 ℃/h in the air atmosphere, preserving heat and calcining for 10 hours, cooling to room temperature along with the furnace, crushing and grinding the obtained calcined product to obtain Pr 3+ Doped LiSrGd (MoO) 4 ) 3 ：10％Pr 3+ Optical temperature measuring luminescent material. The X-ray powder diffraction (XRD) results showed that the obtained phosphor was in a pure phase (as shown in fig. 1). Fluorescence spectrum test results showed that the optimal excitation was 451nm (as shown in FIG. 2) and the optimal emission was 650nm (as shown in FIG. 3). The fluorescence lifetime test results show that the fluorescence lifetime of the sample is 344.6ns (as shown in fig. 4). Testing relative sensitivity, taking 25K as a recording point, measuring emission spectra of eight temperatures from 298K-473K, recording the intensities of 650nm and 605nm emission peaks of each temperature point, fitting in Origin at 650nm/605nm ratio point, calculating relative sensitivity of the sample at 473K to 1.44%/K by fitting formula -1 (as shown in fig. 5).
Example 5:
pr (Pr) 3+ The doped molybdate optical temperature measurement luminescent material is in powder, and has the following molecular formula: liSrLa (MoO) 4 ) 3 ：8％Pr 3+ . The preparation method comprises the following steps: according to the molecular formula metering ratio, lithium carbonate, strontium carbonate, lanthanum oxide, molybdenum oxide and praseodymium oxide with the purity of over 99.9 percent are taken as raw materials, and the specific mass of the lithium carbonate, strontium carbonate, lanthanum oxide, molybdenum oxide and praseodymium oxide is respectively 0.1036g, 0.4139g, 0.4201g, 1.2105g and 0.0382g. Adding 1% -8% of strontium with molar excess on the basis of the original chemical formula calculation proportion, grinding and uniformly mixing the precursor by an agate mortar to obtain a precursor, adding a proper amount of absolute ethyl alcohol into the agate mortar for grinding uniformly, loading the precursor into a corundum crucible, heating to 650 ℃ at a heating rate of 120 ℃/h in an air atmosphere, preserving heat and calcining for 4 hours, cooling to room temperature along with a furnace, placing a sample into the agate mortar, grinding uniformly with absolute ethyl alcohol, loading the sample into the corundum crucible, heating to 950 ℃ at a heating rate of 120 ℃/h in the air atmosphere, preserving heat and calcining for 10 hours, cooling to room temperature along with the furnace, crushing and grinding the obtained calcined product to obtain Pr 3+ Doped LiSrLa (MoO) 4 ) 3 ：8％Pr 3 + Optical temperature measuring luminescent material. The X-ray powder diffraction (XRD) results showed that the obtained phosphor was in a pure phase (as shown in fig. 1). Fluorescence spectroscopy test results showed that the best excitation was 451nm (as shown in FIG. 2) and the best emission was 649nm (as shown in FIG. 3), which is the best sample for excitation emission in the examples. The fluorescence lifetime test results show that the fluorescence lifetime of the sample is 683.9ns (as shown in fig. 4). Testing relative sensitivity, taking 25K as a recording point, measuring emission spectra of eight temperatures from 298K-473K, recording the intensities of 649nm and 604nm emission peaks of each temperature point, fitting in Origin at 649nm/604nm ratio point, calculating relative sensitivity of the sample at 473K to 1.5%/K by fitting formula -1 (as shown in fig. 5).
Comparative example 1:
pr (Pr) 3+ The doped molybdate optical temperature measurement luminescent material is in powder, and has the following molecular formula: liCaY (MoO) 4 ) 3 ：1％Pr 3+ . The preparation is described in example 1. The X-ray powder diffraction (XRD) results indicate that the obtained phosphor is a pure phase. The fluorescence spectrum test results showed that the emission peak was consistent with example 1, but the 653 emission peak intensity was only 30% of that of example 1 (see fig. 6). Test of relative sensitivity the emission spectra of eight temperatures were measured from 298K-473K at 25K as a recording point and fit calculated in Origin at the 653nm/607nm ratio point, the comparative example being lower in relative sensitivity than the example since the sample 607nm emission intensity was higher than the example 607nm emission intensity and the 653nm emission intensity was much lower than the example 653nm emission intensity.
Comparative example 2:
high-temperature solid phase method for preparing LaMg 0.402 Nb 0.598 O 3 ：1.2％Pr 3+ Compounds, see (H.Zhang, Z.Gao, G.Li, Y.Zhu, Y.Liang, A ratiometric optical thermometer with multi-color emission and high sensitivity based on double perovskite LaMg) 0.402 Nb 0.598 O 3 :Pr 3+ thermochromic phosphors, chem. Eng. J.2020,380: 122491-1-11.). The raw material is oxide or carbonate with purity of more than 99.9 percent and containing preparation material elements, and 2 percent boric acid is cosolvent. The stoichiometric materials were thoroughly mixed and dried, and the powder precursor was pre-burned in an air atmosphere at 950 ℃ for 8 hours. After milling, the preheated powder was sintered in a horizontal tube furnace at 1300 ℃ for 4 hours under an air atmosphere. The solid phase synthesis method is adopted in the examples and the preparation method of the comparative example, so that the sample preparation has low requirements on sintering equipment and is easy for mass production. The fluorescence spectrum test results show that the optimal excitation is 450nm, the optimal emission is 655nm, and the range is consistent with the embodiment range. The results show that the comparative example has a relative sensitivity of 0.725%/K at 448K -1 Only 35.5% of the sample of example 1 and only 26% of the sample of example 3. Because the test conditions are limited, the upper test limit temperature 473K is not the temperature corresponding to the maximum relative sensitivity of the embodiments of the present invention. The temperature cycle test result shows that the temperature repetition rate of the comparative example sample is 95%, the temperature repetition rate of the example 3 sample is 98% -99%, the temperature repetition rate of the example sample is better,the circulation stability is better.
Comparative example 3:
preparation of TiO by hydrolytic Sol-gel 2 ：3％Eu 3+ Luminescent materials, see (M.G.Nikolic, Z.Antic, S.Culubrk, J.M.Nedeljkovic, M.D.Dramicanin, temperature sensing with Eu) 3+ doped TiO 2 nanocycles, sens.actuators, B2014, 201:46-50.). Will be doped with 3at% Eu 3+ TiO of (C) 2 Mixing the nano powder, titanium (IV) isopropoxide, water and ethanol, and adding a proper amount of Eu 2 O 3 Dissolved in dilute HNO 3 And added to the mixture. A transparent gel was obtained in a few minutes and after drying the sample was heated at a rate of 5 ℃ for a min to a final temperature of 210 ℃ and held at that temperature for 20 minutes. Finally, calcining the sample at 420 ℃ for 2 hours to obtain TiO 2 ：3％Eu 3+ Luminescent materials. The comparative example is prepared by adopting a sol-gel method, has complex preparation process and harsh reaction conditions, and is not beneficial to large-scale industrial production. The comparative sample had an optimal excitation at 365nm and emission peaks at 438nm and 613nm. The results show that the relative sensitivity of the comparative sample at 473K is 1.8%/K -1 Only 65% of the relative sensitivity value of example 3at the same temperature corresponds to a temperature that is not the maximum relative sensitivity of example 3, as in the case of the comparative example described above, 473K. The temperature resolution results show that the comparative example has a temperature resolution of 0.46K at 473K, which is much higher than the temperature resolution of 0.16K-0.24K@473K for the sample of example 3. The comparison result shows that the sample provided by the invention has better relative sensitivity and temperature resolution.
As can be seen from the combination of the present examples and comparative example 1, in comparative example 1, if the relative sensitivity is calculated by fitting the 653nm/607nm ratio point in Origin according to example 1, the calculated sensitivity is lower, so that the relative sensitivity can be calculated by fitting different emission peak intensities for materials with different doping ratios; as can be seen from the combination of the embodiment of the present invention and the comparative example 2, when the selected luminescent substrates are different, the sensitivity and stability of the temperature measuring material are greatly affected, and the sensitivity and stability (repeatability) of the temperature measuring material are reduced, as wellThe sample can not meet the actual application requirements; as can be seen from a combination of the present invention example and the above comparative example 3, pr of the present invention 3+ Doped molybdate optical temperature measurement material is compared with TiO reported in literature 2 ：3％Eu 3+ The luminescent material has more excellent performance.
While the invention has been described with respect to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. Pr (Pr) 3+ The doped molybdate optical temperature measuring material is characterized in that the optical temperature measuring material is red luminescent material, and the chemical composition formula of the material is LiCa a Sr 1-a M 1-x (MoO 4 ) 3 :xPr 3+ Wherein a is more than or equal to 0 and less than or equal to 1, and 1at%<x<15at%, M is at least one of Y, gd and La; the luminous center is rare earth ion Pr 3+ 。
2. Pr of claim 1 3+ The doped molybdate optical temperature measurement material and the preparation method thereof are characterized by comprising the following steps:
step 1: liCa according to chemical composition a Sr 1-a M 1-x (MoO 4 ) 3 :xPr 3+ Wherein a is more than or equal to 0 and less than or equal to 1, and 1at%<x<15at%, M is at least one of Y, gd and La; respectively selecting a lithium-containing compound raw material, a calcium-containing compound raw material, a strontium-containing compound raw material, a gadolinium-containing compound raw material, an yttrium-containing compound raw material, a lanthanum-containing compound raw material, a praseodymium-containing compound raw material and a molybdenum-containing compound raw material; accurately weighing raw materials according to the stoichiometric ratio of each substance in the chemical composition formula, and grinding in an agate mortar to uniformly mix the raw materials to obtain a precursor;
step 2: loading the uniformly grinded precursor into an alumina crucible, covering the alumina crucible, placing the alumina crucible in a muffle furnace, and presintering the alumina crucible in air;
step 3: taking out the sample obtained by pre-sintering in the step 2, putting the sample into an agate mortar for grinding and mixing uniformly, putting the sample into an alumina crucible again, and calcining the sample in an air atmosphere to obtain Pr 3+ Doped optical thermometric materials.
3. Pr as claimed in claim 2 3+ The preparation method of the doped molybdate optical temperature measurement material is characterized in that in the step 1, the lithium-containing compound raw material is at least one of lithium oxide, lithium nitrate, lithium carbonate, lithium hydroxide and lithium oxalate; the raw materials of the calcium-containing compound are at least one of calcium oxide, calcium nitrate, calcium carbonate, calcium hydroxide and calcium oxalate; the strontium-containing compound raw material is at least one of strontium oxide, strontium nitrate and strontium carbonate; the yttrium-containing compound raw material is at least one of yttrium oxide, yttrium nitrate and yttrium carbonate; the gadolinium-containing compound raw material is at least one of gadolinium oxide and gadolinium nitrate; the lanthanum-containing compound raw material is at least one of lanthanum oxide, lanthanum nitrate and lanthanum carbonate; the molybdenum-containing compound raw material is at least one of molybdenum oxide, molybdenum nitrate and molybdenum carbonate; the praseodymium-containing compound raw material is at least one of praseodymium oxide and praseodymium nitrate.
4. Pr as claimed in claim 2 3+ The preparation method of the doped molybdate optical temperature measurement material is characterized in that in the step 1, the amounts of calcium element and strontium element in the raw materials are respectively required to be in excess of 1-8% compared with the molar amounts of chemical composition formulas.
5. Pr as claimed in claim 2 3+ The preparation method of the doped molybdate optical temperature measurement material is characterized in that in the step 2, the presintering temperature is 600-650 ℃, and the presintering time is 3-4 hours.
6. Pr as claimed in claim 2 3+ The preparation method of the doped molybdate optical temperature measurement material is characterized in that in the step 3, the calcining temperature is 800-950 ℃ and the calcining time is 8-10 hours.
7. Pr of claim 1 3+ The doped molybdate optical temperature measuring material is applied to the preparation of a temperature sensor and the temperature measurement.
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