CN116891742B - Rare earth luminescent material and preparation method and application thereof - Google Patents
Rare earth luminescent material and preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 50
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 46
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 37
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 37
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 37
- 239000000126 substance Substances 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 110
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 108
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 54
- 229910052786 argon Inorganic materials 0.000 claims description 54
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- 239000000725 suspension Substances 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 14
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 10
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 9
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 9
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 9
- LOXWVAXWPZWIOO-UHFFFAOYSA-N 7-bromo-1-chloronaphthalene Chemical compound C1=C(Br)C=C2C(Cl)=CC=CC2=C1 LOXWVAXWPZWIOO-UHFFFAOYSA-N 0.000 claims description 9
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 9
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000005642 Oleic acid Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 9
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 9
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 9
- LEYFXTUKPKKWMP-UHFFFAOYSA-K trichloroytterbium;hexahydrate Chemical compound O.O.O.O.O.O.Cl[Yb](Cl)Cl LEYFXTUKPKKWMP-UHFFFAOYSA-K 0.000 claims description 9
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 8
- IINACGXCEZNYTF-UHFFFAOYSA-K trichloroyttrium;hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Y+3] IINACGXCEZNYTF-UHFFFAOYSA-K 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229960003638 dopamine Drugs 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- PNYPSKHTTCTAMD-UHFFFAOYSA-K trichlorogadolinium;hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Gd+3] PNYPSKHTTCTAMD-UHFFFAOYSA-K 0.000 claims description 4
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000000084 colloidal system Substances 0.000 claims description 3
- 238000000593 microemulsion method Methods 0.000 claims description 3
- 238000012634 optical imaging Methods 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- 239000007853 buffer solution Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000011540 sensing material Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 7
- 238000005259 measurement Methods 0.000 abstract description 7
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 3
- 230000005284 excitation Effects 0.000 abstract description 3
- 238000004020 luminiscence type Methods 0.000 abstract description 3
- 238000013170 computed tomography imaging Methods 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract description 2
- 238000012546 transfer Methods 0.000 abstract description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000013307 optical fiber Substances 0.000 description 5
- 238000002329 infrared spectrum Methods 0.000 description 4
- 238000004891 communication Methods 0.000 description 3
- 238000003384 imaging method Methods 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000009529 body temperature measurement Methods 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- -1 rare earth ions Chemical class 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- NWZBFJYXRGSRGD-UHFFFAOYSA-M sodium;octadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOS([O-])(=O)=O NWZBFJYXRGSRGD-UHFFFAOYSA-M 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- 238000012800 visualization Methods 0.000 description 1
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7772—Halogenides
- C09K11/7773—Halogenides with alkali or alkaline earth metal
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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Abstract
The invention relates to a rare earth luminescent material, in particular to a rare earth luminescent material, a preparation method and application thereof, which are used for solving the defects of limited measurement range, limited sensitivity and complex calibration caused by the fact that the application of the rare earth luminescent material in a near infrared region is generally based on single-mode temperature detection. The chemical formula of the rare earth luminescent material is NaY (1‑x‑y‑z)F4:xNd3+/yYb3+/zGd3+@SiO2 @PDA, wherein x is more than or equal to 1% and less than or equal to 3%, y is more than or equal to 5% and less than or equal to 20%, and z is more than or equal to 0% and less than or equal to 88.5%; the Yb 3+、Nd3+、Gd3+ doped ions simultaneously have two luminescence peaks of 850-930 nanometers and 930-1100 nanometers under the excitation of 808 nanometer laser through energy transfer, thereby realizing the functions of dual-mode near infrared light temperature sensing and CT imaging and solving the problem of limited measurement range.
Description
Technical Field
The invention relates to a rare earth luminescent material, in particular to a rare earth luminescent material, a preparation method and application thereof.
Background
The rare earth luminescent material has luminescent characteristics which are incomparable with other materials, such as rich energy level, long luminescent life, narrow luminescent line and high color purity, because the rare earth luminescent material obtains rich luminescence from ultraviolet to visible to infrared based on the special electron arrangement of doped rare earth ions (Kumar,R.;Nyk,M.;Ohulchanskyy,T.Y;Flask,C.A.;Pras,P.N.,Combined Optical and MR Bioimaging Using Rare Earth Ion Doped NaYF4 Nanocrystals.Adv.Funct.Mater,2009,1 9,853-859.).
Rare earth luminescent materials are very widely used in the Near Infrared (NIR) region. The near infrared wavelengths range from 700 nm to 2500 nm, which has many advantages such as lower absorption and scattering, better penetration properties, etc. The application of rare earth luminescent materials in this wavelength range mainly comprises the following aspects: (1) optical fiber communication: the rare earth luminescent material can emit light with specific wavelength in the near infrared region and is used for an optical fiber amplifier and an optical fiber laser, so that high-speed and long-distance optical fiber communication transmission is realized; (2) biomedical imaging: near infrared light has better penetrability in biological tissues, and can not cause obvious damage to the tissues; the rare earth luminescent material can be used as a near infrared fluorescent probe for biological marking and biological imaging; they can be used for intracellular markers, imaging of living small animals, visualization of human tissue, and the like; (3) sensor technology: there are many characteristic spectra in the near infrared region of wavelengths that interact with matter; the rare earth luminescent material can detect and analyze information such as chemical components, temperature change, gas concentration and the like in a sample by emitting light with specific wavelength and measuring the change of spectrum; therefore, the rare earth luminescent material is widely applied to the fields of spectrum sensors, chemical sensors and the like; (4) laser technology: the near infrared laser has important application in the fields of laser medicine, spectrum analysis, laser radar and the like; the rare earth luminescent material can be used as an activator of a near infrared laser, and emits laser photons after absorbing external energy, so that high-energy and high-power near infrared laser output is realized.
In summary, the rare earth luminescent material has very wide application in the near infrared region, and relates to the fields of optical communication, biomedical imaging, sensor technology, laser technology and the like. These applications make use of the characteristics of near infrared light and the luminescent characteristics of rare earth luminescent materials, but are generally based on single-mode temperature detection, resulting in the following drawbacks:
(1) Limiting the measurement range: single-mode temperature detection generally relies on the characteristic variation of a single transmission mode in an optical fiber, which means that it has a certain limit on the range of temperature variation, and if the temperature variation exceeds the sensitive range of the transmission mode, the measurement result may lose accuracy;
(2) Sensitivity is limited: the sensitivity of single-mode temperature detection may be limited, particularly in the case of small temperature changes, if the temperature change is too weak, a higher sensitivity may be required for detection and measurement;
(3) Complex calibration is required: in order to obtain accurate temperature measurements, single-mode temperature detection typically requires calibration; this involves establishing a temperature-characteristic curve or performing a calibration using a standard temperature source, which can be complex and time consuming.
Disclosure of Invention
The invention aims to solve the defects of limited measurement range, limited sensitivity and more complex calibration caused by the fact that the application of a rare earth luminescent material in a near infrared region is generally based on single-mode temperature detection, and provides a rare earth luminescent material, a preparation method and application thereof.
In order to solve the defects existing in the prior art, the invention provides the following technical solutions:
the rare earth luminescent material is characterized in that: the chemical formula of the catalyst is NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3 +@SiO2 @PDA, wherein x is more than or equal to 1% and less than or equal to 3%, y is more than or equal to 5% and less than or equal to 20%, and z is more than or equal to 0% and less than or equal to 88.5%.
Meanwhile, the invention provides a preparation method of the rare earth luminescent material, which is characterized by comprising the following steps:
Step 1, preparing NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+ by adopting a thermal decomposition method, wherein x is more than or equal to 1% and less than or equal to 3%, y is more than or equal to 5% and less than or equal to 20%, and z is more than or equal to 0% and less than or equal to 88.5%;
step 2, preparing NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 by using NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+ prepared in the step 1 as a raw material through a microemulsion method;
And 3, preparing NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @PDA by using the NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 prepared in the step 2 as a raw material and adopting a colloid chemical synthesis method.
Further, the step 1 specifically includes:
Step 1.1, mixing and reacting N1 mol of yttrium chloride hexahydrate, N2 mol of neodymium chloride hexahydrate, N3 mol of ytterbium chloride hexahydrate, N4 mol of gadolinium chloride hexahydrate, oleic acid and octadecene under the protection of argon environment and at the temperature of T4 ℃ to obtain a solution A, and naturally cooling the solution A to room temperature under the continuous protection of argon;
wherein, N1:N2:N3:N4= (1-x-y-z): x:y:z, T4=100-200;
Step 1.2, dissolving N5 mol of ammonium fluoride in a methanol solution to obtain a transparent solution B; dissolving N6 mol of sodium hydroxide in a methanol solution to obtain a transparent solution C, wherein N1, N2, N3, N4, N5, N6= (1-x-y-z) x, y, z, and 4:1;
Step 1.3, dropwise adding the solution B and the solution C into the solution A at the same time, and mixing and reacting under the condition of normal temperature argon to obtain a suspension D;
Step 1.4, heating the suspension D to a preset temperature T1 ℃ and preserving heat for a preset time T1 min, and then continuously heating to a preset temperature T2 ℃ and preserving heat for a preset time T2 min;
Wherein t1=60 to 90, t2=108 to 110, t2=5 to 10;
Step 1.5, closing argon, vacuumizing a reaction environment, and continuously introducing argon;
Step 1.6, after preserving heat at a preset temperature T3 ℃ for a preset time T3 minutes, cooling to room temperature, closing argon, and centrifugally washing the obtained solution E to obtain NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+;
T3＝250～350,t3＝20～40。
further, the step 2 specifically includes:
Dispersing NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+ prepared in the step 1 into absolute ethyl alcohol and deionized water solution, adding ammonia water, dripping tetraethyl orthosilicate, and centrifugally washing and drying the obtained solution to obtain NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2.
Further, in the step 2, the amount of the tetraethyl orthosilicate substance is equal to or more than the amount of the NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+ substance.
Further, the step 3 specifically includes:
Dissolving NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 prepared in the step 2 in deionized water, regulating the pH value of the solution to be 8.5+/-0.2 by using a tris hydrochloride buffer solution, adding dopamine, heating, stirring at room temperature for at least 8 hours, and centrifugally washing and drying the obtained solution to obtain NaYF 4:Nd3+/Yb3+/Gd3+@SiO2 @PDA.
The invention also provides application of the rare earth luminescent material in preparing a dual-mode near-infrared temperature sensing material.
The invention also provides an application of the rare earth luminescent material in preparing optical imaging materials.
Compared with the prior art, the invention has the beneficial effects that:
(1) The chemical formula of the rare earth luminescent material is NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @PDA, wherein x is more than or equal to 1% and less than or equal to 3%, y is more than or equal to 5% and less than or equal to 20%, and z is more than or equal to 0% and less than or equal to 88.5%; the Yb 3+、Nd3+、Gd3+ doped ions simultaneously have two luminescence peaks of 850-930 nanometers and 930-1100 nanometers under the excitation of 808 nanometer laser through energy transfer, thereby realizing the functions of dual-mode near infrared light temperature sensing and CT imaging and solving the problem of limited measurement range.
(2) The rare earth luminescent material is of a nano core-shell structure, can enhance the luminous intensity under the excitation of laser (808 nm) positioned in a first biological window area, realizes the functions of temperature sensing and optical imaging, and solves the problem of limited sensitivity.
(3) The preparation method of the rare earth luminescent material is simple to operate, and the synthesized sample has the particle size of about 25 nanometers, is easier to uniformly disperse in aqueous solution, and has good biocompatibility.
Drawings
FIG. 1 is an XRD pattern of NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @PDA prepared in example one of the rare earth luminescent materials of the present invention;
FIG. 2 is an electron transmission microscope image of NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @PDA prepared in accordance with an embodiment of the present invention at a scale of 50 nm;
FIG. 3 is an electron transmission microscope image of NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @PDA prepared in accordance with an embodiment of the present invention at a scale of 20 nm;
FIG. 4 shows the near infrared spectrum of NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @ PDA prepared in accordance with example I of the present invention;
FIG. 5 is a graph showing the relationship between the luminous intensity ratio of NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @PDA prepared in the first embodiment of the invention and the temperature at 850-930 nm;
FIG. 6 is a graph showing the relationship between the luminous intensity ratio of NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @PDA prepared in the first embodiment of the invention at 930-1100 nm and the temperature;
FIG. 7 shows the near infrared spectrum of NaY (1-x-y-z)F4:xNd3+/yYb3+ prepared in example two of the present invention.
Detailed Description
The invention is further described below with reference to the drawings and exemplary embodiments.
In the present invention "@" means a relationship of core-shell structure, for example, "NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2" means "SiO 2 coated NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+", and so on.
Example 1
A preparation method of rare earth luminescent material comprises the following steps:
Step 1, preparing NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+ by adopting a thermal decomposition method;
Step 1.1, mixing and reacting N1 mol of yttrium chloride hexahydrate (YCl3.6H2O), N2 mol of neodymium chloride hexahydrate (NdCl3.6H2O), N3 mol of ytterbium chloride hexahydrate (YbCl3.6H2O), N4 mol of gadolinium chloride hexahydrate (GdCl3.6H2O), 12ml of oleic acid and 30ml of octadecyl sodium sulfate under the protection of argon environment at the temperature of T4 ℃ to obtain a solution A, and naturally cooling the solution A to the room temperature under the continuous protection of argon; n1:n2:n3:n4= (1-x-y-z): x:y:z=0.385:0.015:0.1:0.5, n4=0.001 mol, t4=160;
Step 1.2, dissolving N5 mol of ammonium fluoride in a methanol solution to obtain a transparent solution B, n5=0.008; dissolving N6 mol sodium hydroxide in methanol solution to obtain transparent solution C, n6=0.002;
Step 1.3, dropwise adding the solution B and the solution C into the solution A at the same time, and mixing and reacting under the condition of normal temperature argon to obtain a suspension D;
step 1.4, heating the suspension D to a preset temperature T1 ℃ and preserving heat for a preset time T1 min, and then continuously heating to a preset temperature T2 ℃ and preserving heat for a preset time T2 min; t1=60, t2=108, t2=5;
Step 1.5, closing argon, vacuumizing a reaction environment, and continuously introducing argon;
Step 1.6, after preserving heat at a preset temperature T3 ℃ for a preset time T3 minutes, cooling to room temperature, closing argon, and centrifugally washing the obtained solution E to obtain NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+, wherein NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+ (0.002 mol) can be dispersed in 20ml of cyclohexane to be used as a solution F;
T3＝300，t3＝30；
step 2, preparing NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 by using NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+ prepared in the step 1 as a raw material through a microemulsion method;
Dispersing NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+ prepared in the step 1 into absolute ethyl alcohol and deionized water solution, adding ammonia water, dripping tetraethyl orthosilicate, and performing centrifugal washing and drying on the obtained solution to obtain NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2;
The amount of tetraethyl orthosilicate material is equal to 0.002mol;
Step 3, preparing NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @PDA by using NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 prepared in step 2 as a raw material and adopting a colloid chemical synthesis method;
The NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 prepared in step 2 was dissolved in deionized water, the ph=8.5 of the solution was adjusted with 30ml of Tris-HCl buffer, then dopamine was added and heated (DA) was added and stirred at room temperature for 8 hours, DA spontaneously oxidized to adherent Polymeric Dopamine (PDA) and spontaneously deposited on any substrate, and the resulting solution was dried by centrifugation to yield NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @ PDA.
The XRD pattern of NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @ PDA prepared in this example is shown in FIG. 1, and NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @ PDA is the same as NaYF 4 standard, and has the correct phase structure.
The electron transmission microscope images of NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @PDA prepared in this example are shown in FIGS. 2 and 3, which show that NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @PDA has good dispersibility and a particle size of about 25 nanometers.
The optical performance of the NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @pda prepared in this example was characterized, and the obtained near infrared spectrum is shown in fig. 4, which shows the near infrared emission of NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @pda at 850-930 nm as sensor 1 and the fluorescence emission at 930-1100 nm as sensor 2.
The optical performance of NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @pda prepared in this example was characterized, and the fluorescent intensity ratio temperature measurement technique disclosed in document [1] and document [2] was used to obtain the relationship curve of the luminous intensity ratio and temperature, and the results are shown in fig. 5 and 6, which show that both sensor 1 and sensor 2 have temperature sensing performance.
Wherein, the document [1] is ：Zhiyu Zhang,Minkun Jin,Leyi Yao,Chongfeng Guo.NIR dual-mode temperature sensor based on FIR technology in BaYF5:Nd3+/Yb3+.Optical Materials 121(2021)111607.
Document [2] is ：Suo,H.,Zhao,X.,Zhang,Z.,Guo,C.808nm Light-triggered Thermometer-Heater Up-converting Platform based on Nd3+-sensitized Yolk-shell GdOF@SiO2.ACS Appl.Mater.Interfaces 2017,9,43438-43448.
Example two
A preparation method of rare earth luminescent material comprises the following steps:
Step 1, preparing NaY (1-x-y-z)F4:xNd3+/yYb3+ by adopting a thermal decomposition method;
Step 1.1, mixing and reacting N1 mol of yttrium chloride hexahydrate, N2 mol of neodymium chloride hexahydrate, N3 mol of ytterbium chloride hexahydrate, 12ml of oleic acid and 30ml of octadecene under the protection of argon environment at the temperature of T4 ℃ to obtain a solution A, and naturally cooling the solution A to room temperature under the continuous protection of argon; n1:n2:n3= (1-x-y-z): x:y=0.885:0.015:0.1, n1= 0.00177mol; t4=160;
Step 1.2, dissolving N5 mol of ammonium fluoride in a methanol solution to obtain a transparent solution B, n5=0.008; dissolving N6 mol sodium hydroxide in methanol solution to obtain transparent solution C, n6=0.002;
Step 1.3, dropwise adding the solution B and the solution C into the solution A at the same time, and mixing and reacting under the condition of normal temperature argon to obtain a suspension D;
step 1.4, heating the suspension D to a preset temperature T1 ℃ and preserving heat for a preset time T1 min, and then continuously heating to a preset temperature T2 ℃ and preserving heat for a preset time T2 min; t1=60, t2=108, t2=5;
Step 1.5, closing argon, vacuumizing a reaction environment, and continuously introducing argon;
Step 1.6, after preserving heat at a preset temperature T3 ℃ for a preset time T3 minutes, cooling to room temperature, closing argon, and centrifugally washing the obtained solution E to obtain NaY (1-x-y-z)F4:xNd3+/yYb3+, wherein NaY (1-x-y-z)F4:xNd3+/yYb3+ can be dispersed in 20ml of cyclohexane to be used as a solution F;
T3＝300，t3＝30；
Step 2 of this example, the amount of tetraethyl orthosilicate material was equal to 0.003mol;
the rest of the settings in step 2 and step 3 of this embodiment are the same as those in the first embodiment.
The optical performance of NaY (1-x-y-z)F4:xNd3+/yYb3+ prepared in this example was characterized, and the near infrared spectrum obtained is shown in fig. 7, which shows the near infrared emission of NaY (1-x-y-z)F4:xNd3+/yYb3+ at 850-930 nm as sensor 1 and the fluorescence emission at 930-1100 nm as sensor 2.
Example III
A preparation method of rare earth luminescent material comprises the following steps:
step 1, preparing NaGd zF4:xNd3+/yYb3+ by adopting a thermal decomposition method;
Step 1.1, mixing and reacting N4 mol of gadolinium chloride hexahydrate, N2 mol of neodymium chloride hexahydrate, N3 mol of ytterbium chloride hexahydrate, 12ml of oleic acid and 30ml of octadecene under the protection of argon environment at the temperature of T4 ℃ to obtain a solution A, and naturally cooling the solution A to room temperature under the continuous protection of argon; n4:n2:n3=z:x:y=0.885:0.015:0.1, n4= 0.00177mol; t4=160;
Step 1.2, dissolving N5 mol of ammonium fluoride in a methanol solution to obtain a transparent solution B, n5=0.008; dissolving N6 mol sodium hydroxide in methanol solution to obtain transparent solution C, n6=0.002;
Step 1.3, dropwise adding the solution B and the solution C into the solution A at the same time, and mixing and reacting under the condition of normal temperature argon to obtain a suspension D;
Step 1.4, heating the suspension D to a preset temperature T1 ℃ and preserving heat for a preset time T1 min, and then continuously heating to a preset temperature T2 ℃ and preserving heat for a preset time T2 min; t1=70, t2=109, t1=7;
Step 1.5, closing argon, vacuumizing a reaction environment, and continuously introducing argon;
Step 1.6, after preserving heat at a preset temperature T3 ℃ for a preset time T3 minutes, cooling to room temperature, closing argon, centrifugally washing the obtained solution E to obtain NaGd zF4:xNd3+/yYb3+, and dispersing NaGd zF4:xNd3+/yYb3+ into 20ml cyclohexane to obtain a solution F for later use;
T3＝290，t3＝40；
Step 2 and step 3 of this embodiment are the same as those of the first embodiment.
Example IV
A preparation method of rare earth luminescent material comprises the following steps:
step 1, preparing NaY 1-x-y-zF4:xNd3+/yYb3+ by adopting a thermal decomposition method;
Step 1.1, mixing and reacting N1 mol of yttrium chloride hexahydrate, N2 mol of neodymium chloride hexahydrate, N3 mol of ytterbium chloride hexahydrate, 12ml of oleic acid and 30ml of octadecene under the protection of argon environment at the temperature of T4 ℃ to obtain a solution A, and naturally cooling the solution A to room temperature under the continuous protection of argon; n1:n2:n3= (1-x-y-z): x:y=0.89:0.01:0.1, n2=0.00002 mol; t4=100;
Step 1.2, dissolving N5 mol of ammonium fluoride in a methanol solution to obtain a transparent solution B, n5=0.008; dissolving N6 mol sodium hydroxide in methanol solution to obtain transparent solution C, n6=0.002;
Step 1.3, dropwise adding the solution B and the solution C into the solution A at the same time, and mixing and reacting under the condition of normal temperature argon to obtain a suspension D;
Step 1.4, heating the suspension D to a preset temperature T1 ℃ and preserving heat for a preset time T1 min, and then continuously heating to a preset temperature T2 ℃ and preserving heat for a preset time T2 min; t1=90, t1=60, t2=110, t1=10;
Step 1.5, closing argon, vacuumizing a reaction environment, and continuously introducing argon;
step 1.6, after preserving heat at a preset temperature T3 ℃ for a preset time T3 minutes, cooling to room temperature, closing argon, and centrifugally washing the obtained solution E to obtain NaY 1-x-y-zF4:xNd3+/yYb3+, wherein NaY 1-x-y-zF4:xNd3+/yYb3+ can be dispersed in 20ml of cyclohexane to be used as a solution F;
T3＝350，t3＝20；
Step 2 and step 3 of this embodiment are the same as those of the first embodiment.
Example five
A preparation method of rare earth luminescent material comprises the following steps:
step 1, preparing NaY 1-x-y-zF4:xNd3+/yYb3+ by adopting a thermal decomposition method;
Step 1.1, mixing and reacting N1 mol of yttrium chloride hexahydrate, N2 mol of neodymium chloride hexahydrate, N3 mol of ytterbium chloride hexahydrate, 12ml of oleic acid and 30ml of octadecene under the protection of argon environment at the temperature of T4 ℃ to obtain a solution A, and naturally cooling the solution A to room temperature under the continuous protection of argon; n1:n2:n3= (1-x-y-z): x:y=0.87:0.03:0.1, n2=0.00006 mol; t4=200;
Step 1.2, dissolving N5 mol of ammonium fluoride in a methanol solution to obtain a transparent solution B, n5=0.008; dissolving N6 mol sodium hydroxide in methanol solution to obtain transparent solution C, n6=0.002;
Step 1.3, dropwise adding the solution B and the solution C into the solution A at the same time, and mixing and reacting under the condition of normal temperature argon to obtain a suspension D;
step 1.4, heating the suspension D to a preset temperature T1 ℃ and preserving heat for a preset time T1 min, and then continuously heating to a preset temperature T2 ℃ and preserving heat for a preset time T2 min; t1=60, t1=90, t2=108, t2=5;
Step 1.5, closing argon, vacuumizing a reaction environment, and continuously introducing argon;
step 1.6, after preserving heat at a preset temperature T3 ℃ for a preset time T3 minutes, cooling to room temperature, closing argon, and centrifugally washing the obtained solution E to obtain NaY 1-x-y-zF4:xNd3+/yYb3+, wherein NaY 1-x-y-zF4:xNd3+/yYb3+ can be dispersed in 20ml of cyclohexane to be used as a solution F;
T3＝300，t3＝30；
Step 2 and step 3 of this embodiment are the same as those of the first embodiment.
Example six
A preparation method of rare earth luminescent material comprises the following steps:
step 1, preparing NaY 1-x-y-zF4:xNd3+/yYb3+ by adopting a thermal decomposition method;
Step 1.1, mixing and reacting N1 mol of yttrium chloride hexahydrate, N2 mol of neodymium chloride hexahydrate, N3 mol of ytterbium chloride hexahydrate, 12ml of oleic acid and 30ml of octadecene under the protection of argon environment at the temperature of T4 ℃ to obtain a solution A, and naturally cooling the solution A to room temperature under the continuous protection of argon; n1:n2:n3= (1-x-y-z): x:y=0.96:0.01:0.05, n3=0.00010 mol; t4=160;
Step 1.2, dissolving N5 mol of ammonium fluoride in a methanol solution to obtain a transparent solution B, n5=0.008; dissolving N6 mol sodium hydroxide in methanol solution to obtain transparent solution C, n6=0.002;
Step 1.3, dropwise adding the solution B and the solution C into the solution A at the same time, and mixing and reacting under the condition of normal temperature argon to obtain a suspension D;
step 1.4, heating the suspension D to a preset temperature T1 ℃ and preserving heat for a preset time T1 min, and then continuously heating to a preset temperature T2 ℃ and preserving heat for a preset time T2 min; t1=60, t2=108, t2=5;
Step 1.5, closing argon, vacuumizing a reaction environment, and continuously introducing argon;
step 1.6, after preserving heat at a preset temperature T3 ℃ for a preset time T3 minutes, cooling to room temperature, closing argon, and centrifugally washing the obtained solution E to obtain NaY 1-x-y-zF4:xNd3+/yYb3+, wherein NaY 1-x-y-zF4:xNd3+/yYb3+ can be dispersed in 20ml of cyclohexane to be used as a solution F;
T3＝300，t3＝30；
Step 2 and step 3 of this embodiment are the same as those of the first embodiment.
Example seven
The preparation method of the rare earth luminescent material comprises the following steps:
step 1, preparing NaY 1-x-y-zF4:xNd3+/yYb3+ by adopting a thermal decomposition method;
Step 1.1, mixing and reacting N1 mol of yttrium chloride hexahydrate, N2 mol of neodymium chloride hexahydrate, N3 mol of ytterbium chloride hexahydrate, 12ml of oleic acid and 30ml of octadecene under the protection of argon environment at the temperature of T4 ℃ to obtain a solution A, and naturally cooling the solution A to room temperature under the continuous protection of argon; n1:n2:n3= (1-x-y-z): x:y=0.79:0.01:0.2, n3=0.00040 mol; t4=160;
Step 1.2, dissolving N5 mol of ammonium fluoride in a methanol solution to obtain a transparent solution B, n5=0.008; dissolving N6 mol sodium hydroxide in methanol solution to obtain transparent solution C, n6=0.002;
Step 1.3, dropwise adding the solution B and the solution C into the solution A at the same time, and mixing and reacting under the condition of normal temperature argon to obtain a suspension D;
Step 1.4, heating the suspension D to a preset temperature T1 ℃ and preserving heat for a preset time T1 min, and then continuously heating to a preset temperature T2 ℃ and preserving heat for a preset time T2 min; t1=60, t1=20, t2=108, t2=5;
Step 1.5, closing argon, vacuumizing a reaction environment, and continuously introducing argon;
step 1.6, after preserving heat at a preset temperature T3 ℃ for a preset time T3 minutes, cooling to room temperature, closing argon, and centrifugally washing the obtained solution E to obtain NaY 1-x-y-zF4:xNd3+/yYb3+, wherein NaY 1-x-y-zF4:xNd3+/yYb3+ can be dispersed in 20ml of cyclohexane to be used as a solution F;
T3＝300，t3＝30；
Step 2 and step 3 of this embodiment are the same as those of the first embodiment.
The specific parameters of examples one to seven are shown in table 1:
TABLE 1
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Claims (8)
1. A rare earth luminescent material, characterized in that: the chemical formula of the compound is NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @PDA, wherein x is more than or equal to 1% and less than or equal to 3%, y is more than or equal to 5% and less than or equal to 20%, z=0, or x=1.5%, y=10%, and z is more than or equal to 50% and less than or equal to 88.5%, and the PDA is polymerized dopamine.
2. A method for preparing the rare earth luminescent material according to claim 1, comprising the steps of:
Step 1, preparing NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+ by adopting a thermal decomposition method, wherein x is more than or equal to 1% and less than or equal to 3%, y is more than or equal to 5% and less than or equal to 20%, and z=0, or x=1.5%, y=10%, and z is more than or equal to 50% and less than or equal to 88.5%;
step 2, preparing NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 by using NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+ prepared in the step 1 as a raw material through a microemulsion method;
And 3, preparing NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 @PDA by using the NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 prepared in the step 2 as a raw material and adopting a colloid chemical synthesis method.
3. The method for preparing a rare earth luminescent material according to claim 2, wherein the step 1 specifically comprises:
Step 1.1, mixing and reacting N1 mol of yttrium chloride hexahydrate, N2 mol of neodymium chloride hexahydrate, N3 mol of ytterbium chloride hexahydrate, N4 mol of gadolinium chloride hexahydrate, oleic acid and octadecene under the protection of argon environment and at the temperature of T4 ℃ to obtain a solution A, and naturally cooling the solution A to room temperature under the continuous protection of argon;
wherein, N1:N2:N3:N4= (1-x-y-z): x:y:z, T4=100-200;
Step 1.2, dissolving N5 mol of ammonium fluoride in a methanol solution to obtain a transparent solution B; dissolving N6 mol of sodium hydroxide in a methanol solution to obtain a transparent solution C, wherein N1, N2, N3, N4, N5, N6= (1-x-y-z) x, y, z, and 4:1;
Step 1.3, dropwise adding the solution B and the solution C into the solution A at the same time, and mixing and reacting under the condition of normal temperature argon to obtain a suspension D;
Step 1.4, heating the suspension D to a preset temperature T1 ℃ and preserving heat for a preset time T1 min, and then continuously heating to a preset temperature T2 ℃ and preserving heat for a preset time T2 min;
Wherein t1=60 to 90, t2=108 to 110, t2=5 to 10;
Step 1.5, closing argon, vacuumizing a reaction environment, and continuously introducing argon;
Step 1.6, after preserving heat at a preset temperature T3 ℃ for a preset time T3 minutes, cooling to room temperature, closing argon, and centrifugally washing the obtained solution E to obtain NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+;
T3＝250～350,t3＝20～40。
4. The method for preparing a rare earth luminescent material according to claim 2, wherein the step 2 specifically comprises:
Dispersing NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+ prepared in the step 1 into absolute ethyl alcohol and deionized water solution, adding ammonia water, dripping tetraethyl orthosilicate, and centrifugally washing and drying the obtained solution to obtain NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2.
5. The method for preparing a rare earth luminescent material according to claim 4, wherein: in the step 2, the amount of the tetraethyl orthosilicate substance is more than or equal to the amount of the NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+ substance.
6. The method for preparing a rare earth luminescent material according to claim 2, wherein the step 3 specifically comprises:
Dissolving NaY (1-x-y-z)F4:xNd3+/yYb3+/zGd3+@SiO2 prepared in the step 2 in deionized water, regulating the pH value of the solution to be 8.5+/-0.2 by using a tris hydrochloride buffer solution, adding dopamine, heating, stirring at room temperature for at least 8 hours, and centrifugally washing and drying the obtained solution to obtain NaYF 4:Nd3+/Yb3+/Gd3+@SiO2 @PDA.
7. Use of the rare earth luminescent material according to claim 1 for preparing a dual-mode near-infrared temperature sensing material.
8. Use of the rare earth luminescent material according to claim 1 for the preparation of an optical imaging material.
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