CN114606002A - Red-light fluoride nanocrystalline scintillator and preparation method thereof - Google Patents
Red-light fluoride nanocrystalline scintillator and preparation method thereof Download PDFInfo
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- CN114606002A CN114606002A CN202210176315.6A CN202210176315A CN114606002A CN 114606002 A CN114606002 A CN 114606002A CN 202210176315 A CN202210176315 A CN 202210176315A CN 114606002 A CN114606002 A CN 114606002A
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- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 8
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000005642 Oleic acid Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 8
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 8
- 239000011258 core-shell material Substances 0.000 claims abstract description 7
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims abstract description 5
- GAPRPFRDVCCCHR-UHFFFAOYSA-N 3-bromoprop-1-ynyl(trimethyl)silane Chemical compound C[Si](C)(C)C#CCBr GAPRPFRDVCCCHR-UHFFFAOYSA-N 0.000 claims abstract description 4
- LNYNHRRKSYMFHF-UHFFFAOYSA-K europium(3+);triacetate Chemical compound [Eu+3].CC([O-])=O.CC([O-])=O.CC([O-])=O LNYNHRRKSYMFHF-UHFFFAOYSA-K 0.000 claims abstract description 4
- 229940046892 lead acetate Drugs 0.000 claims abstract description 4
- 239000002159 nanocrystal Substances 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 150000002500 ions Chemical class 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 238000004020 luminiscence type Methods 0.000 claims description 10
- 239000011159 matrix material Substances 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910001385 heavy metal Inorganic materials 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 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 3
- 229910052765 Lutetium Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229910052745 lead Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 7
- 230000005284 excitation Effects 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 4
- 150000002367 halogens Chemical class 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 239000002096 quantum dot Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000005281 excited state Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- -1 rare earth ions Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/779—Halogenides
- C09K11/7791—Halogenides with alkali or alkaline earth metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention belongs to the field of inorganic luminescent materials. A red-light fluoride nanocrystalline scintillator with molecular formula of Ba1.8Pb1.2LuF10: eu, and the preparation method thereof comprises the following steps in sequence: barium acetate, lead acetate, 1 millimole of lutetium acetate, europium acetate, oleic acid and octadecene are mixed and reacted to obtain powdery nanocrystalline, mixed liquid of oleic acid and octadecene is used for heat treatment, and then ultrasonic treatment is carried out to obtain a final product. The adopted preparation method is simple, a complex core-shell structure or surface modification and the like are not required to be constructed, the product shows high-efficiency red light emission excited by X rays, and the method has good application prospect in the field of X-ray detection.
Description
Technical Field
The invention belongs to the field of scintillation crystals, and relates to a high-efficiency nanocrystalline scintillator.
Background
The halogen perovskite quantum dot has the advantages of simple preparation method, low cost and high X-ray absorption cross section, can effectively convert X-ray photons into visible photons, and is considered as a scintillator material with potential application prospect. However, such materials have the following disadvantages: the commonly used halogens are Cl, Br and I, the products are ionic crystals, the stability is very poor, and the fluorescence property is very easy to decline. Although a few fluoride systems with high stability also have scintillation property, the matrix has poor X-ray absorption capacity and low light yield, so the development of the efficient scintillator based on the new matrix has very application prospect and scientific significance.
Through specific analysis of relevant knowledge points, the reason that the halogen perovskite quantum dots have high absorption cross sections is that the halogen perovskite quantum dots contain heavy metal elements, particularly Pb, and fluoride systems are generally applied to the fields of biological imaging and the like, and the safety of the fluoride systems needs to be ensured, so that the matrix does not contain Pb elements. For X-ray imaging, the scintillator may be packaged to ensure its safety, in other words, the scintillator may contain a certain amount of Pb element. Based on this, the present invention employs Ba1.8Pb1.2LuF10As a matrix, by doping Eu3+The ion realizes the red light nanocrystalline scintillator with high optical stability and high light yield, and has larger difference with the current common green light scintillator.
Disclosure of Invention
The invention discloses a red-light fluoride nanocrystalline scintillator, which adopts a solvothermal method to prepare Eu3+Ion-doped Ba1.8Pb1.2LuF10The nanocrystalline realizes red scintillation luminescence excited by high-efficiency X rays.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a red-light fluoride nanocrystalline scintillator comprises the following steps:
(1) 1.8 millimole of barium acetate, 1.2, according to mole percentageAdding millimole lead acetate, 1 millimole lutetium acetate and 0.05-0.2 millimole europium acetate into a mixed solution containing 6-8 ml oleic acid and 8-12 ml octadecene, and preserving the heat for 1 hour at the temperature of 150 ℃ under the protection of nitrogen to obtain an anhydrous transparent solution; (2) after the solution is naturally cooled to room temperature, 4-6 ml of methanol solution containing 8-12 mmol of ammonium fluoride is added into the solution drop by drop, and then the temperature is kept for half an hour at 80 ℃; (3) after the methanol solution is completely volatilized, quickly heating to the temperature of 290 ℃ and 310 ℃, preserving the heat for 80-120 minutes at the temperature, and naturally cooling to the room temperature; (4) washing the solution with mixed solution of ethanol and cyclohexane, and drying to obtain powdery nanocrystals; (5) the powdery nanocrystalline is put in the mixed solution containing 6-8 ml of oleic acid and 8-12 ml of octadecene and is preserved for 1-2 hours at the temperature of 150-; (6) washing the solution with a mixed solution of ethanol and cyclohexane, and drying to obtain powdery nanocrystals again; (7) continuously performing ultrasonic treatment on the powdery nanocrystalline in a high-power ultrasonic instrument for 2-4 hours to obtain the final Ba1.8Pb1.2LuF10: and 4, Eu nanocrystalline products.
The red-light fluoride nanocrystalline scintillator obtained by adopting the technical scheme has a chemical formula of Ba1.8Pb1.2LuF10: and Eu. The main characteristics are: firstly, the matrix contains heavy metal elements Pb and Lu at the same time, so that high-energy X rays can be effectively converted into low-energy secondary electrons; secondly, the substrate contains heavy metal element Pb2+And Ba2+Ions enabling the host lattice to sustain Ba3LuF10The crystal structure of (2) improves the stability of X-ray irradiation; III, Ba1.8Pb1.2LuF10Conduction band and Eu3+The 5d energy level of the ion is close to the position, and electrons captured by inherent defects in crystal lattice can quickly return to Eu through conduction band3+The ion 5d energy level is filled in the 4f energy level, so that afterglow luminescence is greatly inhibited, and afterglow luminescence is an important performance index of the scintillator; IV, Eu3+The 5d energy level and the 4f energy level of the ions can indirectly or directly capture a large amount of secondary electrons, and then strong red light is generated; fifthly, reconstructing atoms on the surface of the nanocrystalline by solvent heat treatment and ultrasonic treatment to reduce the surfaceAnd the red light flicker intensity is greatly improved. In addition, the preparation method adopted by the invention is simple, a complex core-shell structure or surface modification and the like do not need to be constructed, and the obtained product has high yield, good dispersibility and uniform shape. The method provides a new matrix system for developing a high-performance red light scintillator material.
Drawings
FIG. 1: example Ba1.8Pb1.2LuF10: x-ray diffraction pattern of Eu nanocrystal
FIG. 2: example Ba1.8Pb1.2LuF10: transmission electron microscope image of Eu nanocrystal
FIG. 3: example Ba1.8Pb1.2LuF10: fluorescence spectrum of Eu nanocrystal under X-ray excitation
FIG. 4 is a schematic view of: example Ba1.8Pb1.2LuF10: the luminous intensity of Eu nanocrystal under the condition of X-ray excitation and Eu3+Ion concentration relation curve
FIG. 5: example Ba1.8Pb1.2LuF10: the flash spectrograms of Eu nanocrystalline before and after solvent heat treatment are that before heat treatment the intensity is lower
FIG. 6: example Ba1.8Pb1.2LuF10: scintillation spectrogram of Eu nanocrystalline before and after ultrasonic treatment
FIG. 7: example Ba1.8Pb1.2LuF10: stability of Eu nanocrystals under X-ray irradiation
FIG. 8: comparative example Pb3LuF10: stability of Eu nanocrystals under X-ray irradiation
FIG. 9: comparative example Ba3LuF10: eu nanocrystal and example Ba1.8Pb1.2LuF10: the contrast graph of fluorescence intensity of Eu nanocrystal under X-ray excitation is Ba3LuF10: eu nanocrystal
Detailed Description
This patent is further described below in conjunction with fig. 1-9.
Examples
A red-light fluoride nanocrystalline scintillator with the chemical formula of Ba1.8Pb1.2LuF10：Eu。
Ba1.8Pb1.2LuF10: the preparation method of Eu comprises the following steps in sequence: (1) adding 1.8 mmol of barium acetate, 1.2 mmol of lead acetate, 1 mmol of lutetium acetate and 0.1 mmol of europium acetate into a mixed solution containing 8 ml of oleic acid and 8 ml of octadecene, and preserving the heat at 150 ℃ for 1 hour under the protection of nitrogen to obtain an anhydrous transparent solution; (2) after the solution is naturally cooled to room temperature, 4 ml of methanol solution containing 8 mmol of ammonium fluoride is added into the solution dropwise, and then the temperature is kept at 80 ℃ for half an hour; (3) after the methanol solution is completely volatilized, quickly heating to 290 ℃, preserving the heat for 100 minutes at the temperature, and naturally cooling to room temperature; (4) washing the solution with mixed solution of ethanol and cyclohexane, and drying to obtain powdery nanocrystals; (5) keeping the temperature of the powdery nanocrystal in a mixed solution containing 8 ml of oleic acid and 12 ml of octadecene at 170 ℃ for 1 hour; (6) washing the solution with a mixed solution of ethanol and cyclohexane, and drying to obtain powdery nanocrystals again; (7) continuously carrying out ultrasonic treatment on the powdery nanocrystalline for 3 hours in a high-power ultrasonic instrument to obtain the final Ba1.8Pb1.2LuF10: and 4, Eu nanocrystalline products.
Ba prepared by the above method1.8Pb1.2LuF10: eu nanocrystals, powder X-ray diffraction analysis shows that the synthesized product is pure cubic phase (figure 1), and transmission electron microscope analysis shows that the product is cubic and has an average grain size of 10 nm (figure 2); under the condition of X-ray excitation, the nanocrystal shows Eu3+Corresponding to the 4f-4f transition (fig. 3), it should be noted that after stopping the X-ray excitation, the afterglow spectrum is hardly detected; the rare earth ions have rich energy level structures, and the matching degree of secondary electrons in excited state energy levels has a remarkable influence on the luminescence performance, as shown in FIG. 4, along with Eu3+The ion doping concentration is gradually increased from 1 to 6 percent (mol percent), the luminous intensity is enhanced by about 5 times, and the ion doping concentration is mainly caused by the increase of the number of excited state energy levelsStrongly contributing to the enhancement of the electron capturing efficiency, but Eu3+When the ion doping concentration exceeds 6%, the luminous intensity begins to decrease. As can be seen from fig. 5, after the solvothermal treatment, the scintillation luminescence intensity is significantly improved, which indicates that the solvothermal treatment can promote the atomic reconstruction of the indicated defect, reduce the defect concentration, and reduce the probability of radiationless relaxation, thereby enhancing luminescence. Similarly, as can be seen from fig. 6, after the ultrasonic treatment, the scintillation luminous intensity can be further improved. More importantly, as shown in fig. 7, the luminescent intensity of the nanocrystal is less changed under the condition of continuous irradiation of long-time X-rays, which is helpful for improving the stability of images.
The invention is characterized in that the heavy metal elements Pb and Lu in the matrix are utilized to greatly improve the X-ray absorption efficiency; by means of ion doping, the host crystal lattice can maintain Ba3LuF10The crystal structure of (1) improves the stability of X-ray irradiation and greatly inhibits afterglow luminescence; through solvent heat treatment and ultrasonic treatment, atoms on the surface of the nanocrystalline are reconstructed, surface defects are reduced, and the scintillation strength is greatly improved.
Comparative example 1
Comparative example Pb3LuF10: eu nanocrystal and example Ba1.8Pb1.2LuF10: the Eu nanocrystal preparation method is characterized in that the raw materials of the comparative example do not contain barium acetate.
Preparation of Pb according to the above method3LuF10: eu nanocrystalline, under X-ray excitation condition, the luminous intensity of Eu nanocrystalline is gradually weakened along with the prolonging of irradiation time, which shows that the Eu nanocrystalline shows poor X-ray irradiation stability, and the Ba in the substrate is proved from the reverse side2+The importance of the ion.
Comparative example 2
Comparative example Ba3LuF10: the difference between the preparation method of the Eu nano-crystal and the embodiment is that the raw material has no lead ions, and the product has no lead ions doped.
Preparation of Ba according to the above method3LuF10: eu nanocrystalline, under the condition of X-ray excitation, the scintillation luminescence of nanocrystalline is strongThe degree is obviously lower than that of the examples, which shows that the lead ions doped in the product are beneficial to improving the X-ray absorption coefficient, thereby enhancing the scintillation luminescence.
Claims (7)
1. A red-light fluoride nanocrystalline scintillator and a preparation method thereof are characterized in that the chemical formula is as follows: ba1.8Pb1.2LuF10：Eu。
2. The red-light fluoride nanocrystal scintillator and the preparation method thereof of claim 1, wherein the nanocrystal scintillator is an X-ray excited near-infrared luminescent nanocrystal.
3. The near-infrared fluoride core-shell nanocrystal scintillator of claim 1, wherein the matrix contains heavy metal elements Pb and Lu simultaneously, which can effectively convert high-energy X-rays into low-energy secondary electrons.
4. The near-infrared fluoride core-shell nanocrystal scintillator according to claim 1, wherein the matrix contains heavy metal element Pb at the same time2+And Ba2+Ions enabling the host lattice to sustain Ba3LuF10The crystal structure of (2) improves the stability of X-ray irradiation.
5. The near-infrared fluoride core-shell nanocrystal scintillator of claim 1, wherein Ba is present1.8Pb1.2LuF10Conduction band and Eu3+The position of the 5d energy level of the ion is close, and afterglow luminescence is greatly inhibited.
6. The near-infrared fluoride core-shell nanocrystal scintillator of claim 1, wherein Eu is3+The 5d energy level and the 4f energy level of the ion can indirectly or directly capture a large amount of secondary electrons, and then strong red light is generated.
7. A preparation method of a near-infrared fluoride core-shell nanocrystalline scintillator is characterized by sequentially comprising the following steps:
(1) adding 1.8 millimole of barium acetate, 1.2 millimole of lead acetate, 1 millimole of lutetium acetate and 0.05-0.2 millimole of europium acetate into a mixed solution containing 6-8 ml of oleic acid and 8-12 ml of octadecene according to the mol percentage, and preserving the heat for 1 hour at the temperature of 150 ℃ under the protection of nitrogen to obtain an anhydrous transparent solution;
(2) after the solution is naturally cooled to room temperature, 4-6 ml of methanol solution containing 8-12 mmol of ammonium fluoride is added into the solution drop by drop, and then the temperature is kept for half an hour at 80 ℃;
(3) after the methanol solution is completely volatilized, quickly heating to the temperature of 290 ℃ and 310 ℃, preserving the heat for 80-120 minutes at the temperature, and naturally cooling to the room temperature;
(4) washing the solution with mixed solution of ethanol and cyclohexane, and drying to obtain powdery nanocrystals; (5) the powdery nanocrystalline is put in the mixed solution containing 6-8 ml of oleic acid and 8-12 ml of octadecene and is preserved for 1-2 hours at the temperature of 150-; (6) washing the solution with a mixed solution of ethanol and cyclohexane, and drying to obtain powdery nanocrystals again; (7) continuously performing ultrasonic treatment on the powdery nanocrystalline in a high-power ultrasonic instrument for 2-4 hours to obtain the final Ba1.8Pb1.2LuF10: and 4, Eu nanocrystalline products.
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