CN110964527A - Method for controllably preparing strong-luminescence rare earth up-conversion material - Google Patents

Method for controllably preparing strong-luminescence rare earth up-conversion material Download PDF

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CN110964527A
CN110964527A CN201911290437.2A CN201911290437A CN110964527A CN 110964527 A CN110964527 A CN 110964527A CN 201911290437 A CN201911290437 A CN 201911290437A CN 110964527 A CN110964527 A CN 110964527A
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rare earth
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石峰
高嘉忆
刘苗
莫秀兰
武燕龙
王婷婷
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Shaanxi Normal University
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    • 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
    • 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
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Abstract

The invention discloses a controllable preparation method of a strong-luminescence rare earth up-conversion luminescent material, which is characterized in that two rare earth up-conversion luminescent materials with different sizes are mixed and heated at high temperature to prepare nano particles with uniform and stable sizes, and compared with the rare earth up-conversion luminescent material with the same size prepared by the traditional solvothermal method, the fluorescence intensity is enhanced. The invention solves the common problem of lower luminous efficiency of the up-conversion nano material, effectively enhances the luminous efficiency of the up-conversion material, provides a simple, feasible and controllable new method for preparing the high-efficiency luminous up-conversion material, simplifies the operation steps of improving the luminous efficiency of the up-conversion material by the traditional method, and is convenient for batch production of the up-conversion nano material with high-efficiency luminescence and uniform particle size.

Description

Method for controllably preparing strong-luminescence rare earth up-conversion material
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a preparation method of a fluorescence-enhanced rare earth up-conversion nano material.
Background
Upconversion luminescent materials can convert long-wavelength radiation into short-wavelength radiation and are generally composed of a host, an activator, a sensitizer. The fluorescent material has the advantages of large anti-Stokes displacement, long fluorescence service life, high light stability, strong chemical stability, high signal to noise ratio and the like, and has wide application in the fields of biomedical imaging, cancer diagnosis, illumination, photoelectric devices and the like. However, the sensitizer of the up-conversion luminescent material has a small absorption cross section, which results in low luminescent efficiency and affects the application of the up-conversion material. Therefore, how to increase the luminescence intensity of the upconversion material is the first problem to be solved by the material, various methods for increasing the luminescence intensity of the upconversion material are specifically introduced as follows:
1. metal ion doping
The method for doping metal ions into the up-conversion luminescent material is simple and feasible and can effectively improve the up-conversion luminescent efficiency. When metal ions are doped into lattice nodes or lattice gaps of the up-conversion material, the symmetry of a local crystal field of a luminescence center is reduced, so that phonon energy of lattice vibration is reduced, and the luminescence intensity is enhanced. A commonly used dopant ion is Mn2+、Fe3+、Ca2+And the like.
2. Construction of core-shell structures
The core-shell structure mainly comprises homogeneous shell layer coating and heterogeneous shell layer coating. The structure can reduce the surface defects and impurities of the up-conversion luminescent material and the energy loss caused by large specific surface area, thereby improving the luminous efficiency.
3. Metal surface plasmon resonance
The metal nano particles can form a strong electric field in a sub-wavelength area on the surface of the metal, so that the up-conversion exciting light at the plasma resonance frequency is greatly enhanced, the excited state service life can be shortened, the radiation attenuation rate is enhanced, and the luminous efficiency of the up-conversion material is finally improved.
4. Dye sensitization
The dye has a high extinction coefficient, can play a role of an antenna, effectively captures external excitation photons, transfers energy to sensitized ions through fluorescence resonance energy transfer, and further improves the up-conversion luminous efficiency, but the optimal doping structure design and the selection of the dye need further exploration.
The above method still has some unsolved problems in enhancing the upconversion luminous efficiency, such as: (1) how to accurately control the optimal doping concentration of various ions when rare earth doping ions are adjusted; (2) when a synergistic sensitizer is introduced to change the excitation wavelength and optimize upconversion luminescence, the problem of low luminous efficiency still needs to be solved; (3) the mechanism of plasmon resonance for fluorescence enhancement is not completely understood when plasmon resonance is used to enhance upconversion efficiency.
Disclosure of Invention
In view of this, the present invention provides a simple and effective method for increasing the luminescence intensity of the upconversion material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: uniformly dispersing the small-size and large-size rare earth up-conversion luminescent materials in cyclohexane or toluene according to the mass ratio of 1: 2-6, adding the materials into a mixed solution of oleic acid and octadecene according to the volume ratio of 1: 2-3, stirring at 70-80 ℃ under the protection of anhydrous and oxygen-free inert gas to remove the cyclohexane or toluene, stirring at 290-310 ℃ to react for 60-90 minutes, cooling the system to room temperature after the reaction is finished, and performing centrifugal washing with anhydrous ethanol to obtain the strong-luminescence rare earth up-conversion luminescent material.
In the method, the rare earth up-conversion luminescent material with small size and large size is preferably uniformly dispersed in cyclohexane or toluene according to the mass ratio of 1: 4-5.
The size of the small-size rare earth up-conversion luminescent material is 5-15 nm, and the size of the large-size rare earth up-conversion luminescent material is 20-35 nm.
The rare earth up-conversion luminescent material is NaREF4Yb and Ln, wherein RE and Ln are respectively independent and represent any one of Y, Yb, Ho, Er, Lu, Tm and Gd, and RE and Ln are different.
In the above method, the reaction is preferably stirred at 300 ℃ for 60 minutes.
The strong luminescent rare earth up-conversion material obtained by the method has a hexagonal phase structure.
In the above method, the inert gas is nitrogen or argon.
The invention has the following beneficial effects:
1. according to the invention, two up-conversion materials with different sizes are blended and heated, and due to an Ostwald curing mechanism, large grains can phagocytose small grains to grow into larger grains, so that the specific surface area of the nano particles is effectively reduced. Meanwhile, compared with an up-conversion luminescent material with the same size, the obtained material has longer fluorescence lifetime and stronger luminous intensity.
2. The preparation method is simple and easy to implement, has strong operability, simplifies the reaction steps of improving the up-conversion luminous efficiency by the traditional method, is convenient for batch production, and effectively obtains the up-conversion nano material with uniform size and high luminous intensity.
Drawings
FIG. 1 is a 10nm NaYF prepared in example 14Transmission electron micrographs of 18% Yb and 2% Er.
FIG. 2 is a 35nm NaYF prepared in example 14Transmission electron micrographs of 18% Yb and 2% Er.
FIG. 3 is a 37nm NaYF prepared in example 14Transmission electron micrographs of 18% Yb and 2% Er.
FIG. 4 is a 37nm NaYF prepared in comparative example 14Transmission electron micrographs of 18% Yb and 2% Er.
FIG. 5 shows NaYF prepared in example 1 and having dimensions of 10nm (a), 35nm (b), 37nm (c) and comparative example 1 and having dimensions of 37nm (d)4XRD patterns of 18% Yb and 2% Er.
FIG. 6 shows NaYF prepared in example 1 and having dimensions of 10nm (a), 35nm (b), 37nm (c) and comparative example 1 and having dimensions of 37nm (d)4Fluorescence spectrum diagram of 18% Yb and 2% Er under 980nm excitation.
FIG. 7 shows the dimensions 10nm (a), 35nm (b), 37nm (c) prepared in example 1 and the dimensions prepared in comparative example 137nm (d) NaYF4The fluorescence lifetime decay pattern of 18% Yb and 2% Er.
FIG. 8 is a 36nm NaYF prepared in example 24Transmission electron micrographs of 18% Yb and 2% Er.
FIG. 9 is a 36nm NaYF prepared in example 34Transmission electron micrographs of 18% Yb and 2% Er.
Detailed Description
The invention will be further described in detail with reference to the following figures and examples, but the scope of the invention is not limited to these examples.
Example 1
0.2428g (0.80mmol) YCl3·6H2O、0.0698g(0.18mmol)YbCl3·6H2O、0.0076g(0.02mmol)ErCl3·6H2O, 6mL of oleic acid and 15mL of octadecene are added into a 100mL three-neck flask, and stirred for 1h at 160 ℃ under the protection of anhydrous, oxygen-free and inert gases to form a uniform transparent solution which is slightly yellowish. The system was then cooled to room temperature and 0.1g (2.5mmol) NaOH and 0.1482g (4mmol) NH dissolved were added4Stirring 10mL of methanol solution of F at normal temperature for 60min, heating to 55-60 ℃, continuously stirring for 60min to remove methanol, heating to 110-120 ℃, vacuumizing for 20min, heating to 300 ℃ at the speed of 38 ℃/min, keeping the temperature for 60min, cooling to room temperature after the reaction is finished, and centrifugally washing with absolute ethyl alcohol to obtain a rare earth up-conversion luminescent material NaYF with the size of 10nm418% Yb and 2% Er (see FIG. 1).
0.2428g (0.80mmol) YCl3·6H2O、0.0698g(0.18mmol)YbCl3·6H2O、0.0076g(0.02mmol)ErCl3·6H2O, 6mL of oleic acid and 15mL of octadecene are added into a 100mL three-neck flask, and stirred for 1h at 160 ℃ under the protection of anhydrous, oxygen-free and inert gases to form a uniform transparent solution which is slightly yellowish. The system was then cooled to room temperature and 0.1g (2.5mmol) NaOH and 0.1482g (4mmol) NH dissolved were added4Stirring 10mL of methanol solution of F at normal temperature for 60min, heating to 55-60 ℃, continuously stirring for 60min to remove methanol, heating to 110-120 ℃, vacuumizing for 10min, heating to 300 ℃ at the speed of 19 ℃/min, keeping the temperature for 60min, and cooling to the temperature of 300 ℃ after the reaction is finishedCentrifugally washing the mixture at room temperature by using absolute ethyl alcohol to obtain the rare earth up-conversion luminescent material NaYF with the size of 35nm418% Yb and 2% Er (see FIG. 2).
20mg of NaYF with a size of 10nm418% Yb, 2% Er and 100mg NaYF with a size of 35nm4Uniformly dispersing 18% Yb and 2% Er in 3mL cyclohexane, adding the obtained dispersion into a mixed solution of 6mL oleic acid and 15mL octadecene, stirring at 80 ℃ for 5-10 min under the protection of anhydrous oxygen-free argon gas to remove cyclohexane, heating to 300 ℃, stirring at constant temperature for reaction for 60min, cooling the system to room temperature after the reaction is finished, and centrifugally washing with anhydrous ethanol to obtain a rare earth up-conversion material NaYF with the size of 37nm418% Yb and 2% Er (see FIG. 3).
Comparative example 1
0.2428g (0.80mmol) YCl3·6H2O、0.0698g(0.18mmol)YbCl3·6H2O、0.0076g(0.02mmol)ErCl3·6H2O, 6mL of oleic acid and 15mL of octadecene are added into a 100mL three-neck flask, and stirred for 1h at 160 ℃ under the protection of anhydrous, oxygen-free and inert gases to form a uniform transparent solution which is slightly yellowish. The system was then cooled to room temperature and 0.1g (2.5mmol) NaOH and 0.1482g (4mmol) NH dissolved were added4Stirring 10mL of methanol solution of F at normal temperature for 60min, heating to 55-60 ℃, continuously stirring for 60min to remove methanol, heating to 110-120 ℃, vacuumizing for 10min, heating to 300 ℃ at the speed of 15 ℃/min, keeping the temperature for 75min, cooling to room temperature after the reaction is finished, and centrifugally washing with absolute ethyl alcohol to obtain a rare earth up-conversion luminescent material NaYF with the size of 37nm418% Yb, 2% Er (see FIG. 4).
As can be seen from comparison of the above-mentioned figures 1 to 3, the obtained material is spherical nanocrystal with uniform size distribution. And when the small-size and large-size upconversion nanoparticles react, the large grains can 'phagocytose' the small grains to form the spherical upconversion nanoparticles with new sizes.
The samples with the sizes of 10nm, 35nm and 37nm prepared in the example 1 and the sample with the size of 37nm prepared in the comparative example 1 are characterized by an X-ray diffractometer and a transient/steady state fluorescence spectrometer, and the results are shown in the figures 5-7.
As can be seen from fig. 5, the obtained samples all have good crystallinity, which is pure hexagonal phase NaYF in comparison with standard cards4And (3) the material has no diffraction peak of other impurities. As can be seen in FIG. 6, two different sizes of NaYF were used4After reaction of 18% Yb and 2% Er, the fluorescence intensity of the obtained sample (c) under 980nm excitation is obviously stronger than that of the two adopted raw materials (a and b) with different sizes and that of the sample (d) with the same size prepared by the traditional method in the comparative example 1, which shows that the method can effectively improve the luminous intensity of the up-conversion material. As can be seen in FIG. 7, two different sizes of NaYF were used4After the reaction of 18% Yb and 2% Er, the fluorescence lifetime of the obtained sample is also obviously superior to that of the two adopted raw materials with different sizes and the sample with the same size prepared by the traditional method in the comparative example 1, and the method provided by the invention can be further used for effectively improving the luminous intensity of the up-conversion material.
Example 2
In this example, 20mg of NaYF with a size of 10nm was added418% Yb, 2% Er and 40mg NaYF with a size of 35nm418% Yb and 2% Er were uniformly dispersed in 3mL cyclohexane, and the other steps were the same as in example 1 to obtain a rare earth up-conversion material NaYF having a size of 36nm418% Yb, 2% Er (see FIG. 8).
Example 3
In this example, 20mg of NaYF with a size of 10nm was added418% Yb, 2% Er and 80mg NaYF with a size of 35nm418% Yb and 2% Er were uniformly dispersed in 3mL cyclohexane, and the other steps were the same as in example 1 to obtain a rare earth up-conversion material NaYF having a size of 36nm418% Yb and 2% Er (see FIG. 9).
In the above embodiment, two different sizes of rare earth upconversion luminescent materials NaYF418% Yb, 2% Er also with NaGdF of different sizes4:18％Yb,2％Er、NaLuF4:18％Yb,2％Er、NaYbF4:18％Yb,2％Er、NaLuF418% Yb, 2% Tm and the like, and then the two raw materials with different sizes are reacted by the method of the invention, so that the rare earth up-conversion luminescent material with obviously enhanced luminescence can be obtained.

Claims (7)

1. A method for controllably preparing a strong luminous rare earth up-conversion material is characterized by comprising the following steps: uniformly dispersing the small-size and large-size rare earth up-conversion luminescent materials in cyclohexane or toluene according to the mass ratio of 1: 2-6, adding the materials into a mixed solution of oleic acid and octadecene according to the volume ratio of 1: 2-3, stirring at 70-80 ℃ under the protection of anhydrous and oxygen-free inert gas to remove the cyclohexane or toluene, stirring at 290-310 ℃ to react for 60-90 minutes, cooling the system to room temperature after the reaction is finished, and performing centrifugal washing with anhydrous ethanol to obtain the strong-luminescence rare earth up-conversion luminescent material.
2. The method for controllably preparing a strong luminescent rare earth up-conversion material according to claim 1, wherein: uniformly dispersing the small-size and large-size rare earth up-conversion luminescent materials in cyclohexane or toluene according to the mass ratio of 1: 4-5.
3. The method for controllable preparation of a strong luminescent rare earth up-conversion material according to claim 1 or 2, characterized in that: the size of the small-size rare earth up-conversion luminescent material is 5-15 nm, and the size of the large-size rare earth up-conversion luminescent material is 20-35 nm.
4. The method for controllable preparation of a strong luminescent rare earth up-conversion material according to claim 1 or 2, characterized in that: the rare earth up-conversion luminescent material is NaREF4Yb and Ln, wherein RE and Ln are respectively independent and represent any one of Y, Yb, Ho, Er, Lu, Tm and Gd, and RE and Ln are different.
5. The method for controllably preparing a strong luminescent rare earth up-conversion material according to claim 1, wherein: the reaction was stirred at 300 ℃ for 60 minutes.
6. The method for controllably preparing a strong luminescent rare earth up-conversion material according to claim 1, wherein: the strong luminous rare earth up-conversion material is in a hexagonal phase structure.
7. The method for controllably preparing a strong luminescent rare earth up-conversion material according to claim 1, wherein: the inert gas is nitrogen or argon.
CN201911290437.2A 2019-12-16 2019-12-16 Method for controllably preparing strong-luminescence rare earth up-conversion material Pending CN110964527A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112625685A (en) * 2020-12-11 2021-04-09 湖北文理学院 Spherical hexagonal NaYF4Upconverting material and method for the production thereof
CN114203745A (en) * 2022-02-18 2022-03-18 广州粤芯半导体技术有限公司 Near-infrared image sensor structure and manufacturing method thereof
CN116023944A (en) * 2021-10-26 2023-04-28 中国科学院福建物质结构研究所 H (H) + Ion doped luminescent-enhanced rare earth inorganic nano luminescent material, and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN1935938A (en) * 2006-09-20 2007-03-28 东华大学 Method for preparing up-conversion fluorescent matrix material NaYF4 nano crystal
WO2014116631A1 (en) * 2013-01-22 2014-07-31 University Of Massachusetts Medical School Compositions and methods for upconverting luminescence with engineered excitation and applications thereof
CN104403672A (en) * 2014-12-10 2015-03-11 中国科学院长春光学精密机械与物理研究所 Up-conversion luminescent material as well as preparation method and application thereof
CN107815302A (en) * 2016-09-14 2018-03-20 首都师范大学 A kind of rare earth up-conversion luminescence nanomaterial of controlledly synthesis core shell structure and preparation method and application

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1935938A (en) * 2006-09-20 2007-03-28 东华大学 Method for preparing up-conversion fluorescent matrix material NaYF4 nano crystal
WO2014116631A1 (en) * 2013-01-22 2014-07-31 University Of Massachusetts Medical School Compositions and methods for upconverting luminescence with engineered excitation and applications thereof
CN104403672A (en) * 2014-12-10 2015-03-11 中国科学院长春光学精密机械与物理研究所 Up-conversion luminescent material as well as preparation method and application thereof
CN107815302A (en) * 2016-09-14 2018-03-20 首都师范大学 A kind of rare earth up-conversion luminescence nanomaterial of controlledly synthesis core shell structure and preparation method and application

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112625685A (en) * 2020-12-11 2021-04-09 湖北文理学院 Spherical hexagonal NaYF4Upconverting material and method for the production thereof
CN112625685B (en) * 2020-12-11 2022-08-30 湖北文理学院 Spherical hexagonal NaYF 4 Upconverting material and method for the production thereof
CN116023944A (en) * 2021-10-26 2023-04-28 中国科学院福建物质结构研究所 H (H) + Ion doped luminescent-enhanced rare earth inorganic nano luminescent material, and preparation method and application thereof
CN114203745A (en) * 2022-02-18 2022-03-18 广州粤芯半导体技术有限公司 Near-infrared image sensor structure and manufacturing method thereof

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Application publication date: 20200407