CN108998029B - Water-soluble NaYF4:Yb3+,Er3+@NaGdF4Method for producing crystalline particles - Google Patents

Water-soluble NaYF4:Yb3+,Er3+@NaGdF4Method for producing crystalline particles Download PDF

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CN108998029B
CN108998029B CN201810696918.2A CN201810696918A CN108998029B CN 108998029 B CN108998029 B CN 108998029B CN 201810696918 A CN201810696918 A CN 201810696918A CN 108998029 B CN108998029 B CN 108998029B
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nagdf
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CN108998029A (en
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张正龙
孟佳佳
李贵安
张宝宝
弥小虎
付正坤
郑海荣
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Shaanxi Normal University
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Abstract

The invention discloses a water-soluble NaYF4:Yb3+,Er3+@NaGdF4The preparation method of crystal particles utilizes a hydrothermal method, takes sodium fluoride as a fluorine source and trisodium citrate as a surfactant, and generates NaGdF by changing4The molar quantity of the shell layer precursor controls the shell layer thickness, and the prepared NaYF4:Yb3+,Er3+@NaGdF4The crystallinity of crystal particles is high, the shapes are uniform and are hexagonal disc-shaped, and the fluorescence emission efficiency is high. Compared with the existing high-temperature thermal decomposition method and solvothermal method, the preparation method is simple, convenient, easy to operate and controllable, the surfaces of the prepared crystal particles do not need to be further modified, and the crystal particles have good biocompatibility and can be directly applied to in vivo experimental research.

Description

Water-soluble NaYF4:Yb3+,Er3+@NaGdF4Method for producing crystalline particles
Technical Field
The invention relates to a method for directly preparing NaYF with water solubility, paramagnetism and up-conversion fluorescence integrated4:Yb3+,Er3+@NaGdF4A method of crystallizing particles.
Background
The rare earth doped up-conversion luminescent material has the advantages of long fluorescence life, weak background fluorescence, high crystallinity, low toxicity and the like, and is widely applied to the fields of illumination display systems, optical agriculture, solar cell spectrum conversion materials, biological photodynamic therapy, magnetic resonance imaging and the like. Because of lower phonon energy and good chemical stability, NaYF4Generally used as a matrix material, but the rare earth-doped up-conversion materials primarily prepared by thermal decomposition and solvothermal methods are not water-soluble, and need to be surface-modified before practical use, and in addition, the rare earth-doped up-conversion materials are applied to the field of biologyAnother problem faced is its low quantum yield. The method for modifying the surface of the rare earth doped material generally comprises a method for coating a medium pore material SiO2Organic ligand modification (PEI, PEG, phospholipid molecules and the like) and an ion exchange method, and the whole process of synthesizing water-soluble and low-toxicity sample particles is complex. Therefore, it is very important to improve the fluorescence emission efficiency of the rare earth doped up-conversion material and simultaneously meet the water solubility of the material.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a NaYF which is simple and easy to operate, has mild reaction conditions and integrates water solubility, paramagnetism and up-conversion fluorescence into a whole and is directly synthesized4:Yb3+,Er3+@NaGdF4A method of hexagonal phase crystalline particles.
The technical scheme adopted for solving the technical problems comprises the following steps:
1. dissolving trisodium citrate in deionized water, and sequentially adding 0.5mol/L Y (NO)3)3Aqueous solution, 0.5mol/L Yb (NO)3)3Aqueous solution and 0.5mol/L Er (NO)3)3Stirring the aqueous solution at room temperature for 25-30 minutes, sequentially adding sodium nitrate and sodium fluoride, continuously stirring for 20-30 minutes, transferring the obtained transparent solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting at 170-190 ℃ for 18-20 hours, naturally cooling to room temperature, centrifuging, washing and drying to obtain hexagonal-phase NaYF4:Yb3+,Er3+Crystal particles.
2. Mixing hexagonal phase NaYF4:Yb3+,Er3+Dispersing the crystal particles in deionized water, and sequentially adding trisodium citrate and 0.5mol/L Gd (NO)3)3Stirring the aqueous solution at room temperature for 20-35 minutes, sequentially adding sodium nitrate and sodium fluoride, continuously stirring for 20-35 minutes, transferring the obtained mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting at 170-190 ℃ for 18-20 hours, naturally cooling to room temperature, centrifuging, washing and drying to obtain hexagonal-phase NaYF4:Yb3+,Er3+@NaGdF4Core shell crystal particles.
The steps are as followsIn step 1, Er (NO) is preferred3)3、Yb(NO3)3、Y(NO3)3The molar ratio of the trisodium citrate to the sodium fluoride to the sodium nitrate is 1: 9-11: 38-41: 39-45: 55-70: 300-450.
In the step 1, it is further preferable that the obtained transparent solution is transferred to a polytetrafluoroethylene-lined autoclave and reacted at 180 ℃ for 20 hours.
In the above step 2, Gd (NO) is preferable3)3The molar ratio of the trisodium citrate to the sodium fluoride to the sodium nitrate is 1: 1-2: 1-3: 9-12.
In the step 2, it is further preferable that the obtained mixed solution is transferred to a polytetrafluoroethylene-lined autoclave and reacted at 180 ℃ for 20 hours.
The invention utilizes a hydrothermal method to prepare NaYF4:Yb3+,Er3+@NaGdF4The preparation method of the crystal particles is simple and easy to operate, the reaction conditions are mild, the shell thickness is uniform and controllable, the core-shell crystal yield is high, and the obtained NaYF4:Yb3+,Er3+@NaGdF4The crystal particles have uniform appearance, good crystallinity, stable luminescence and better biocompatibility, and the fluorescence emission intensity of the core-shell structure crystal can be enhanced by regulating the thickness of the shell layer by changing the molar quantity of the shell layer precursor.
Drawings
FIG. 1 is a NaYF prepared in example 14:Yb3+,Er3+SEM image of crystal particles.
FIG. 2 is a NaYF prepared in example 14:Yb3+,Er3+@NaGdF4SEM image of crystal particles.
FIG. 3 is a NaYF prepared in example 24:Yb3+,Er3+@NaGdF4SEM image of crystal particles.
FIG. 4 is a NaYF prepared in example 34:Yb3+,Er3+@NaGdF4SEM image of crystal particles.
FIG. 5 is a NaYF prepared in example 44:Yb3+,Er3+@NaGdF4Crystal particleSEM image of the pellet.
FIG. 6 is a NaYF prepared in example 54:Yb3+,Er3+@NaGdF4SEM image of crystal particles.
FIG. 7 is a NaYF prepared in example 54:Yb3+,Er3+@NaGdF4Pictures of the solution after dispersing the crystal particles into serum, phosphate buffer, cell culture fluid and water for 0.5 h.
FIG. 8 is a NaYF prepared in example 44:Yb3+,Er3+@NaGdF4Samples of crystalline particles dispersed in water with Gd3+Concentration and T1Weighted MR image relaxation Rate (1/T)1) A graph of the relationship (c).
FIG. 9 shows NaYF prepared in examples 1-54:Yb3+,Er3+@NaGdF4Fluorescence emission spectrum of single crystal particle under 980nm excitation.
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
1. 1.264g (4.3mmol) trisodium citrate was dispersed in 32mL deionized water, followed by the sequential addition of 0.59mL0.5mol/L Y (NO)3)3Aqueous solution, 0.15mL of 0.5mol/L Yb (NO)3)3Aqueous solution, 0.015mL of 0.5mol/L Er (NO)3)3Stirring the aqueous solution at room temperature for 25 minutes, then adding 3.214g (37.8mmol) of sodium nitrate and 0.274g (6.5mmol) of sodium fluoride in sequence, and continuing to stir for 30 minutes to completely dissolve the sodium nitrate and the sodium fluoride; transferring the obtained transparent solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting at 180 ℃ for 20 hours, naturally cooling to room temperature, centrifuging, washing with deionized water, and drying at 50 ℃ for 10 hours to obtain hexagonal phase NaYF with the thickness of 0.47 mu m4:Yb3+,Er3+Submicron crystalline particles (see FIG. 1).
2. Weighing 20mg of NaYF prepared in the step 14:Yb3+,Er3+Adding the submicron crystal particles into 22mL deionized water, ultrasonically dispersing uniformly, and then sequentially adding0.252g (0.86mmol) trisodium citrate, 0.12mL 0.5mol/L Gd (NO)3)3Stirring the aqueous solution at room temperature for 30 minutes, then adding 0.648g (7.6mmol) of sodium nitrate and 0.055g (1.3mmol) of sodium fluoride in sequence, and continuing to stir for 25 minutes to completely dissolve the sodium nitrate and the sodium fluoride; then transferring the obtained mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 20 hours at 180 ℃, naturally cooling to room temperature, centrifuging, washing with deionized water, and drying for 10 hours at 50 ℃ to obtain the hexagonal disc type NaYF with the thickness of 0.50 mu m4:Yb3+,Er3+@NaGdF4Hexagonal phase submicron crystalline particles (see FIG. 2), noted NaGdF4(0.20)。
Example 2
In this example, hexagonal phase NaYF4:Yb3+,Er3+The submicron crystal particles were prepared in the same manner as in step 1 of example 1. In step 2 of this example, 20mg of NaYF prepared in step 1 was weighed4:Yb3+,Er3+Adding the submicron crystal particles into 22mL deionized water, uniformly dispersing by ultrasonic, and then sequentially adding 0.32g (1.08mmol) of trisodium citrate and 0.15mL of 0.5mol/L Gd (NO)3)3Stirring the aqueous solution at room temperature for 30 minutes, then adding 0.81g (9.5mmol) of sodium nitrate and 0.07g (1.63mmol) of sodium fluoride in sequence, and continuing to stir for 25 minutes to completely dissolve the sodium nitrate and the sodium fluoride; then transferring the obtained mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 20 hours at 180 ℃, naturally cooling to room temperature, centrifuging, washing with deionized water, and drying for 10 hours at 50 ℃ to obtain hexagonal disc type NaYF with the thickness of 0.54 mu m4:Yb3+,Er3+@NaGdF4Hexagonal phase submicron crystalline particles (see figure 3).
Example 3
In this example, hexagonal phase NaYF4:Yb3+,Er3+The submicron crystal particles were prepared in the same manner as in step 1 of example 1. In step 2 of this example, 20mg of NaYF prepared in step 1 was weighed4:Yb3+,Er3+Adding submicron crystal particles into 22mL deionized water, uniformly dispersing by ultrasonic, and then sequentially adding 0.421g (1.44mmol) of trisodium citrate,0.20mL 0.5mol/L Gd(NO3)3stirring the aqueous solution at room temperature for 30 minutes, then adding 1.09g (12.67mmol) of sodium nitrate and 0.10g (2.18mmol) of sodium fluoride in sequence, and continuing to stir for 25 minutes to completely dissolve the sodium nitrate and the sodium fluoride; then transferring the obtained mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 20 hours at 180 ℃, naturally cooling to room temperature, centrifuging, washing with deionized water, and drying for 10 hours at 50 ℃ to obtain hexagonal disc-shaped NaYF with the thickness of 0.60 mu m4:Yb3+,Er3+@NaGdF4Hexagonal phase submicron crystalline particles (see figure 4).
Example 4
In this example, hexagonal phase NaYF4:Yb3+,Er3+The submicron crystal particles were prepared in the same manner as in step 1 of example 1. In step 2 of this example, 20mg of NaYF prepared in step 1 was weighed4:Yb3+,Er3+Adding the submicron crystal particles into 22mL deionized water, uniformly dispersing by ultrasonic, and then sequentially adding 0.64g (2.16mmol) of trisodium citrate and 0.30mL of 0.5mol/L Gd (NO)3)3Stirring the aqueous solution at room temperature for 30 minutes, then adding 1.65g (19.41mmol) of sodium nitrate and 0.14g (3.27mmol) of sodium fluoride in sequence, and continuing to stir for 25 minutes to completely dissolve the sodium nitrate and the sodium fluoride; then transferring the obtained mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 20 hours at 180 ℃, naturally cooling to room temperature, centrifuging, washing with deionized water, and drying for 10 hours at 50 ℃ to obtain hexagonal disc-shaped NaYF with the thickness of 0.61 mu m4:Yb3+,Er3+@NaGdF4Hexagonal phase submicron crystalline particles (see figure 5).
Example 5
In this example, hexagonal phase NaYF4:Yb3+,Er3+The submicron crystal particles were prepared in the same manner as in step 1 of example 1. In step 2 of this example, 20mg of NaYF prepared in step 1 was weighed4:Yb3+,Er3+Adding the submicron crystal particles into 22mL deionized water, uniformly dispersing by ultrasonic, and then sequentially adding 1.267g (4.32mmol) of trisodium citrate and 0.60mL of 0.5mol/L Gd (NO)3)3Aqueous solution, chamberStirring for 30 minutes at room temperature, then adding 3.214g (37.80mmol) of sodium nitrate and 0.27g (6.54mmol) of sodium fluoride in sequence, and continuing to stir for 25 minutes to completely dissolve the sodium nitrate and the sodium fluoride; then transferring the obtained mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 20 hours at 180 ℃, naturally cooling to room temperature, centrifuging, washing with deionized water, and drying for 10 hours at 50 ℃ to obtain the hexagonal disc type NaYF with the thickness of 0.62 mu m4:Yb3+,Er3+@NaGdF4Hexagonal phase submicron crystalline particles (see figure 6).
To prove the NaYF prepared by the method of the invention4:Yb3+,Er3+@NaGdF4The crystal particles have good biocompatibility, and the inventors dispersed the crystal particles prepared in example 5 into serum, a cell culture solution, a phosphate buffer solution, and water, respectively. After half an hour, NaYF can be found4:Yb3+,Er3+@NaGdF4The crystal particles are still uniformly dispersed in serum, cell buffer solution and phosphate cell culture solution (see figure 7), which proves that the prepared rare earth particles have better biological stability and compatibility in the cell-like growth environment.
To prove that the NaYF prepared by the invention4:Yb3+,Er3+@NaGdF4The crystal particles have paramagnetism, and the inventors have prepared NaYF in example 44:Yb3+,Er3+@NaGdF4The crystal particles are subjected to in vitro T1Weighted MR imaging test with water as a blank and a magnetic field of 0.5T. As can be seen in FIG. 8, NaYF was dispersed in water4:Yb3+,Er3+@NaGdF4Sample Gd3+Increase in concentration, T1The higher the brightness of the weighted MR image, i.e. T1The smaller the value. For Gd3+Linear fit between concentration and reciprocal of longitudinal relaxation time with a slope of 3.81mM-1S-1. The experimental phenomena and results show that the synthesized NaYF4:Yb3+,Er3+@NaGdF4The sample has potential application in medical magnetic resonance imaging technology.
To prove that the NaYF prepared by the invention4:Yb3+,Er3+@NaGdF4The crystal particles have excellent up-conversion fluorescence emission, and the inventor provides NaYF prepared in examples 1-54:Yb3+,Er3+@NaGdF4Single-particle in situ fluorescence emission spectroscopy measurement of single crystal particles was performed, and the results are shown in FIG. 9. As can be seen in FIG. 9, NaYF4:Yb3+,Er3+Coated inert NaGdF4Compared with a naked core, the fluorescence emission intensity of the shell is obviously enhanced.

Claims (3)

1. Water-soluble NaYF4:Yb3+,Er3+@NaGdF4A process for the preparation of crystalline particles, characterized in that it consists of the following steps:
(1) dissolving trisodium citrate in deionized water, and sequentially adding 0.5mol/L Y (NO)3)3Aqueous solution, 0.5mol/L Yb (NO)3)3Aqueous solution and 0.5mol/L Er (NO)3)3Stirring the aqueous solution at room temperature for 25-30 minutes, sequentially adding sodium nitrate and sodium fluoride, continuously stirring for 20-30 minutes, transferring the obtained transparent solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting at 170-190 ℃ for 18-20 hours, naturally cooling to room temperature, centrifuging, washing and drying to obtain hexagonal-phase NaYF4:Yb3 +,Er3+Crystal particles; wherein, said Er (NO)3)3、Yb(NO3)3、Y(NO3)3The molar ratio of the trisodium citrate to the sodium fluoride to the sodium nitrate is 1: 9-11: 38-41: 39-45: 55-70: 300-450;
(2) mixing hexagonal phase NaYF4:Yb3+,Er3+Dispersing the crystal particles in deionized water, and sequentially adding trisodium citrate and 0.5mol/L Gd (NO)3)3Stirring the aqueous solution at room temperature for 20-35 minutes, sequentially adding sodium nitrate and sodium fluoride, continuously stirring for 20-35 minutes, transferring the obtained mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting at 170-190 ℃ for 18-20 hours, naturally cooling to room temperature, centrifuging, washing and drying to obtain hexagonal-phase NaYF4:Yb3+,Er3+@NaGdF4Core-shell crystal particles; the Gd (NO)3)3The molar ratio of the trisodium citrate to the sodium fluoride to the sodium nitrate is 1: 1-2: 1-3: 9-12.
2. The water-soluble NaYF of claim 14:Yb3+,Er3+@NaGdF4A method for producing crystal particles, characterized by: in the step (1), the obtained transparent solution is transferred into a high-pressure reaction kettle with a polytetrafluoroethylene lining and reacts for 20 hours at 180 ℃.
3. The water-soluble NaYF of claim 14:Yb3+,Er3+@NaGdF4A method for producing crystal particles, characterized by: in the step (2), the obtained mixed solution is transferred into a high-pressure reaction kettle with a polytetrafluoroethylene lining and reacts for 20 hours at 180 ℃.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105838374A (en) * 2016-04-25 2016-08-10 陕西师范大学 Ytterbium/thulium-ion-codoped hexagonal-phase sodium yttrium fluoride microcrystal with red-light oriented emission performance
CN105838373A (en) * 2016-04-25 2016-08-10 陕西师范大学 Beta-NaYF4:Yb<3+>/Er<3+> micron crystal with red light directional emission performance

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105838374A (en) * 2016-04-25 2016-08-10 陕西师范大学 Ytterbium/thulium-ion-codoped hexagonal-phase sodium yttrium fluoride microcrystal with red-light oriented emission performance
CN105838373A (en) * 2016-04-25 2016-08-10 陕西师范大学 Beta-NaYF4:Yb<3+>/Er<3+> micron crystal with red light directional emission performance

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"Water-Soluble NaYF4:Yb,Er(Tm)/NaYF4/Polymer Core/Shell/Shell Nanoparticles with Significant Enhancement of Upconversion Fluorescence;Guang-Shun Yi et al.;《Chem. Mater.》;20061230;第19卷;第341-343页 *

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