CN111809273A - Preparation method of rare earth ion doped yttrium vanadate nanotube and nanotube - Google Patents
Preparation method of rare earth ion doped yttrium vanadate nanotube and nanotube Download PDFInfo
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- CN111809273A CN111809273A CN202010701074.3A CN202010701074A CN111809273A CN 111809273 A CN111809273 A CN 111809273A CN 202010701074 A CN202010701074 A CN 202010701074A CN 111809273 A CN111809273 A CN 111809273A
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- D01D5/0007—Electro-spinning
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- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
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- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
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- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
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Abstract
The invention discloses a preparation method of a rare earth ion doped yttrium vanadate nanotube and the nanotube, comprising the following steps: s1, mixing polyvinylpyrrolidone with an ethanol water solution to obtain a mixed solution, adding Y after the mixed solution is clarified3+、NH4VO3And doping ions, and stirring for reaction to obtain sol; s2, controlling the spinning voltage to be 15-18kV, controlling the spinning receiving distance to be 15-25cm, and keeping the air humidity to be 30-50% to carry out electrostatic spinning to obtain precursor nanofiber; s3, drying the precursor nano-fiber in a vacuum environment at 80-120 ℃ for 3h, heating to 700-Doped YVO4A nanotube. The method can obtain YVO by adjusting the process parameters, the solution parameters and the heating rate of electrostatic spinning and doping rare earth ions or modifying the surface function4The nanotube has both drug-loading and photothermal therapy properties.
Description
Technical Field
The invention relates to the field of nano material preparation, in particular to a preparation method of a rare earth ion doped yttrium vanadate nanotube and the nanotube.
Background
YVO chemical formula of yttrium vanadate4It is tetragonal system, and has large refractive index value and poor birefringence. Yttrium vanadate having 3.3GW/cm2And has excellent optical transparency in an extremely wide spectral range. If a certain concentration of rare earth ions are doped into yttrium vanadate crystals, the rare earth ions will react with Y3+The substitution position, the yttrium vanadate doped with rare earth ions has important application in the fields of optical fiber communication, fluorescence and laser.
After the yttrium vanadate material is subjected to nanocrystallization, the performance of the yttrium vanadate material is greatly changed, for example, the resolution of a display device can be improved, and the activity of the yttrium vanadate material as a photocatalyst can be improved; its application field will be expanded too, such as can apply to fingerprint recognition, biomedicine field. As is known, the micro size and micro shape of the material have important influence on the performance of the material and the application range of the material, so that YVO with special shape and special size4Controlled synthesis of materials, for YVO4The application of the material has great significance. So far, researchers have employed sol-gel techniques, hydrothermal techniques, combustion methods, coprecipitation methods, sonochemical methods, dialysis methods, electrostatic spinning methods, and the likePreparing YVO with different nanometer sizes (several nanometers to several hundred nanometers in size) and different nanometer structure shapes (such as nanometer particles, nanometer rods, nanometer fibers and porous membranes)4And (3) nano materials. Although one-dimensional YVO can be obtained by an electrostatic spinning method and a hydrothermal method4Nanometer materials, but most of the obtained nanometer yttrium vanadate materials are linear and rod-shaped materials, and are not suitable for application in the field of drug delivery.
Disclosure of Invention
Aiming at the problems, the invention researches and designs a preparation method of a rare earth ion doped yttrium vanadate nanotube and the nanotube so as to solve the problem that most of linear and rod-shaped YVO prepared by the traditional method4Nano materials are not suitable for the application in the field of drug delivery. The technical means adopted by the invention are as follows:
a preparation method of rare earth ion doped yttrium vanadate nanotubes comprises the following steps:
s1, mixing polyvinylpyrrolidone with an ethanol water solution to obtain a mixed solution, adding Y after the mixed solution is clarified3+、NH4VO3And doping ions, and stirring for reaction to obtain sol;
s2, controlling the spinning voltage to be 15-18kV, controlling the spinning receiving distance to be 15-25cm, and keeping the air humidity to be 30-50% to carry out electrostatic spinning to obtain precursor nanofiber;
s3, drying the precursor nano-fiber in a vacuum environment at 80-120 ℃ for 3-6h, heating to 700-4A nanotube.
Preferably, in step S1, the mass fraction of polyvinylpyrrolidone in the mixed solution is 10-30 wt.%.
Preferably, in step S1, the mass fraction of ethanol in the aqueous solution of ethanol is 40-60 wt.%.
Preferably, the dopant ion may be Ce3+、Tb3+、Yb3+、Er3+、Tm3+And Ho3+Of (5) or of Ce3+/Tb3+、Yb3+/Er3+、Yb3+/Tm3+And Yb3+/Ho3+Double ion doping, etc.
Preferably, in step S1, the doping ion is Yb3+And Er3+，Y3+And NH4VO3、Yb3+And Er3+Are respectively Y3+:NH4VO3＝1.0:1.02、Y3+:Yb3+＝100.0:(1-30)、Y3+:Er3+＝100.0:1.0。
Preferably, in step S1, Y3+Yb is derived from one or two of yttrium nitrate and yttrium acetate3+Er is derived from one or two of ytterbium nitrate and ytterbium acetate3+Derived from one or the combination of erbium nitrate and erbium acetate.
A rare earth ion doped yttrium vanadate nanotube prepared by any one of the methods.
Compared with the prior art, the preparation method of the rare earth ion doped yttrium vanadate nanotube and the nanotube have the beneficial effects that: the yttrium vanadate nanotube is prepared by combining the traditional electrostatic spinning technology with a high-temperature annealing process. By adjusting the process parameters and solution parameters of electrostatic spinning and the heating rate, one-dimensional YVO with a polycrystalline structure and an outer diameter of 40-200nm can be obtained4Nanotubes, which may be 50-1000nm in length, or even longer. The YVO4The wall thickness of the nanotubes can be adjusted between 5-20nm by experimental parameters. By subjecting the YVO to4The nanotube is doped with rare earth ions or modified on the surface, so that the nanotube has the functions of drug loading and photothermal therapy.
Drawings
FIG. 1 shows YVO obtained in example 2 of the present invention4:Er3+/Yb3+SEM image of nanotube;
FIG. 2 shows a single YVO obtained in example 2 of the present invention4:Er3+/Yb3+SEM image of nanotube;
FIG. 3 shows YVO obtained in example 2 of the present invention4:Er3+/Yb3+TEM image of nanotubes;
FIG. 4 shows YVO obtained in examples 1 to 4 of the present invention4:Er3+/Yb3+XRD spectrogram of the nanotube;
FIG. 5 shows YVO obtained in examples 1 to 4 of the present invention4:Er3+/Yb3+The up-conversion emission spectrum of the nanotube under the excitation of 980nm laser.
In FIG. 4, (a) 1% molEr/5% molYb corresponds to example 1; (b) 1% molEr/10% molYb corresponds to example 2; (c) 1% molEr/20% molYb corresponds to example 3; (d) 1% mol Er/30% mol Yb corresponds to example 4.
Detailed Description
Example 1:
5.0g of polyvinylpyrrolidone was dissolved in 50ml of a mixed solution of water and ethanol (water: ethanol 1:1, mass ratio) until it was clear. Adding a certain amount of Y (NO) into the solution3)3、NH4VO3、Yb(CH3COO)3、Er(NO3)3. Wherein Y (NO)3)3:NH4VO31.0:1.02, stoichiometric ratio; y (NO)3)3:Er(NO3)3100.0:1.0, stoichiometric ratio; y (NO)3)3:Yb(CH3COO)3100.0:5.0, stoichiometric ratio. And (3) continuously stirring by using a magnetic stirrer to finally obtain uniform and stable sol. Controlling the spinning voltage to be 15kV, the spinning receiving distance to be 20cm, keeping the air humidity to be 40% +/-10%, performing electrostatic spinning to obtain precursor nanofibers, and drying in a vacuum oven at 80 ℃ for 3 h. Calcining the dried precursor composite nanofiber at the temperature rising rate of 2 ℃/min to 800 ℃, calcining at 800 ℃ for 4h, and naturally cooling to obtain the final YVO4:Er3+/Yb3+A nanotube sample.
Example 2:
5.0g of polyvinylpyrrolidone was dissolved in 50ml of a mixed solution of water and ethanol (water: ethanol 1:1, mass ratio) until it was clear. Adding a certain amount of Y (NO) into the solution3)3、NH4VO3、Yb(CH3COO)3、Er(NO3)3. Wherein Y (NO)3)3:NH4VO31.0:1.02, stoichiometric ratio; y (NO)3)3:Er(NO3)3100.0:1.0, stoichiometric ratio; y (NO)3)3:Yb(CH3COO)310.0:1.0, stoichiometric ratio. And (3) continuously stirring by using a magnetic stirrer to finally obtain uniform and stable sol. Controlling the spinning voltage to be 15kV, the spinning receiving distance to be 20cm, keeping the air humidity to be 40% +/-10%, performing electrostatic spinning to obtain precursor nanofibers, and drying in a vacuum oven at 80 ℃ for 3 h. Calcining the dried precursor composite nanofiber at the temperature rising rate of 2 ℃/min to 800 ℃, calcining at 800 ℃ for 4h, and naturally cooling to obtain the final YVO4:Er3+/Yb3+A nanotube sample.
Example 3:
5.0g of polyvinylpyrrolidone was dissolved in 50ml of a mixed solution of water and ethanol (water: ethanol 1:1, mass ratio) until it was clear. Adding a certain amount of Y (NO) into the solution3)3、NH4VO3、Yb(CH3COO)3、Er(NO3)3. Wherein Y (NO)3)3:NH4VO31.0:1.02, stoichiometric ratio; y (NO)3)3:Er(NO3)3100.0:1.0, stoichiometric ratio; y (NO)3)3:Yb(CH3COO)35.0:1.0, stoichiometric ratio. And (3) continuously stirring by using a magnetic stirrer to finally obtain uniform and stable sol. Controlling the spinning voltage to be 15kV, the spinning receiving distance to be 20cm, keeping the air humidity to be 40% +/-10%, performing electrostatic spinning to obtain precursor nanofibers, and drying in a vacuum oven at 80 ℃ for 3 h. Calcining the dried precursor composite nanofiber at the temperature rising rate of 2 ℃/min to 800 ℃, calcining at 800 ℃ for 4h, and naturally cooling to obtain the final YVO4:Er3+/Yb3+A nanotube sample.
Example 4:
5.0g of polyvinylpyrrolidone was dissolved in 50ml of a mixed solution of water and ethanol (water: ethanol 1:1, mass ratio) until it was clear. Adding a certain amount of Y (NO) into the solution3)3、NH4VO3、Yb(CH3COO)3、Er(NO3)3. Wherein Y (NO)3)3:NH4VO31.0:1.02, stoichiometric ratio; y (NO)3)3:Er(NO3)3100.0:1.0, stoichiometric ratio; y (NO)3)3:Yb(CH3COO)310.0:3.0, stoichiometric ratio. And (3) continuously stirring by using a magnetic stirrer to finally obtain uniform and stable sol. Controlling the spinning voltage to be 15kV, the spinning receiving distance to be 20cm, keeping the air humidity to be 40% +/-10%, performing electrostatic spinning to obtain precursor nanofibers, and drying in a vacuum oven at 80 ℃ for 3 h. Calcining the dried precursor composite nanofiber at the temperature rising rate of 2 ℃/min to 800 ℃, calcining at 800 ℃ for 4h, and naturally cooling to obtain the final YVO4:Er3+/Yb3+A nanotube sample.
As can be seen from FIG. 1, the YVO obtained4:Er3+/Yb3+The average diameter of the nanotubes is about 100nm, and the length can reach more than several micrometers.
As can be seen from FIG. 2, the single YVO4:Er3+/Yb3+The outer diameter of the nanotube is about 80nm, and the thickness of the tube wall is about 10-20 nm.
As can be seen from FIG. 3, the YVO obtained4:Er3+/Yb3+The nanotubes have an outer diameter size distribution of 40-150nm and a wall thickness of about 10-20 nm.
As can be seen from FIG. 4, all diffraction peaks in the XRD pattern and YVO of zircon structure4The standard card (JCPDSno.17-0341) of (1) is corresponding to the standard card, and no other phase impurity peak appears; no diffraction peaks of Er and Yb compounds appear. YVO where 2 θ appears 25.02 °, 33.50 °, 49.80 °4Three strong characteristic peaks corresponding to tetragonal phase YVO4Crystals of (200), (112) and (312)And (5) kneading. YVO when the doping concentration of Yb ions is increased4The diffraction peak position of the sample has no obvious change, which indicates that Er ions and Yb ions are in all YVO4Successful doping was achieved in the samples.
As can be seen from FIG. 5, in YVO4:Er3+/Yb3+In the up-conversion emission spectrum of the nanotube, the emission peaks at 525nm and 545nm respectively correspond to Er3+Is/are as follows2H11/2→4I15/2And4S3/2→4I15/2transition; the emission peak at 665nm corresponds to Er3+Is/are as follows4F9/2→4I15/2And (4) transition.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (7)
1. A preparation method of rare earth ion doped yttrium vanadate nanotubes is characterized by comprising the following steps: the method comprises the following steps:
s1, mixing polyvinylpyrrolidone with an ethanol water solution to obtain a mixed solution, adding Y after the mixed solution is clarified3+、NH4VO3And doping ions, and stirring for reaction to obtain sol;
s2, controlling the spinning voltage to be 15-18kV, controlling the spinning receiving distance to be 15-25cm, and keeping the air humidity to be 30-50% to carry out electrostatic spinning to obtain precursor nanofiber;
s3, drying the precursor nano-fiber in a vacuum environment at 80-120 ℃ for 3-6h, heating to 700-4A nanotube.
2. The method for preparing rare earth ion doped yttrium vanadate nanotubes according to claim 1, wherein the method comprises the following steps: in step S1, the mass fraction of polyvinylpyrrolidone in the mixed solution is 10 to 30 wt.%.
3. The method for preparing rare earth ion doped yttrium vanadate nanotubes according to claim 1, wherein the method comprises the following steps: in step S1, the mass fraction of ethanol in the aqueous solution of ethanol is 40-60 wt.%.
4. The method for preparing rare earth ion doped yttrium vanadate nanotubes according to claim 1, wherein the method comprises the following steps: the doping ion is Ce3+、Tb3+、Yb3+、Er3+、Tm3+Or Ho3+Is single ion doped, or is Ce3+/Tb3+、Yb3+/Er3+、Yb3+/Tm3 +Or Yb3+/Ho3+Double ion doping of (2).
5. The method for preparing rare earth ion doped yttrium vanadate nanotubes according to claim 4, wherein the method comprises the following steps: in step S1, the doping ion is Yb3+And Er3+，Y3+And NH4VO3、Yb3+And Er3+Are respectively Y3+:NH4VO3＝1.0:1.02、Y3+:Yb3+＝100.0:(1-30)、Y3+:Er3+＝100.0:1.0。
6. The method for preparing rare earth ion doped yttrium vanadate nanotubes according to claim 5, wherein the method comprises the following steps: in step S1, Y3+Yb is derived from one or two of yttrium nitrate and yttrium acetate3+Er is derived from one or two of ytterbium nitrate and ytterbium acetate3+Derived from one or the combination of erbium nitrate and erbium acetate.
7. A rare earth ion doped yttrium vanadate nanotube is characterized in that: prepared by the method of any one of claims 1 to 6.
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Cited By (2)
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| CN113979464A (en) * | 2021-10-27 | 2022-01-28 | 福建省长汀金龙稀土有限公司 | Method for preparing rare earth oxide powder by oxidizing and roasting rare earth mixture |
| CN114843494A (en) * | 2022-03-04 | 2022-08-02 | 大连海事大学 | Rare earth titanate electrode material with tube centerline structure and preparation method thereof |
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| CN114843494A (en) * | 2022-03-04 | 2022-08-02 | 大连海事大学 | Rare earth titanate electrode material with tube centerline structure and preparation method thereof |
| CN114843494B (en) * | 2022-03-04 | 2024-02-20 | 大连海事大学 | Rare earth titanate electrode material with tube centerline structure and preparation method thereof |
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