CN108192595B - Magnetic-up-conversion nanoparticle aggregate and preparation method thereof - Google Patents
Magnetic-up-conversion nanoparticle aggregate and preparation method thereof Download PDFInfo
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- CN108192595B CN108192595B CN201810072161.XA CN201810072161A CN108192595B CN 108192595 B CN108192595 B CN 108192595B CN 201810072161 A CN201810072161 A CN 201810072161A CN 108192595 B CN108192595 B CN 108192595B
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
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Abstract
The invention discloses a magnetic-up-conversion nanoparticle aggregate, which is prepared by the following method: under the protection of nitrogen, uniformly mixing an oleic acid modified magnetic nanoparticle chloroform solution and an oleic acid modified up-conversion nanoparticle chloroform solution according to a mass ratio of 4:1-1: 10; adding dodecyl trimethyl ammonium bromide water solution, and stirring for 5-15 minutes at 35-45 ℃; then adding 0.2g of polyvinylpyrrolidone and 4.0-10.0mL of glycol, stirring for 3-8 hours at 75-85 ℃, and cooling to room temperature; and (4) centrifuging and washing to obtain the magnetic-up-conversion nano particle aggregate. The preparation method is simple and convenient, has good repeatability, and can realize accurate regulation and control of the content, the size, the superparamagnetism and the up-conversion luminescence performance of each component of the magnetic-up-conversion nanoparticle aggregate by adjusting the reaction parameters such as the proportion of the magnetic nanoparticles to the up-conversion nanoparticles and the addition amount of ethylene glycol; can simultaneously meet the application requirements of biological separation, biological imaging, biological detection, magnetic heat treatment and the like.
Description
Technical Field
The invention belongs to the field of nano composite materials, and particularly relates to a magnetic-up-conversion nano particle aggregate and a preparation method thereof.
Background
With the rapid development of biomedical nano materials, the construction of diagnosis and treatment platforms based on multifunctional nano composite materials becomes a research hotspot. The magneto-optical composite material has both magnetic response capability and fluorescence property, thereby showing huge application prospect in the fields of targeted drug delivery, biological imaging, biological detection, photodynamic therapy, cell separation and the like, and receiving wide attention of researchers in recent years.
Compared with traditional fluorescent nano materials such as semiconductor nanocrystals, organic dyes, quantum dots and the like, the rare earth doped up-conversion nano material has unique anti-Stokes luminescent properties, the exciting light of the rare earth doped up-conversion nano material is near infrared light, the rare earth doped up-conversion nano material has stronger biological tissue penetrating capability, small damage to organisms and good photochemical stability, can effectively avoid the interference of background fluorescence of the organisms, and the unique properties enable the up-conversion nano material to have potential application prospects in biomedicine.
Magnetic nano materials, such as iron-based nanocrystals, ferroferric oxide nano materials and the like, show unique size effect on the nano scale and generally have strong magnetic response capability. Medical experiments prove that the magnetic nano material can escape from phagocytosis of a reticuloendothelial cell system under a magnetic field, has a clear in-vivo metabolic pathway, and is widely applied to the fields of biological separation, drug targeting transportation, magnetic resonance imaging and the like. In addition, the magnetic nano material also has magnetic-thermal conversion capacity, can generate heat energy under an alternating magnetic field, improves the tissue temperature and kills tumor cells.
If the rare earth up-conversion luminescent material is compounded with the magnetic nano material, a multifunctional diagnosis and treatment platform integrating the capabilities of magnetic thermal treatment, magnetic resonance imaging, fluorescence imaging and the like is constructed, the multifunctional diagnosis and treatment platform can meet the multifunctional requirement of the modern biomedical field on the nano composite material, and has important practical application significance. However, the current methods for preparing magnetic-upconversion nanocomposites are mainly seed growth, cross-linker coupling and SiO2Coating methods, and the like. The preparation methods have the common problems that the preparation process is complex, the reaction process is difficult to control, and the regulation and control of the performance of the composite material cannot be realized accurately by regulating the content of each component in the composite material.
Disclosure of Invention
The invention aims to solve the problem that the content, the magnetic property and the up-conversion luminescence property of each component of a magnetic-up-conversion nano composite material prepared by the prior art cannot be accurately regulated and controlled, and provides a magnetic-up-conversion nano particle aggregate with simple preparation process and good repeatability and a preparation method thereof.
A method for preparing magnetic-up-conversion nanoparticle aggregates, comprising:
1) under the protection of nitrogen, uniformly mixing an oleic acid modified magnetic nanoparticle chloroform solution and an oleic acid modified up-conversion nanoparticle chloroform solution according to a mass ratio of 4:1-1: 10;
2) adding 1-3 mL of dodecyl trimethyl ammonium bromide aqueous solution, and stirring for 5-15 minutes at 35-45 ℃;
3) then adding polyvinylpyrrolidone and 4.0-10.0mL of glycol, stirring for 3-8 hours at 75-85 ℃, and cooling to room temperature;
4) centrifuging and washing to obtain magnetic-up-conversion nano particle aggregates;
the oleic acid modified magnetic nanoparticles in the step 1) are Fe and Fe3O4、Fe2O3、FePt、CoFe2O、NiFeO4Or MnFeO4(ii) a The oleic acid modified rare earth doped up-conversion nano particle is NaYF4：Yb3+，Er3+、NaYF4：Yb3+，Tm3+、NaYF4：Yb3+，Ho3+、NaGdF4：Yb3+，Er3+、NaGdF4：Yb3+，Tm3+Or NaGdF4：Yb3+，Ho3+；
The concentration of the dodecyl trimethyl ammonium bromide aqueous solution in the step 2) is 65.0 mu M, and the addition amount is 1 mL; the stirring is carried out for 10 minutes at 40 ℃;
the molecular weight of the polyvinylpyrrolidone in the step 3) is 40000, and the addition amount is 0.2 g; the stirring is carried out for 6 hours at 80 ℃.
The oleic acid modified up-conversion nanoparticle chloroform solution is prepared by the following method:
mixing rare earth chloride, sodium hydroxide, ammonium fluoride, oleic acid and octadecene according to the molar ratio of 2:5:8:38:74, heating to 310 ℃ under the protection of nitrogen, reacting for 1.5 hours, and cooling to room temperature; adding an acetone solution, centrifuging, and dispersing in a chloroform solution to obtain an oleic acid modified rare earth doped up-conversion nanoparticle chloroform solution with the size of 48.6 nm and the concentration of 30 mg/mL.
The rare earth chloride is yttrium chloride, ytterbium chloride or erbium chloride.
The oleic acid modified magnetic nanoparticle chloroform solution is prepared by the following method:
mixing oleic acid, oleylamine, ferric acetylacetonate, 1, 2-hexadecanediol and benzyl ether according to the mole ratio of 2:2:2:10:105, addingHeating to 200 ℃ under the protection of nitrogen for reaction for 1 hour, heating to 300 ℃ for reaction for 1 hour, and cooling to room temperature; washing with magnetic field for three times, dispersing in chloroform to obtain Fe with size of 5.2 nm and concentration of 20 mg/mL3O4Nanoparticle chloroform solution.
The invention provides a magnetic-up-conversion nanoparticle aggregate, which is prepared by the following method: under the protection of nitrogen, uniformly mixing an oleic acid modified magnetic nanoparticle chloroform solution and an oleic acid modified up-conversion nanoparticle chloroform solution according to a mass ratio of 4:1-1: 10; adding 1-3 mL of 65.0 mu M dodecyl trimethyl ammonium bromide aqueous solution, and stirring for 5-15 minutes at 35-45 ℃; then adding 0.2g of polyvinylpyrrolidone and 4.0-10.0mL of glycol, stirring for 3-8 hours at 75-85 ℃, and cooling to room temperature; and (4) centrifuging and washing to obtain the magnetic-up-conversion nano particle aggregate. The preparation method is simple and convenient, has good repeatability, and can realize accurate regulation and control of the content, the size, the superparamagnetism and the up-conversion luminescence performance of each component of the magnetic-up-conversion nanoparticle aggregate by adjusting the reaction parameters such as the proportion of the magnetic nanoparticles to the up-conversion nanoparticles and the addition amount of ethylene glycol; the nano composite material prepared by the method has highly controllable content, size, magnetism and up-conversion luminescence property of each component, and can simultaneously meet the application requirements of biological separation, biological imaging, biological detection, magnetic heat treatment and the like.
Drawings
FIG. 1 scanning electron micrograph of magnetically-upconverting nanoparticle aggregates;
FIG. 2 magnetic-upconverting nanoparticle aggregate size versus magnetic nanoparticle to upconverting nanoparticle ratio;
figure 3 magnetic-upconversion nanoparticle aggregate size versus ethylene glycol volume.
Detailed Description
Example 1 preparation of magnetic-upconversion nanoparticle aggregates
Under the protection of nitrogen, the oleic acid modified magnetic nanoparticle chloroform solution and the oleic acid modified up-conversion nanoparticle chloroform solution are mixed according to the ratio of 4:1, adding 1mL of dodecyl trimethyl ammonium bromide aqueous solution with the concentration of 65.0 mu M, stirring for 10 minutes at 40 ℃, adding 0.2g of polyvinylpyrrolidone and 5.0mL of glycol, stirring for 6 hours at 80 ℃, cooling to room temperature, and centrifugally washing to obtain a magnetic-up-conversion nanoparticle aggregate with the size of 412 nm; a scanning electron micrograph of the magnetic-upconverting nanoparticle aggregates is shown in fig. 1.
Example 2 preparation of magnetic-upconversion nanoparticle aggregates
Under the protection of nitrogen, performing the following steps of (1) mixing an oleic acid modified magnetic nanoparticle chloroform solution and an oleic acid modified up-conversion nanoparticle chloroform solution according to the weight ratio of 1:1, adding 1mL of dodecyl trimethyl ammonium bromide aqueous solution with the concentration of 65.0 mu M, stirring for 10 minutes at 40 ℃, adding 0.2g of polyvinylpyrrolidone and 5.0mL of glycol, stirring for 6 hours at 80 ℃, cooling to room temperature, and centrifugally washing to obtain the 523 nm-sized magnetic-up-conversion nanoparticle aggregate.
Example 3 preparation of magnetic-upconversion nanoparticle aggregates
Under the protection of nitrogen, performing the following steps of (1) mixing an oleic acid modified magnetic nanoparticle chloroform solution and an oleic acid modified up-conversion nanoparticle chloroform solution according to the weight ratio of 1:10, adding 1mL of dodecyl trimethyl ammonium bromide aqueous solution with the concentration of 65.0 mu M, stirring for 10 minutes at 40 ℃, adding 0.2g of polyvinylpyrrolidone and 5.0mL of glycol, stirring for 6 hours at 80 ℃, cooling to room temperature, and centrifugally washing to obtain the magnetic-up-conversion nanoparticle aggregate with the size of 854 nm.
Example 4 preparation of magnetic-upconversion nanoparticle aggregates
Under the protection of nitrogen, uniformly mixing an oleic acid modified magnetic nanoparticle chloroform solution and an oleic acid modified up-conversion nanoparticle chloroform solution according to a mass ratio of 4:1, adding 1mL of dodecyl trimethyl ammonium bromide aqueous solution with a concentration of 65.0 mu M, stirring for 10 minutes at 40 ℃, adding 0.2g of polyvinylpyrrolidone and 4.0mL of ethylene glycol, stirring for 6 hours at 80 ℃, cooling to room temperature, and centrifugally washing to obtain a magnetic-up-conversion nanoparticle aggregate with the size of 201 nm.
Example 5 preparation of magnetic-upconversion nanoparticle aggregates
Under the protection of nitrogen, uniformly mixing an oleic acid modified magnetic nanoparticle chloroform solution and an oleic acid modified up-conversion nanoparticle chloroform solution according to a mass ratio of 4:1, adding 1mL of 65.0 mu M dodecyl trimethyl ammonium bromide aqueous solution, stirring at 40 ℃ for 10 minutes, adding 0.2g of polyvinylpyrrolidone and 7.5 mL of ethylene glycol, stirring at 80 ℃ for 6 hours, cooling to room temperature, and performing centrifugal washing to obtain a magnetic-up-conversion nanoparticle aggregate with the size of 423 nm.
Example 6 preparation of magnetic-upconversion nanoparticle aggregates
Under the protection of nitrogen, uniformly mixing an oleic acid modified magnetic nanoparticle chloroform solution and an oleic acid modified up-conversion nanoparticle chloroform solution according to a mass ratio of 4:1, adding 1mL of dodecyl trimethyl ammonium bromide aqueous solution with a concentration of 65.0 mu M, stirring for 10 minutes at 40 ℃, adding 0.2g of polyvinylpyrrolidone and 10.0mL of ethylene glycol, stirring for 6 hours at 80 ℃, cooling to room temperature, and centrifugally washing to obtain a 471 nm-sized magnetic-up-conversion nanoparticle aggregate.
The size of the magnetic-up-conversion nanoparticle aggregate prepared in the embodiments 1 to 6 can be regulated; as shown in fig. 2, the relationship between the size of the magnetic-upconversion nanoparticle aggregates and the ratio of the magnetic nanoparticles to the upconversion nanoparticles is shown; fig. 3 shows the relationship between the aggregate size of the magnetic-up-conversion nanoparticles and the volume of ethylene glycol.
Example 7 preparation of oleic acid-modified rare earth-doped upconversion nanoparticle chloroform solution
Mixing rare earth chlorides (yttrium chloride, ytterbium chloride and erbium chloride), sodium hydroxide, ammonium fluoride, oleic acid and octadecene according to a molar ratio of 2:5:8:38:74, heating to 310 ℃ under the protection of nitrogen, reacting for 1.5 hours, and cooling to room temperature; adding an acetone solution, centrifuging, and dispersing in a chloroform solution to obtain an oleic acid modified rare earth doped up-conversion nanoparticle chloroform solution with the size of 48.6 nm and the concentration of 30 mg/mL.
Example 8 preparation of oleic acid-modified magnetic nanoparticle chloroform solution
Oleic acid, oleylamine,Mixing ferric acetylacetonate, 1, 2-hexadecanediol and benzyl ether according to the molar ratio of 2:2:2:10:105, heating to 200 ℃ under the protection of nitrogen for reaction for 1 hour, heating to 300 ℃ for reaction for 1 hour, and cooling to room temperature; washing with magnetic field for three times, dispersing in chloroform to obtain Fe with size of 5.2 nm and concentration of 20 mg/mL3O4Nanoparticle chloroform solution.
Claims (10)
1. A method for preparing magnetic-up-conversion nanoparticle aggregates, comprising:
1) under the protection of nitrogen, uniformly mixing an oleic acid modified magnetic nanoparticle chloroform solution and an oleic acid modified up-conversion nanoparticle chloroform solution according to a mass ratio of 4:1-1: 10;
2) adding 1-3 mL of dodecyl trimethyl ammonium bromide aqueous solution, and stirring for 5-15 minutes at 35-45 ℃;
3) then adding polyvinylpyrrolidone and 4.0-10.0mL of glycol, stirring for 3-8 hours at 75-85 ℃, and cooling to room temperature;
4) and (4) centrifuging and washing to obtain the magnetic-up-conversion nano particle aggregate.
2. The method of preparing magnetic-upconversion nanoparticle aggregates according to claim 1, characterized in that: the oleic acid modified magnetic nanoparticles in the step 1) are Fe and Fe3O4、Fe2O3、FePt、CoFe2O、NiFeO4Or MnFeO4。
3. The method for preparing magnetic-upconversion nanoparticle aggregates according to claim 1 or 2, characterized in that: the oleic acid modified rare earth doped up-conversion nanoparticles in the step 1) are NaYF4：Yb3+，Er3+、NaYF4：Yb3+，Tm3+、NaYF4：Yb3+，Ho3+、NaGdF4：Yb3+，Er3+、NaGdF4：Yb3+，Tm3+Or NaGdF4：Yb3+，Ho3+。
4. The method of preparing magnetic-upconversion nanoparticle aggregates according to claim 3, characterized in that: the concentration of the dodecyl trimethyl ammonium bromide aqueous solution in the step 2) is 65.0 mu M, and the addition amount is 1 mL.
5. The method of preparing magnetic-upconversion nanoparticle aggregates according to claim 4, characterized in that: the molecular weight of the polyvinylpyrrolidone in the step 3) is 40000, and the addition amount is 0.2 g.
6. The method of preparing magnetic-upconversion nanoparticle aggregates according to claim 5, characterized in that: the stirring in step 2) is carried out at 40 ℃ for 10 minutes.
7. The method of preparing magnetic-upconversion nanoparticle aggregates according to claim 6, characterized in that: the stirring in step 3) is carried out at 80 ℃ for 6 hours.
8. The method of preparing magnetic-upconversion nanoparticle aggregates according to claim 1, characterized in that: the oleic acid modified up-conversion nanoparticle chloroform solution is prepared by the following method:
mixing rare earth chloride, sodium hydroxide, ammonium fluoride, oleic acid and octadecene according to the molar ratio of 2:5:8:38:74, heating to 310 ℃ under the protection of nitrogen, reacting for 1.5 hours, and cooling to room temperature; adding an acetone solution, centrifuging, and dispersing in a chloroform solution to obtain an oleic acid modified rare earth doped up-conversion nanoparticle chloroform solution with the size of 48.6 nm and the concentration of 30 mg/mL.
9. The method of preparing magnetic-upconversion nanoparticle aggregates according to claim 8, characterized in that: the rare earth chloride is yttrium chloride, ytterbium chloride or erbium chloride.
10. The method for the preparation of magnetic-up-conversion nanoparticle aggregates according to claim 1, 8 or 9, characterized in that: the oleic acid modified magnetic nanoparticle chloroform solution is prepared by the following method:
mixing oleic acid, oleylamine, ferric acetylacetonate, 1, 2-hexadecanediol and benzyl ether according to the molar ratio of 2:2:2:10:105, heating to 200 ℃ under the protection of nitrogen for reaction for 1 hour, heating to 300 ℃ for reaction for 1 hour, and cooling to room temperature; washing with magnetic field for three times, dispersing in chloroform to obtain Fe with size of 5.2 nm and concentration of 20 mg/mL3O4Nanoparticle chloroform solution.
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| CN105903013A (en) * | 2016-04-26 | 2016-08-31 | 东北师范大学 | Fe3O4 nanometer particle aggregate and preparation method thereof |
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| CN105903013A (en) * | 2016-04-26 | 2016-08-31 | 东北师范大学 | Fe3O4 nanometer particle aggregate and preparation method thereof |
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