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Preparation method for Fe3S4 nanocrystalline material

A nanocrystalline material, fe3s4 technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of complex precursor preparation, poor stability, complex synthesis conditions, etc. The effect of size controllable, good crystallinity and good crystallinity

Active Publication Date: 2013-01-16
UNIV OF SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] The prior art discloses a lot of research results on simulated magnetosomes and their preparation methods. For example, "Dalton Meeting" reported a method of using a mixed solvent to synthesize simulated magnetosomes Fe through a high-pressure hydrothermal reactor. 3 S 4 method of nanocrystalline materials (Dalton Transactions, 2009, 42:9246-9252), but the results show that only Fe can be synthesized by this method 3 S 4 Flower-like microspheres, which limit its further application; another example is that "Langmuir" reported a bacterium-dependent precursor biosynthesis method (Langmuir, 2008, 24:5787-5794), but this method requires The synthesis conditions are relatively complicated, and precursors cannot be obtained in large quantities; "Crystal Engineering Communications" also discloses a method for synthesizing ferromagnetic Fe3S4 nanoparticles through single-source precursors (CrystEngComm, 2010, 12: 3658-3663), However, the preparation of the precursor in this method is very complicated, and the dispersibility and biocompatibility of the synthesized nanoparticles are poor; another example is "Material Science and Engineering" and "Chemical Physics Letters" respectively reported a hydrothermal reaction The high-pressure synthesis method of the autoclave (Materials Science and Engineering, 1999, B64:170-173; ChemicalPhysics Letters, 2005, 403:396-399), using a mixed solvent to prepare the simulated magnetosome Fe3S4 nanocrystalline material, but this method gets Nano-Fe 3 S 4 The stability is poor and cannot meet the needs of practical applications

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  • Preparation method for Fe3S4 nanocrystalline material
  • Preparation method for Fe3S4 nanocrystalline material
  • Preparation method for Fe3S4 nanocrystalline material

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preparation example Construction

[0041] The invention provides a Fe 3 S 4 The preparation method of nanocrystalline material comprises the following steps:

[0042] A) Mix the iron source compound and β-cyclodextrin in ethylene glycol, and heat to obtain a suspension;

[0043] B) Mix and react the suspension with a sulfur source compound to obtain Fe 3 S 4 nanocrystalline material.

[0044] In the present invention, the iron source compound and β-cyclodextrin are first mixed in ethylene glycol, heated to obtain a suspension, and then the suspension is mixed with the sulfur source compound to obtain Fe 3 S 4 nanocrystalline material. The present invention uses ethylene glycol as a solvent and β-cyclodextrin as a surfactant to prepare Fe 3 S 4 Nanocrystalline materials have good crystallinity, stability, water solubility and biocompatibility. The encapsulation of β-cyclodextrin makes Fe 3 S 4 The surface of nanocrystalline materials has a very thin protective layer, similar to biological magnetosomes...

Embodiment 1

[0059] Dissolve 0.0260g (0.35mmol) of thioacetamide in 5mL of ethylene glycol solvent until fully dissolved to obtain an ethylene glycol solution of thioacetamide; under nitrogen protection, dissolve 0.0883g (0.25mmol) of iron acetylacetonate , 0.25mmol β-cyclodextrin and 0.5mmol polyethylene glycol with a number average molecular weight of 4000 were dissolved in 20mL of ethylene glycol solvent, heated to 160°C and kept for reaction until the reaction mixture turned into a turbid yellow suspension , adding the ethylene glycol solution of thioacetamide to it, and immediately obtained a suspension containing a large amount of black precipitate, which was stirred and reacted at 160°C for 2 hours to obtain Fe 3 S 4 nanocrystal suspension, then the reaction system was cooled to 60°C and the Fe 3 S 4 The black precipitate in the nanocrystal suspension was centrifuged and magnetically separated, then washed 3 times with deionized water, and then vacuum freeze-dried to obtain Fe 3 ...

Embodiment 2

[0068] Dissolve 0.0260g (0.35mmol) of thioacetamide in 5mL of ethylene glycol solvent until fully dissolved to obtain an ethylene glycol solution of thioacetamide; under nitrogen protection, dissolve 0.0883g (0.25mmol) of iron acetylacetonate Dissolve 0.25mmol β-cyclodextrin (β-CD) in 20mL ethylene glycol solvent, raise the temperature to 160°C and keep it warm for reaction. When the reaction mixture turns into a turbid yellow suspension, add thioethyl The ethylene glycol solution of amide immediately obtained a suspension containing a large amount of black precipitate, which was stirred and reacted at 160°C for 2 hours to obtain Fe 3 S 4 nanocrystal suspension, then the reaction system was cooled to 60°C and the Fe 3 S 4 The black precipitate in the nanocrystal suspension was centrifuged and magnetically separated, then washed 3 times with deionized water, and then vacuum freeze-dried to obtain Fe 3 S 4 nanocrystalline material.

[0069] get Fe 3 S 4 After the nanocrys...

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Abstract

The invention provides a preparation method for a Fe2S4 nanocrystalline material. The method comprises the following steps of: mixing an iron source compound and beta-cyclodextrin in ethylene glycol, and heating to obtain turbid liquid; and mixing the obtained turbid liquid and a sulphur source compound and reacting to obtain the Fe3S4 nanocrystalline material. According to the method, the Fe3S4 nanocrystalline material which is prepared by using the ethylene glycol as a solvent and the beta-cyclodextrin as surfactant is high in crystallinity, stability, water solubility and biocompatibility. By the wrapping of the beta-cyclodextrin, the surface of the Fe3S4 nanocrystalline material is provided with a very thin protection film, so that the nanocrystalline material is similar to biological magnetosome in nature, has the function which is similar to that of the biological magnetosome, and can be used in the fields of magnetic resonance imaging, medicine carrying and other biological medicines.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a Fe 3 S 4 Preparation methods of nanocrystalline materials. Background technique [0002] Magnetosomes are nano-magnetic particles that exist in magnetotactic bacteria and have a guiding function. They can guide bacteria to swim to the most favorable living environment. The main component of magnetosomes is Fe 3 o 4 and Fe 3 S 4 , generally 20nm~100nm truncated octahedron, parallelepiped or hexagonal prism, has the advantages of small and uniform particles, large specific surface area, biofilm coating, non-aggregation between particles and no cytotoxicity. The field has a wide range of application values, such as magnetosomes can be used as carriers of enzymes, drugs, antibodies and genes; using its own magnetism, magnetosomes can be used as magnetically oriented drugs and antibodies, and to manufacture biosensors, etc. , so magnetosomes will be a new bio...

Claims

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Application Information

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IPC IPC(8): C01G49/12B82Y30/00
Inventor 俞书宏冯梅陆杨
Owner UNIV OF SCI & TECH OF CHINA
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