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Method for hydrothermally preparing mono-dispersed hollow magnetic nanometer particles

A magnetic nanoparticle, monodisperse technology, applied in the direction of magnetism, nanotechnology, chemical instruments and methods of organic materials/organic magnetic materials, can solve the constraints on the industrialization of hollow magnetic nanoparticles, the large diameter of hollow magnetic nanoparticles, Not suitable for large-scale production and other issues, to achieve the effect of easy large-scale promotion, good dispersion, and convenient industrial production

Inactive Publication Date: 2012-08-15
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Caruso et al. (F.Caruso, M.Spasova, A.Susha, M.Giersig, R.A.Caruso, Chem.Mater., 2001, 13, 109-116) scholars use a combination of physical and chemical methods to combine Fe 3 o 4 Nanoparticles are adsorbed on the surface of polymer microspheres, and then fired at high temperature to obtain hollow magnetic particles. The main problem of this method is that the preparation steps are cumbersome, and the prepared hollow magnetic nanoparticles have a large diameter and a wide particle size distribution.
[0005] Although researchers have done a lot of work on the preparation of hollow magnetic nanoparticles, the main problems at present are the complex and cumbersome process, high cost, uneven shape and unsuitable for large-scale production, which seriously restrict the development of hollow magnetic nanoparticles. Industrialization development

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  • Method for hydrothermally preparing mono-dispersed hollow magnetic nanometer particles
  • Method for hydrothermally preparing mono-dispersed hollow magnetic nanometer particles
  • Method for hydrothermally preparing mono-dispersed hollow magnetic nanometer particles

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Embodiment 1

[0039] Such as figure 1 As shown, the technical process for preparing hollow magnetic nano-ions is as follows: configure 20 ml of 0.15 mol / L urea solution, and add 50 ml of 0.4 mol / L FeSO at 25 °C and 750 rpm stirring conditions. 4 solution and 5 milliliters of 0.05 mol / liter of polyvinylpyrrolidone solution, then add 0.05 gram of solid ascorbic acid, after it dissolves completely, add 40 milliliters of 0.2 mol / liter of sodium carbonate solution in the above-mentioned sol mixed solution. After the above solution is fully mixed, adjust the pH value to 10.5 with 0.2 mol / liter sodium hydroxide solution, then add 0.001 mol of ethylenediamine, mix and stir for 30 minutes, transfer to a hydrothermal device, and heat at 200°C for 10 Hour. The product obtained after hydrothermal treatment is separated by magnet, washed with water, washed with alcohol and freeze-dried to obtain a large amount of black hollow magnetic Fe with monodisperse characteristics. 3 o 4 Nanoparticles, particl...

Embodiment 2

[0042] Configure 20 ml of 0.2 mol / L urea solution, and add 30 ml of 0.4 mol / L FeSO at 25°C and 750 rpm stirring conditions 4 solution and 20 mL of 0.4 mol / L CoSO 4 solution, then add 3 milliliters of polyvinyl alcohol-200 (PEG-200) dispersant, add 0.1 gram of solid ascorbic acid to the above solution after mixing, after it is completely dissolved, add 30 milliliters of 0.25 mol / liter of Sodium carbonate solution, adjust the pH value to 11.0 with 0.2 mol / L sodium hydroxide solution, then add 0.0001 mol trisodium citrate, mix and stir thoroughly for 30 minutes, transfer to a hydrothermal device, and heat at 220°C for 10 hours. The black product obtained after hydrothermal treatment is separated by magnet, washed with water, washed with alcohol and freeze-dried to obtain hollow magnetic CoFe with monodisperse characteristics. 2 o 4 Nanoparticles, particle size about 150nm, shell thickness 40nm.

Embodiment 3

[0044] Prepare 20 ml of 0.05 mol / L urea solution, add 40 ml of 0.35 mol / L CoSO at 25°C and 750 rpm stirring conditions 4 solution and 3 milliliters of 0.1 mol / liter cetyltrimethylammonium bromide solution, then add 0.02 gram of solid ascorbic acid, after it is completely dissolved, add 30 milliliters of 0.3 mol / liter carbonic acid sodium solution. After the above solution is fully mixed, adjust the pH value to 10.0 with 0.2 mol / liter sodium hydroxide solution, then add 0.001 mol of ethylenediamine, mix and stir for 30 minutes, then transfer to a hydrothermal device, and heat it at 235°C for 8 Hour. The product obtained after hydrothermal treatment was separated by magnet, washed with water, washed with alcohol and freeze-dried to obtain a large amount of hollow magnetic Co with monodisperse characteristics. 3 o 4 Nanoparticles, particle size about 80nm, shell thickness 20nm.

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Abstract

The invention relates to a method for hydrothermally preparing mono-dispersed hollow magnetic nanometer particles. The method comprises the following steps of: firstly, mixing a divalent metal salt solution with a urea solution; secondly, adding an organic dispersant and a divalent metal oxidation inhibitor; thirdly, slowly adding an alkali precipitant solution into the solution; fourthly, adjusting the pH (Potential of Hydrogen) value of the mixed solution to 10-12; and finally, adding a surface radical modifier, and carrying out hydrothermal reaction for 5-15 hours at the temperature of 150-250 DEG C, so as to prepare the magnetic nanometer particles having a hollow structure. Compared with the prior art, the method provided by the invention has the advantages of simple technique step, low cost and the like, and is easy to be large-scale.

Description

technical field [0001] The invention belongs to the field of inorganic ultrafine powder and nanotechnology, and in particular relates to a hydrothermal preparation method of a hollow-structured magnetic nanometer material. Background technique [0002] Magnetic nanoparticles with a hollow structure are a novel material with broad application prospects. Due to their magnetic response properties and hollow structure, they have important applications in the fields of protein and nucleic acid separation, targeted drug carriers, nuclear magnetic resonance imaging, and catalysis. [0003] The formation mechanism of hollow structure nanoparticles mainly includes Kirkendall effect and Ostwald ripening mechanism, and the preparation methods mainly include hard template method and soft template method. The hard template method mainly includes four main processes: the first is the preparation of the hard template, the second is to functionalize the surface of the template to obtain a g...

Claims

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Application Information

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IPC IPC(8): C01G49/08C01G51/00C01G51/04C01G49/00B82Y40/00H01F1/42
Inventor 高国崔大祥
Owner SHANGHAI JIAO TONG UNIV
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