Method for preparing carbon-coated superparamagnetic ferroferric colloidal spheres

A technology of ferric oxide and superparamagnetism, which is applied in the direction of iron oxide/iron hydroxide, magnetic properties of inorganic materials, oxides of ferrous iron, etc. It can solve the problems of high reaction conditions, complicated process, poor stability, etc. problems, achieve high chemical and colloidal stability, simple process, and overcome the high cost of raw materials

Inactive Publication Date: 2012-05-09
UNIV OF SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The above methods for preparing ferroferric oxide particles either mainly focus on the synthesis mechanism, or require high reaction conditions and complicated processes, and cannot prepare particles with both large particle size and superparamagnetic characteristics.
In addition, the common ferroferric oxide is often surface-modified with high-molecular organic substances, and its stability at high temperatures is not good, so these methods are limited in practical applications

Method used

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  • Method for preparing carbon-coated superparamagnetic ferroferric colloidal spheres
  • Method for preparing carbon-coated superparamagnetic ferroferric colloidal spheres
  • Method for preparing carbon-coated superparamagnetic ferroferric colloidal spheres

Examples

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Embodiment 1

[0033] Embodiment 1. prepares uniform ferric oxide colloidal ball

[0034] Take 0.3g of ferrocene, dissolve it in 30.0mL of acetone, ultrasonically disperse it, then add 1.5ml of 30% hydrogen peroxide dropwise, stir magnetically at 1000r / min for 30 minutes, and then transfer the solution to a volume of 40ml In an autoclave, seal and heat to 240°C, keep it warm for 72 hours, and then cool to room temperature to obtain a black powdery solid; then wash the sample 3 times with acetone and ethanol to remove residual organic matter in the solid powder; then the solid The powder was dried in a vacuum oven at 40°C for 6 hours to obtain the product.

[0035] like figure 1 Shown, according to the X-ray diffraction of present embodiment product Figure, all diffraction peak positions correspond to (111), (220), (311), (222), (400), (422), (511), (440) face of ferric oxide respectively, show product as Ferric oxide; By the transmission electron microscope electron diffraction image of ...

Embodiment 2

[0036] Example 2. Effect of the amount of ferrocene on the product

[0037] Take 0.1g and 0.2g of ferrocene, dissolve them in 30.0mL of acetone, ultrasonically disperse and then add 1.5ml of 30% hydrogen peroxide dropwise, stir magnetically at 1000r / min for 30 minutes, and transfer the solution to In an autoclave with a capacity of 40ml, sealed and heated to 240°C for 72 hours, and then cooled to room temperature to obtain a black powdery solid; then acetone and ethanol were respectively washed the sample 3 times to remove the residual organic matter in the solid powder; then The solid powder was dried in a vacuum oven at 40°C for 6 hours to obtain the product. The appearance of the product is as Figure 8 (0.10g) and Figure 9 (0.20g). Figure 8 and Figure 9 It is shown that the smaller the amount of ferrocene, the smaller the thickness of the carbon layer on the surface of the iron tetroxide nanospheres.

Embodiment 3

[0038] Example 3. Effect of the amount of hydrogen peroxide on the product

[0039] The same solution was prepared in the same way as in Example 1, that is, 0.3g of ferrocene was weighed and dissolved in 30.0ml of acetone, but the amount of hydrogen peroxide added later was changed to 0.5ml, 1.5ml, and 3ml, respectively. , and the other processes are the same. The obtained results were confirmed by X-ray diffraction analysis that they were all colloidal spheres of iron tetroxide. The difference was that colloidal spheres with particle sizes of 90 nm, 150 nm and 200 nm were obtained respectively. A smaller amount of hydrogen peroxide can only obtain small particles with weak magnetic properties, not ferric oxide, and too much hydrogen peroxide has little effect on the change of particle size, so the amount of hydrogen peroxide is usually 0.5ml- between 3ml. The obtained product looks like Figure 10 , Figure 11 and Figure 12 shown. Figure 10 , Figure 11 and Figure ...

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Abstract

The invention discloses a method for preparing carbon-coated superparamagnetic ferroferric oxide gel, which comprises: dissolving ferrocene and surfactant in an acetone solvent; adding solution of hydrogen peroxide into the solution to directly oxidize the ferrocene to synthesize polycrystal uniform magnetic nano balls under a low-temperature (180 to 240 DEG C) solvothermal condition; and allowing the polycrystal uniform magnetic nano balls to react in a magnetic field to prepare a magnetic linear nano material. The polycrystal uniform magnetic nano balls and nano chains are characterized in that: the particle size of the polycrystal uniform magnetic nano balls is limited to a narrow range and controllable; and the nano chains consist of uniform spherical particles and have high stability, and the inter-chain distance is controllable. The superparamagnetic polycrystal uniform nano ball and linear nano chain materials have high superparamagnetism and high chemical stability and gel stability and have promising application prospect in the field of biomedicine, nano self-assembly and the like; the nano balls are grafted by medicaments and can be used as medicament carriers; under theaction of the magnetic field, the nano balls can be used as magnetic control photonic crystal; and the nano chains have a promising application prospect in the field of Bragg reflectors, magnetic probes, biomedicine and the like.

Description

technical field [0001] The invention belongs to the technical field of magnetic nanomaterial preparation, in particular to a preparation method of carbon-coated superparamagnetic ferric oxide nanospheres. Background technique [0002] According to China's "Inorganic Salt Industry" (2007, Vol. 39, Page 5), nano-Fe3O4 is widely used in magnetic liquids, magnetic recording materials, catalysis, biomedicine, and microwave absorbing materials. For example, the ferrofluid prepared by ferroferric oxide has been widely used in the fields of vacuum sealing, voice coil heat dissipation, rapid printing, mineral sorting, precision grinding, sensors and aerospace technology. In biomedicine, Fe3O4 nanoparticles have broad application prospects in targeted drug delivery, NMR enhancer, magnetic separation and other fields. [0003] Journal of the American Chemical Society (J.AM.CHEM.SOC., 2002, volume 124, page 8204) reported a method for synthesizing monodisperse iron ferric oxide nanopar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01F1/34C01G49/08C04B35/628
Inventor 陈乾旺王辉孙玉冰
Owner UNIV OF SCI & TECH OF CHINA
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