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Superparamagnetism composite microsphere with controllable magnetic saturation intensity and preparation method thereof

A saturation-strength, superparamagnetic technology, used in magnetic materials, magnetic objects, electrical components, etc., to solve the problem that uniform, superparamagnetic composite microspheres cannot meet the particle size and other problems

Inactive Publication Date: 2012-07-04
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Existing methods for preparing superparamagnetic composite microspheres cannot meet the requirements of high magnetic saturation intensity with uniform particle size and controllable morphology

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: Polyacrylonitrile microspheres with a particle size of 300nm are dispersed in the dispersion liquid N,N-dimethylformamide, the mass percentage is 5%, FeCl 3 Add it into the dispersion liquid, the mass percentage is 20%, react at 50°C for 10 hours, then add excess sodium nitrate solution with a syringe pump, keep the temperature and continue to react for 16 hours. After the reaction is finished, the reaction solution is precipitated with deionized water, the precipitated solution is suction-filtered, washed three times with deionized water, and the obtained polymer microspheres containing iron ions are vacuum-dried for future use.

[0017] The polymer microspheres containing iron ions obtained above were heat-treated at 600° C. for 1 hour under a nitrogen atmosphere in a tube furnace to obtain superparamagnetic iron nanoparticles / carbon composite microspheres with a magnetic saturation strength of 40 emu / g.

Embodiment 2

[0018] Example 2: Polyacrylonitrile microspheres with a particle size of 100nm are dispersed in the dispersion liquid N,N-dimethylformamide, the mass percentage is 2%, FeCl 3 Add to the dispersion liquid, the mass percentage is 30%, react at 60°C for 12 hours, then add excess potassium nitrite solution with a syringe pump, keep the temperature and continue to react for 24 hours. After the reaction is finished, the reaction solution is precipitated with deionized water, the precipitated solution is suction-filtered, washed three times with deionized water, and the obtained polymer microspheres containing iron ions are vacuum-dried for future use.

[0019] The polymer microspheres containing iron ions obtained above were heat-treated at 800° C. for 2 hours under a nitrogen atmosphere in a tube furnace to obtain superparamagnetic iron nanoparticles / carbon composite microspheres with a magnetic saturation strength of 120 emu / g.

Embodiment 3

[0020] Example 3: the particle size is 800nm ​​polyacrylonitrile-polystyrene copolymer microspheres dispersed in the dispersion liquid toluene, the mass percentage is 3%, the CoSO 4 Add it into the dispersion liquid, the mass percentage is 40%, react at 80°C for 12 hours, then add excess sodium nitrite solution with a syringe pump, keep the temperature and continue to react for 36 hours. After the reaction is finished, the reaction solution is precipitated with deionized water, the precipitated solution is suction-filtered, washed three times with deionized water, and the obtained polymer microspheres containing cobalt ions are vacuum-dried for future use.

[0021] The polymer microspheres containing cobalt ions obtained above were heat-treated at 1000° C. for 2 hours in a nitrogen atmosphere in a tube furnace to obtain superparamagnetic cobalt nanoparticles / carbon composite microspheres with a magnetic saturation strength of 160 emu / g.

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PUM

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Abstract

The invention relates to a superparamagnetism composite microsphere with controllable magnetic saturation intensity and a preparation method thereof, comprising the following steps of using a polymer microsphere as a template, complexing metal (iron, cobalt and nickel) ions, improving the complexing amount of the metal ion by using an additional complexing agent, controlling the metal ion concentration, sorts of the additional complexing agent and additional complexing agent concentration so as to obtain the composite microsphere with controllable content of the metal ion, and obtaining the superparamagnetism metal nano-particle / carbon composite microsphere with controllable magnetic saturation intensity by pyrolyzing the composite microsphere. The method is simple and effective, has convenient preparation process and is a general method for preparing the superparamagnetism composite microsphere with controllable magnetic saturation intensity.

Description

technical field [0001] The invention relates to a superparamagnetic composite microsphere with controllable magnetic saturation intensity and a preparation method thereof. Background technique [0002] Due to the large specific surface area of ​​magnetic metal nanoparticles, the surface bond state is severely mismatched, resulting in many active centers with very high surface activity, which are easily oxidized in the air and lose their magnetism. In addition, in the application of biomedicine, Magnetic nanoparticles are easy to aggregate, and measures must be taken to protect and stabilize magnetic nanoparticles. Composite microspheres prepared by compounding with other materials can maintain the unique advantages of magnetic nanoparticles and realize functional integration between materials. With the increasingly in-depth combination of nanotechnology and biomedicine, magnetic composite microspheres have shown broad application prospects in the fields of cell labeling and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01F1/047C01B31/02
Inventor 褚轶雯汪长春
Owner FUDAN UNIV