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Preparation method of Fe3O4/alpha-Fe2O3 magnetic microspheres in core/shell structure

A technology of magnetic microspheres and core-shell structure, which is applied in the preparation of Fe3O4/α-Fe2O3 core-shell magnetic microspheres and the field of core-shell magnetic microspheres, which can solve the problems of strict low-temperature burning process and achieve Simple method, improved magnetic properties, wide application prospects

Active Publication Date: 2014-01-01
秦河新材股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method also has the problem of strict low-temperature burning process requirements, and the obtained γ-Fe 2 o 3 The cladding layer is still a metastable phase, not as good as α-Fe 2 o 3 Stablize

Method used

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  • Preparation method of Fe3O4/alpha-Fe2O3 magnetic microspheres in core/shell structure
  • Preparation method of Fe3O4/alpha-Fe2O3 magnetic microspheres in core/shell structure
  • Preparation method of Fe3O4/alpha-Fe2O3 magnetic microspheres in core/shell structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Weigh 1.5mmol FeSO 4 ·7H 2 O was dissolved in ethylene glycol, and after dissolution, 0.8g of PVP and 3.5mmol of urea were added, stirred to completely dissolve, and a light green solution was obtained.

[0020] (2) Transfer the above solution to a stainless steel reaction kettle lined with polytetrafluoroethylene, seal it, react at 200°C for 24h, and cool it down to room temperature naturally;

[0021] (3) The obtained precipitate was centrifuged and washed repeatedly with water and ethanol to obtain Fe 3 o 4 nanosphere dispersion;

[0022] (4) Weigh 0.037mmol FeCl 3 ·6H 2 O was dissolved in deionized water, and then 0.1 g of PVP and 0.33 mmol of urea were added in sequence, and stirred to completely dissolve to ensure that the reactants were evenly mixed, and then the prepared Fe 3 o 4 Microspheres, after reacting at 90°C for 24h, naturally cool to room temperature;

[0023] (5) Centrifuge the obtained precipitate, wash repeatedly with water and ethanol, a...

Embodiment 2

[0025] (1) Weigh 1.5mmol FeSO 4 ·7H 2 O was dissolved in ethylene glycol, and after dissolution, 0.8g of PVP and 3.5mmol of urea were added, stirred to completely dissolve, and a light green solution was obtained.

[0026] (2) Transfer the above solution to a stainless steel reaction kettle lined with polytetrafluoroethylene, seal it, react at 200°C for 24h, and cool it down to room temperature naturally;

[0027] (3) The obtained precipitate was centrifuged and washed repeatedly with water and ethanol to obtain Fe 3 o 4 nanosphere dispersion;

[0028] (4) Weigh 0.074mmol FeCl 3 ·6H 2 O was dissolved in deionized water, and then 0.1 g of PVP and 0.33 mmol of urea were added in sequence, and stirred to completely dissolve to ensure that the reactants were evenly mixed, and then the prepared Fe 3 o 4 Microspheres, after reacting at 90°C for 24h, naturally cool to room temperature;

[0029] (5) Centrifuge the obtained precipitate, wash repeatedly with water and ethanol, a...

Embodiment 3

[0031] (1) Weigh 1.5mmol FeSO 4 ·7H 2 O was dissolved in ethylene glycol, and after dissolution, 0.8g of PVP and 5.0mmol of urea were added, stirred to completely dissolve, and a light green solution was obtained.

[0032] (2) Transfer the above solution to a stainless steel reaction kettle lined with polytetrafluoroethylene, seal it, react at 200°C for 16 hours, and cool it down to room temperature naturally;

[0033] (3) The obtained precipitate was centrifuged and washed repeatedly with water and ethanol to obtain Fe 3 o 4 nanosphere dispersion;

[0034] (4) Weigh 0.05mmol FeCl 3 ·6H 2 O was dissolved in deionized water, and then 0.1 g of PVP and 0.33 mmol of urea were added in sequence, and stirred to completely dissolve to ensure that the reactants were evenly mixed, and then the prepared Fe 3 o 4 Microspheres, after reacting at 90°C for 12h, naturally cool to room temperature;

[0035] (5) Centrifuge the obtained precipitate, wash repeatedly with water and ethano...

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Abstract

The invention discloses a preparation method of Fe3O4 / alpha-Fe2O3 magnetic microspheres in a core / shell structure. The preparation method disclosed by the invention comprises the following steps: dissolving certain FeSO4.7H2O in glycol; after FeSO4.7H2O is dissolved, adding polyvinylpyrrolidone (PVP) and urea into the resulting solution for complete dissolving by stirring to obtain a light green solution; transferring the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene liner; sealing the reaction kettle; carrying out reaction at 160-220 DEG C for 6-24 hours; naturally cooling the resulting product to room temperature; carrying out separation and washing to obtain Fe3O4 nanometer spheres; dissolving a certain amount of FeCl3.6H2O in deionized water by means of a liquid-phase coating method; sequentially adding PVP and urea into the resulting solution for complete dissolving by stirring; adding in the prepared Fe3O4 nanometer particle after ensuring that the reactants are uniformly mixed; carrying out reaction at 80-95 DEG C for 6-24 hours; naturally cooling the reaction product to room temperature; and washing and drying the product to obtain the Fe3O4 / Fe2O3 composite magnetic microspheres. The thickness of the shell layer can be regulated by regulating the molar ratio of FeCl3.6H2O to urea. The preparation method disclosed by the invention is simple in process, low in cost, and high in yield; and the morphology and the structure of the product are easily controllable.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic functional materials, and relates to a method for preparing magnetic microspheres with a core-shell structure, in particular to a Fe 3 o 4 / α-Fe 2 o 3 A method for preparing magnetic microspheres with a core-shell structure. Background technique [0002] Fe 3 o 4 is an important magnetic iron oxide, nano-Fe 3 o 4 Due to its unique electrical and magnetic properties, it has wider application value in the fields of magnetic liquid, magnetic recording material, catalysis, microwave absorbing material and biomedicine. Therefore, in recent years, the Fe 3 o 4 The research on the preparation of nanostructures and their properties is very active. But there are also nanostructured Fe 3 o 4 The problem of being easily oxidized during use, resulting in Fe 3 o 4 The sample is unstable and the magnetic properties decrease. In order to solve this problem, the method of coating treatment i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02H01F1/11C01G49/06C01G49/08
Inventor 王德宝宋彩霞姜丽红周艳红蔺玉胜
Owner 秦河新材股份有限公司
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