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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, applied in the preparation of magnetic microspheres with core-shell structure and Fe3O4/α-Fe2O3 core-shell structure magnetic microspheres, can solve the problems of strict low-temperature burning process and achieve Simple method, wide application prospect, novel structure effect

Active Publication Date: 2015-04-08
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 method for preparing Fe3O4 / α-Fe2O3 core-shell structure magnetic microspheres. In the present invention, a certain amount of FeSO4·7H2O is first dissolved in ethylene glycol, and after dissolution, polyvinylpyrrolidone (PVP) and urea are added respectively, and stirred to completely dissolve to obtain a light green solution; the mixed solution is transferred to a polytetrafluoroethylene In a vinyl fluoride-lined stainless steel reactor, seal it, react at 160-220°C for 6 to 24 hours, and then naturally cool to room temperature; then separate and wash to obtain Fe3O4 nanospheres. Then use the liquid phase coating method to dissolve a certain amount of FeCl3·6H2O in deionized water, then add PVP and urea in sequence, stir to completely dissolve to ensure that the reactants are evenly mixed, then add the prepared Fe3O4 nanospheres, and After reacting at 80-95°C for 6-24 hours, it is naturally cooled to room temperature; then it is washed and dried to obtain Fe3O4 / Fe2O3 composite magnetic microspheres. The shell thickness is adjusted by adjusting the molar ratio of FeCl3·6H2O and urea. The invention has simple process, low cost, high output and easy control of product morphology and structure.

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 Patents(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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