Magnetic ferric oxide micrometer flower material with multi-stage structure and preparation method thereof

A technology of ferric oxide and micron flowers is applied in the directions of iron oxide, iron oxide/iron hydroxide, etc., to achieve the effects of convenient practical industrial application, regular product morphology and low production cost

Inactive Publication Date: 2012-09-12
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no hierarchical structure alpha-iron trioxide (α-Fe 2 o 3 ) Relevant literature and patent reports of microflowers

Method used

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  • Magnetic ferric oxide micrometer flower material with multi-stage structure and preparation method thereof
  • Magnetic ferric oxide micrometer flower material with multi-stage structure and preparation method thereof
  • Magnetic ferric oxide micrometer flower material with multi-stage structure and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0028] A method for preparing a magnetic ferric oxide micron flower material with a multi-level structure, comprising the following steps:

[0029] (1) Take 0.005mol ferric chloride hexahydrate as iron source, 100ml ethylene glycol as solvent, add surfactant tetrabutylammonium chloride, stir under normal temperature and pressure, make ferric chloride hexahydrate and Surfactant dissolves completely, and obtaining ferric chloride concentration is the clear solution of 0.05 mol / L;

[0030] (2) Add 0.5mol urea to the clear solution prepared in step (1), stir, and mix thoroughly to obtain a reddish-brown clear solution;

[0031] (3) The above solution prepared in step (2) was reacted at 190°C for 60 min by the ethylene glycol-assisted method;

[0032] (4) Centrifuged after the reaction, the obtained yellow-green precipitate was washed 3 times with absolute ethanol, and then dried at 60°C for 12 h to obtain α-Fe 2 o 3 Precursor;

[0033] (5) Put the precursor in a vacuum atmosph...

Embodiment 2

[0041] (1) Take 0.01mol ferric chloride hexahydrate as the iron source, 100ml ethylene glycol as the solvent, then add 0.00065mol of surfactant tetrabutylammonium chloride, stir at normal temperature and pressure to make hexahydrate trichloride Iron and tensio-active agent dissolve completely, and obtaining ferric chloride concentration is the clear solution of 0.1 mol / L;

[0042] (2) Add 0.1mol urea to the clear solution prepared in step (1), stir, and mix thoroughly to obtain a reddish-brown clear solution;

[0043] (3) The above solution prepared in step (2) was reacted at 192°C for 70 min by ethylene glycol-assisted method;

[0044] (4) Centrifuged after the reaction, the obtained yellow-green precipitate was washed 3 times with absolute ethanol, and then dried at 65 °C for 12 h to obtain α-Fe 2 o 3 Precursor;

[0045] (5) Put the precursor in a vacuum atmosphere box-type furnace, introduce air, and calcine at a high temperature of 340-390 ° C for 5 hours to obtain the ...

Embodiment 3

[0047] (1) Take 0.06mol ferric chloride hexahydrate as iron source, 100ml ethylene glycol as solvent, then add surfactant cetyltrimethylammonium bromide, stir at normal temperature and pressure to make hexahydrate trimethylammonium bromide Ferric chloride and tensio-active agent dissolve completely, obtain the clarification solution that ferric chloride concentration is 0.6 mol / L;

[0048] (2) Add 0.03mol urea to the clear solution prepared in step (1), stir, and mix thoroughly to obtain a reddish-brown clear solution;

[0049] (3) The above solution prepared in step (2) was reacted at 197°C for 30 min by the ethylene glycol-assisted method;

[0050] (4) Centrifuged after the reaction, the obtained yellow-green precipitate was washed 4 times with absolute ethanol, and then dried at 55°C for 13 h to obtain α-Fe 2 o 3 Precursor;

[0051] (5) The precursor is placed in a vacuum atmosphere box furnace, air is introduced, and it is calcined at a high temperature of 380-460 °C fo...

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Abstract

The invention discloses a magnetic ferric oxide micrometer flower material with a multi-stage structure and a preparation method of the magnetic ferric oxide micrometer flower material. The magnetic ferric oxide micrometer flower material with the multi-stage structure has the shape of a flower which is arranged by nano-pieces with the thickness of 85-95nm in an interlaced way assembled by spherical particles with the particle sizes from 20nm to 30nm and has the multi-stage structure, and integrates the nano-grains, the nano-pieces and the micro flower. The preparation method comprises the following steps of: preparing a solution with the concentration of 0.05-0.6mol / L based on hexahydrated ferric trichloride as an iron source and ethylene glycol as solvent, adding a surface active agent, stirring to obtain clear solution, adding urea, reacting for 30-90min by an ethylene glycol auxiliary method at the temperature of 190-197 DEG C, centrifugally separating, cleaning and drying, and calcining for 1-5h at high temperature of 300-500 DEG C, so that the magnetic ferric oxide micrometer flower material can be obtained. The preparation method is simple in technology, low in cost, easy to produce on a large scale, and safe and reliable in production process; and the product is good in repeatability, regular in shape, concentrated in particle size distribution, and free from agglomeration.

Description

technical field [0001] The invention relates to a magnetic ferric oxide material, in particular to a magnetic ferric oxide micron flower material with a multi-level structure, and also relates to a preparation method of the material. Background technique [0002] Due to the quantum size effect, surface effect, macroscopic quantum tunneling effect, Coulomb blockage and dielectric confinement effect, nanoparticles have excellent properties in terms of light, electricity, magnetism, heat, mechanical properties, chemical properties, and biophysical properties. New features different from conventional solids and macroscopic particles. The performance of nanomaterials largely depends on the microscopic morphology of nanoparticles. Therefore, the synthesis of nanomaterials with various special shapes has become an indispensable and important part of the field of nanoscience. [0003] Ferric oxide is a cheap, environmentally friendly, and most stable iron oxide. It has the characte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/06
Inventor 赵贵哲周兴刘亚青柳学义
Owner ZHONGBEI UNIV
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