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Preparation method of F-doped gamma-ferric oxide hollow microspheres with adjustable bandwidth

A technology of ferric oxide and fluorine doping, which is applied in the direction of iron oxide, iron oxide/iron hydroxide, nanotechnology for materials and surface science, etc., and can solve the problems of difficult mass preparation and large-scale production, complex processes, etc. problem, to achieve the effect of low cost, simple process and excellent optical performance

Inactive Publication Date: 2012-06-20
SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0004] At present, soft / hard template methods are usually used to prepare micro-nano materials with hollow structures. Such methods usually face a series of post-treatment processes such as template removal. The process is relatively complicated and difficult to mass-produce and scale-up

Method used

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  • Preparation method of F-doped gamma-ferric oxide hollow microspheres with adjustable bandwidth
  • Preparation method of F-doped gamma-ferric oxide hollow microspheres with adjustable bandwidth
  • Preparation method of F-doped gamma-ferric oxide hollow microspheres with adjustable bandwidth

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The steps and conditions of the fluorine-doped γ-ferric oxide hollow microspheres prepared in this example are as follows:

[0030] 1) 16mmolFeCl 3 Dissolve in 40ml ethylene glycol, stir well to form FeCl 3 A clear solution with a concentration of 0.4mol / 1, i.e. the first solution;

[0031] 2) NH 4 F follow R F =0.1 was added to the first solution, fully stirred to form the second solution;

[0032] 3) Add ethylenediamine dropwise to the second solution, the volume ratio of the added amount to ethylene glycol is 0.2:1, and fully stir to form the third solution;

[0033] 4) Transfer the third solution obtained above into a closed reaction vessel, and keep it warm for 12 hours under the condition of 200° C. to obtain a precipitate;

[0034] 5) Finally, the precipitate obtained in the above step 4) was washed several times with dehydrated ethanol and deionized water, dried, and calcined at 250°C to obtain the fluorine-doped γ-iron sesquioxide hollow microstructure. bal...

Embodiment 2

[0037] Except step 1) use Fe(NO 3 ) 3 , Fe 2 (SO 4 ) 3 Except for its mixture, other steps and conditions are the same as in Example 1, and fluorine-doped γ-iron sesquioxide hollow microspheres can also be obtained.

[0038] The transmission electron microscope (TEM) photo and the electron diffraction pattern (ED) of the fluorine-doped gamma-iron sesquioxide hollow microspheres prepared in the present embodiment are respectively as follows figure 2 shown, from figure 2 It can be seen that the edge and center of the prepared product have obvious contrast, wherein the edge is darker and the center is lighter, which shows that the prepared sample has a hollow structure, good dispersion, uniform particle size, and a size of 200 ~300nm, the wall thickness is 20~40nm;

Embodiment 3

[0040] This example prepares fluorine-doped γ-ferric oxide hollow microspheres, the steps and conditions are as follows:

[0041] 1) Fe 2 (SO 4 ) 3 Dissolve in 40ml ethylene glycol, stir well to form Fe 2 (SO 4 ) 3 The concentration is the first solution of 0.05mol / 1;

[0042] 2) Put NaF in accordance with R F =0.5 was added to the first solution, fully stirred to form the second solution;

[0043] 3) adding ethylenediamine dropwise to the second solution, the volume ratio of the added amount to ethylene glycol is 0.35:1, fully stirring to form the third solution;

[0044] 4) transfer the third solution obtained above into a closed reaction vessel, and keep it warm for 16 hours under the condition of 220° C. to obtain a precipitate;

[0045] 5) Finally, the precipitate obtained in the above step 4) was washed several times with dehydrated ethanol and deionized water, dried, and calcined at 250°C to obtain the fluorine-doped γ-iron sesquioxide hollow microstructure. ba...

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Abstract

The invention provides a preparation method of F-doped gamma-ferric oxide hollow microspheres with adjustable bandwidth. The preparation method comprises the steps of: (A) adding soluble ferric salt to 40 mL of ethylene glycol solution, and sufficiently stirring to form a first solution; (B) weighing a certain amount of fluoride salt, dissolving in the first solution, and sufficiently stirring to form a second solution, wherein 0<RF<=3 and RF is the atom number ratio of F to Fe; (C) adding ethylene diamine to the second solution to obtain a third solution; and (D) placing the third solution in a sealed reaction container, insulating heat for several hours to obtain precipitate, washing the precipitate, drying, and finally calcining at 250 DEG C to prepare the F-doped gamma-ferric oxide hollow microspheres, wherein the bandwidth of the F-doped gamma-ferric oxide hollow microspheres is adjusted by adjusting the RF value. The prepared F-doped gamma-ferric oxide hollow microspheres have the characteristics of good dispersivity, uniform size, regular crystal form and the like; and the raw materials are low in cost, and the preparation method is simple in process, can realize large-scale preparation and is suitable for scale production.

Description

technical field [0001] The invention relates to a preparation method of fluorine-doped gamma-ferric oxide hollow microspheres with adjustable bandwidth. Background technique [0002] Semiconductor materials, due to their unique and excellent optics, catalysis, electricity, and magnetism, are widely used in electronic devices, information storage, magnetic resonance imaging (MRI), solar photovoltaic power generation, photocatalysis and other fields. With the development of technology, it is found that when the size of the material reaches the nanoscale, it often exhibits different electrical, magnetic, and optical properties from bulk materials, so nanomaterials have attracted more and more attention. In recent years, the practical application of nanomagnetic materials in magnetic storage, superfluid, magnetic transport of drugs, photocatalysis, etc. has become increasingly widespread. Ferric oxide (Fe 2 o 3 ) is an important class of magnetic semiconductor compounds, whic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/06B82Y30/00B82Y40/00
Inventor 朱路平邴乃慈汪玲玲
Owner SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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