Method for preparing nano-gamma-Fe2O3 hollow magnetic microsphere

A technology of magnetic microspheres and hollow spheres, applied in the direction of iron oxide/iron hydroxide, iron oxide, etc., can solve the problems of complex operation, difficult process control, less preparation, etc., and achieve high product purity, low raw materials, and simple process. Effect

Active Publication Date: 2008-12-10
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But so far, most of the reports are on the preparation of γ-Fe2O3 nanoparticles. >O3 is relatively less prepared
Moreover, some pr

Method used

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  • Method for preparing nano-gamma-Fe2O3 hollow magnetic microsphere

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Experimental program
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Effect test

Embodiment 1

[0013] Weigh 0.30g of DBS into 100ml of deionized water, stir thoroughly for 30min, add 0.27g of ferric chloride and 0.20g of ferric sulfate, stir for a while, add 1.5g of urea and continue stirring. Then it was transferred into a 250ml three-hole bottle and refluxed at 100°C for 3h. The obtained precipitate was centrifuged, water-settled, and alcohol-settled, then put into an oven, and dried at 100°C;

[0014] Put the above powder into a muffle furnace for heat treatment at 300°C for 2 hours, then put it into a quartz tube furnace at 350°C H 2 Heat treatment under atmosphere for 2h, then slowly drop to 200°C in O 2 The final product can be obtained by heat treatment under atmosphere for 2 hours. The product is a hollow spherical structure composed of short nanorods with good crystallinity. The crystal phase composition of the product is as figure 1 shown.

Embodiment 2

[0016] Weigh 0.50g of DBS into 100ml of deionized water, stir thoroughly for 30min, add 0.27g of ferric chloride and 0.25g of ferric sulfate, stir for a while, add 1.8g of urea and continue stirring. Then it was transferred to a 250ml three-hole bottle and refluxed at 100°C for 5h. The obtained precipitate was centrifuged, washed with water, and washed with alcohol, and then put into an oven and dried at 100°C;

[0017] Put the above powder into a muffle furnace for heat treatment at 300°C for 2 hours, then put it into a quartz tube furnace at 350°C H 2 Heat treatment under atmosphere for 2h, then slowly drop to 200°C in O 2 The final product can be obtained by heat treatment under atmosphere for 3 hours. The product is a hollow spherical structure composed of short nanorods with good crystallinity.

Embodiment 3

[0019] Weigh 0.40g of DBS into 100ml of deionized water, stir thoroughly for 30min, add 0.27g of ferric chloride and 0.18g of ferric sulfate, stir for a while, add 1.40g of urea and continue stirring. Then it was transferred into a 250ml three-hole bottle and refluxed at 100°C for 2h. The obtained precipitate was centrifuged, washed with water, and washed with alcohol, and then put into an oven and dried at 100°C;

[0020] Put the above powder into a muffle furnace for heat treatment at 350°C for 1h, then put it into a quartz tube furnace at 300°C H 2 Heat treatment under atmosphere for 3h, then slowly lower to 180°C in O 2 The final product can be obtained by heat treatment under atmosphere for 3 hours. The product is a hollow spherical structure composed of short nanorods with good crystallinity.

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Abstract

The invention discloses a method for preparing gamma-Fe2O3 nanometer hollow magnetic microspheres, which comprises the following steps that: a certain quantity of sodium dodecylbenzenesulfonate (DBS) is added into 100ml of water, then a certain quantity of FeCl3.6H2O and Fe2(SO4)3 are added into the mixed liquid and stirred for 20 to 60 minutes, then urea is added into the mixed liquid, the mixed liquid is refluxed for 2 to 5 hours at a temperature of between 95 and 105 DEG C, and a precipitate is centrifugated, washed for a plurality of times, and dried at a temperature of 100 DEG C after alcohol being washed to produce an alpha-FeOOH precursor. The precursor is subject to heat treatment for 0.5 to 3 hours under an air atmosphere of between 250 and 400 DEG C, then the obtained product is subject to heat treatment for 1 to 3 hours under an H2 atmosphere of between 300 and 450 DEG C, finally the temperature is slowly decreased to between 150 and 250 DEG C, the atmosphere is changed from H2 to O2, and a final product is prepared after 1 to 3 hours of heat treatment. The product prepared by the method has high purity, definite compositions and crystal forms, and homogeneous hollow spherical structures.

Description

technical field [0001] The present invention relates to a method for preparing nanoparticles, especially for preparing gamma-Fe 2 o 3 A method for nanohollow magnetic microspheres. Background technique [0002] Recently, the preparation of nanomaterials with special structure or morphology has become a hot spot in the field of materials research. As a special nanostructure, hollow spherical nanomaterials can produce some peculiar microscopic "encapsulation" due to their low density and high specific surface properties, and their hollow parts can accommodate a large number of guest molecules or large-sized guests. , The nature of the "wrapping" effect has attracted people's attention. γ-Fe 2 o 3 It is a functional material with a wide range of applications. Due to its good magnetic, catalytic and gas-sensing properties and good absorption and shielding effects on ultraviolet rays, it is used as magnetic recording materials, magnetic liquids, electromagnetic wave absorpti...

Claims

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Application Information

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IPC IPC(8): C01G49/06
Inventor 李春忠王淑芬曹宏明顾锋胡彦杰
Owner EAST CHINA UNIV OF SCI & TECH
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