Preparation method of nano-particle assembled flower-shaped iron sub-micron particles

A technology of submicron particles and nanoparticles, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of wide particle size distribution, easy aggregation of iron particles, low energy utilization rate, etc. Achieve the effect of good stability, low heat treatment temperature and low cost

Active Publication Date: 2018-06-29
YANSHAN UNIV
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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing flower-shaped elemental iron submicron particles assembled by nanoparticles with simple operation, high safety factor and large-scale production, so as to solve the existing main method for preparing elemental iron particles assembled by nanometers— Liquid phase and gas phase methods have the problems of easy agglomeration of iron particles, wide particle size distribution, and low energy utilization

Method used

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  • Preparation method of nano-particle assembled flower-shaped iron sub-micron particles
  • Preparation method of nano-particle assembled flower-shaped iron sub-micron particles
  • Preparation method of nano-particle assembled flower-shaped iron sub-micron particles

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Embodiment 1

[0020] Dissolve 1.20g of ferric chloride hexahydrate, 5.40g of urea and 7.20g of tetrabutylammonium bromide in 180ml of ethylene glycol under mechanical stirring to obtain an orange-yellow solution; heat the above solution to reflux at 180°C After 45 minutes, cool naturally to room temperature; centrifuge the cooled solution to separate the green precipitate, wash the green precipitate 3 times with absolute ethanol, and dry it in vacuum at 60°C to obtain a light green powder; place the prepared light green powder in In the quartz boat, put it into the temperature-controlled area of ​​the tube furnace quartz tube, heat treatment at 400°C for 2.0 hours in an air atmosphere, pass argon gas into the tube furnace quartz tube for 1.0 hour, and then inject it into the tube furnace quartz tube Introduce the mixed gas of argon and hydrogen, the volume ratio of argon and hydrogen in the mixed gas is 10:3, and keep warm at 400°C for 2 hours under the mixed atmosphere, and cool to room tem...

Embodiment 2

[0026] Dissolve 1.20g of ferric chloride hexahydrate, 2.70g of urea and 3.60g of tetrabutylammonium bromide in 180ml of ethylene glycol under mechanical stirring to obtain an orange-yellow solution; heat the above solution to reflux at 150°C After 30 minutes, cool naturally to room temperature; centrifuge the cooled solution to separate the green precipitate, wash the green precipitate 4 times with absolute ethanol, and dry it in vacuum at 60°C to obtain a light green powder; place the prepared light green powder in In the quartz boat, put it into the temperature-controlled area of ​​the tube furnace quartz tube, heat treatment at 400°C for 2.0 hours in an air atmosphere, pass argon gas into the tube furnace quartz tube for 1.0 hour, and then inject it into the tube furnace quartz tube Introduce a mixture of argon and hydrogen, the volume ratio of argon and hydrogen in the mixture is 10:3, and keep warm at 400°C for 3 hours under the mixed atmosphere, and cool to room temperatu...

Embodiment 3

[0028] Dissolve 1.20g of ferric chloride hexahydrate and 5.40g of urea in 180ml of ethylene glycol under mechanical stirring to obtain an orange-yellow solution; heat the above solution to 195°C and reflux for 60 minutes, and naturally cool to room temperature; The cooled solution was centrifuged to separate the green precipitate, washed with absolute ethanol for 3 times, and vacuum-dried at 60°C to obtain a light green powder; the prepared light green powder was placed in a quartz boat and placed in a tube In the temperature-controlled area of ​​the furnace quartz tube, heat treatment at 400°C for 2.0 hours in an air atmosphere, pass argon into the tube furnace quartz tube for 1.0 hour, and then pass a mixture of argon and hydrogen into the tube furnace quartz tube , the volume ratio of argon and hydrogen in the mixed gas is 10:3, and it is kept at 400°C for 4 hours under the mixed atmosphere, and cooled to room temperature with the furnace under the argon atmosphere, and the ...

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Abstract

The invention discloses a preparation method of nano-particle assembled flower-shaped iron sub-micron particles. The preparation method mainly comprises the following steps: first, obtaining a morphology and particle size controllable intermediate product by heating and refluxing a solution which is obtained by dissolving ferric trichloride hexahydrate, urea and tetrabutylammonium bromide into ethylene glycol; and then, performing heat treatment at 400 DEG C to obtain three-dimensional flower-shaped iron particles with uniform particle size distribution and good dispersivity. According to thepreparation method of the nano-particle assembled flower-shaped iron sub-micron particles, equipment and a process are simple; the method is safe and reliable; the heat treatment temperature is low; the obtained iron particles are controllable in morphology and uniform in particle size distribution; the particle sizes of three-dimensional flower-shaped structures are about 2.0 mu m; the flower-shaped structures are formed by assembling nano-rod-shaped structures of about 30 nm; the specific surface area is large; the saturation magnetization intensity and the coercive force are high; and the three-dimensional flower-shaped structures can be applied to the aspects, such as magnetic recording, electromagnetic wave absorption, catalysis and the like.

Description

technical field [0001] The invention belongs to the field of material technology, in particular to a method for preparing elemental iron submicron particles. Background technique [0002] Chemical composition is one of the main factors that determine the properties of materials. When the particle size is reduced to micronano, its microstructure and morphology also play an important role in its properties. The excellent performance of many nanomaterials in a certain field is determined by the particularity of their structure and morphology. The flower-shaped iron submicron particles assembled by nanoparticles can increase its magnetic anisotropy, enhance its electromagnetic properties, and improve its stability. It has a wide range of potential applications in industries such as electronics, life sciences, environmental protection, and machinery. [0003] The preparation methods of iron particles assembled from nanoparticles mainly include liquid phase method and gas phase ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/22B22F1/00B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00B22F9/22B22F1/0553B22F1/07B22F1/054
Inventor 李雪爱曲项燕郭万春王海燕
Owner YANSHAN UNIV
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