Nitrogen-doped and carbon-coated magnetic nanoparticle composite microspheres and preparation method thereof

A technology of magnetic nanoparticles and nitrogen-doped carbon, which is applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve problems such as complex synthesis technology, and achieve easy reunion, absorption frequency bandwidth, Effects that are easy to prepare in large quantities

Active Publication Date: 2018-12-18
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0005] Aiming at the complex synthesis technology of binary and multi-component composite wave-absorbing materials, the present invention proposes a time-saving, high-efficiency, green and environmentally friendly method for preparing nitrogen-doped carbon-coated magnetic nanoparticle composite microspheres; Layer-coated nitrogen-containing organic monomers, and then calcined in a protective atmosphere to obtain composite microspheres with a core-shell structure; and by adjusting the mass ratio of glycerol metal precursors and nitrogen-containing organic monomers, the electromagnetic parameters of the composite material can be regulated, Make it meet the requirements of impedance matching and absorption characteristics, and prepare composite microspheres with excellent microwave absorption performance

Method used

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  • Nitrogen-doped and carbon-coated magnetic nanoparticle composite microspheres and preparation method thereof
  • Nitrogen-doped and carbon-coated magnetic nanoparticle composite microspheres and preparation method thereof
  • Nitrogen-doped and carbon-coated magnetic nanoparticle composite microspheres and preparation method thereof

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Embodiment 1

[0030] Step 1: Measure 15ml of glycerin into a beaker filled with 85ml of isopropanol, and stir well. Weigh 0.404g Fe(NO) 3 9H 2 O was added to the above solution, stirred under ultrasonic conditions for 10 min, then poured into a reaction kettle, and reacted at a reaction temperature of 200° C. for 12 h. After the reaction, the product was centrifuged and washed with alcohol several times, and the washed solid product was dried in an oven at a drying temperature of 70°C to finally obtain the iron glycerol precursor.

[0031] Step 2: Dissolve 1.0g of PEG-800 in 100ml of water, transfer the solution into a 250ml three-necked flask, then weigh 0.1g of the iron glycerol precursor in step 1 and add it into it, and continue stirring for 1h until the formation of Uniform suspension; slowly inject 0.1g of pyrrole into the above system, and after stirring for 1h, slowly add 15ml of 0.2mol / L FeCl prepared in advance dropwise 3 Solution, continue to react for 2h, after the reaction i...

Embodiment 2

[0036] Step 1: Measure 5ml of glycerin into a beaker filled with 25ml of isopropanol, and stir well. Weigh 0.200g of cobalt oxalate and add it to the above solution, stir for 10 minutes under ultrasonic conditions, pour it into a reaction kettle, and react at a reaction temperature of 120° C. for 16 hours. After the reaction, the product was centrifuged and washed with alcohol several times, and the washed solid product was dried in an oven at a drying temperature of 60°C to finally obtain the cobalt glycerol precursor.

[0037] Step 2: Measure 0.5g of polyvinylpyrrolidone (PVP) and dissolve it in 100ml of water, transfer the solution into a 250ml three-neck flask, then weigh 0.15g of the iron glycerol precursor in step 1 and add it, and continue stirring under ultrasonic conditions 0.5h until a uniform suspension is formed; slowly inject 0.15g of aniline into the above system, and after stirring for 2h, slowly add 10ml of 0.1mol / L ammonium persulfate solution prepared in adva...

Embodiment 3

[0039] Step 1: Measure 25ml of glycerin into a beaker filled with 200ml of isopropanol, and stir well. Weigh 0.5g of ferric nitrate and 0.5g of cobalt nitrate and add to the above solution, stir for 10min under ultrasonic conditions, pour into the reaction kettle, and react at the reaction temperature of 160°C for 6h. After the reaction, the product was centrifuged and washed with alcohol several times, and the washed solid product was dried in an oven at a drying temperature of 80°C to finally obtain the iron-cobalt glycerol precursor.

[0040] Step 2: Take 2.0g of cetyltrimethylammonium bromide (CTAB) and dissolve it in 100ml of water, transfer the solution into a 250ml three-neck flask, then weigh 0.2g of the glycerol iron cobalt precursor in step 1 and add it , under ultrasonic conditions, continue to stir for 1.5h to form a uniform suspension; slowly inject 0.4g of pyrrole into the above system, and after stirring for 1h, slowly add 15ml of 0.4mol / L hydrogen peroxide solu...

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Abstract

The invention provides a nitrogen-doped and carbon-coated magnetic nanoparticle composite microspheres and a preparation method thereof, and belongs to the technical field of materials with an electromagnetic function. According to the method, a glycerin metal complex and a nitrogenous organic compound are taken as main raw materials. A monodispersed glycerin metal complex precursor is prepared according to a self-template method at first; then the surface of the precursor is coated to form a shell by virtue of in-situ polymerization for nitrogenous organic monomers, and a carbon source and anitrogen source are introduced; and finally, calcining is carried out under an inert gas, and a core is subjected to thermal decomposition to form magnetic nanoparticles while the shell is carbonizedto form nitrogen-doped carbon. The nitrogen-doped and carbon-coated magnetic nanoparticle composite microspheres are green and environment-friendly, and efficient and time-saving in preparation process, and suitable for being prepared in a large scale; the electromagnetic parameters of the composite microspheres and the sizes of the magnetic nanoparticles can be regulated and controlled by changing the mass ratio of metal salt to the nitrogenous organic monomers, and an annealing temperature, so that impedance matching and attenuation characteristic are achieved; and the prepared composite microspheres are high in absorption intensity for electromagnetic wave, wide in effective absorption frequency band, easy to prepare in a large scale, and capable of meeting many use needs.

Description

technical field [0001] The invention belongs to the technical field of electromagnetic functional materials, and relates to the preparation technology of carbon materials and magnetic particles, in particular to a preparation method of nitrogen-doped carbon-coated magnetic nanoparticle composite microspheres. Background technique [0002] With the rapid development of modern military technology and microwave communication technology, electromagnetic absorbing materials have attracted more and more attention. In the military field, as the basis of stealth technology, microwave-absorbing materials have greatly improved the survival, penetration and deep strike capabilities of weapon systems in modern warfare; at the same time, in communications, electronics, and medical industries, electromagnetic waves are increasingly used. The resulting electromagnetic pollution seriously threatens human health and the ecological environment. By coating the surface of weaponry or electroni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/30B22F1/00B22F1/02B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00B22F9/30B22F1/054B22F1/16
Inventor 陈平郭翔贾彩霞邱红芳杨森王琦
Owner DALIAN UNIV OF TECH
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