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Method for filling carbon nano tube with magnetic nano metal iron particles

A technology of carbon nanotubes and magnetic nanometers, which is applied in the field of preparation of nanocomposite materials, can solve the problems of complex process and low filling rate of nano-metal iron, and achieve high controllability, facilitate mass production, and simple and easy-to-operate methods Effect

Inactive Publication Date: 2009-06-17
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

The template method is also a method for filling magnetic nano-metal iron in carbon nanotubes [Boa JC, et al.Advanced Materials, 2002, 14(20): 1483]. This method first needs to synthesize a nano-sized template, and the reaction ends Finally, these templates must be removed, and the process is very complicated.
In addition, heating the mixture of carbon nanotubes and ferrocene under a nitrogen atmosphere can also fill nano-metal iron in carbon nanotubes [Lin HY, et al. Materials Letters, 2007, 61(16): 3547], but nano The filling rate of metallic iron is very low
Use wet chemical method to uniformly fill magnetic nano-metal iron particles in carbon nanotubes, fill magnetic nano-metal iron particles in carbon nanotubes with different structures with a diameter of 10-100 nanometers, and use carbon nanotubes with different diameters as templates to control magnetic properties The particle size of nano-metal iron particles and the preparation of magnetic nano-metal iron particles filled carbon nanotube composites have not yet been reported in literature and patents

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  • Method for filling carbon nano tube with magnetic nano metal iron particles
  • Method for filling carbon nano tube with magnetic nano metal iron particles
  • Method for filling carbon nano tube with magnetic nano metal iron particles

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Embodiment 1

[0030] (1) At room temperature, add 5g of carbon nanotubes with a diameter of 10-20 nanometers to 250ml of concentrated nitric acid (68%), ultrasonically disperse for 30 minutes, reflux in an oil bath at 125°C for 24 hours, and then reflux The temperature of the reaction mixture was reduced to 23°C, filtered with a 0.85μm filter membrane, washed with deionized water and filtered to a pH of 6.8 to obtain carbon nanotubes with functional groups such as carbonyl, hydroxyl, and carboxyl groups introduced on the surface, and dried at 60°C in the air Dry for 24 hours;

[0031] (2) Prepare ferrous sulfate into an aqueous solution with a concentration of 20%, and put the carbon nanotubes with carbonyl, hydroxyl, carboxyl and other functional groups on the surface obtained in step (1) into the ferrous sulfate aqueous solution, ultrasonically disperse for 30 minutes, and electromagnetically stir After 24 hours, filter with a filter membrane and dry in the air at 60°C for 12 hours to obtain ...

Embodiment 2

[0036] (1) At room temperature, add 4.5g of carbon nanotubes with a diameter of 20-40 nanometers to 200ml of concentrated nitric acid (68%), ultrasonically disperse for 30 minutes, reflux in an oil bath at 120°C for 20 hours, and then The temperature of the refluxing reaction mixture is lowered to 24℃, filtered with a 0.85μm filter membrane, washed with deionized water and filtered to a pH of 6.5 to obtain carbon nanotubes with carbonyl, hydroxyl, carboxyl and other functional groups introduced on the surface, in the air at 60℃ Dry for 24 hours;

[0037] (2) Prepare ferrous sulfate into an aqueous solution with a concentration of 25%, and put the carbon nanotubes with carbonyl, hydroxyl, carboxyl and other functional groups on the surface obtained in step (1) into the ferrous sulfate aqueous solution, ultrasonically disperse for 30 minutes, and electromagnetically stir After 24 hours, filter with a filter membrane and dry in the air at 60°C for 12 hours to obtain carbon nanotubes ...

Embodiment 3

[0042] (1) At room temperature, add 6g of carbon nanotubes with a diameter of 40-60 nanometers to 300ml of concentrated nitric acid (68%), ultrasonically disperse for 30 minutes, reflux in an oil bath at 130°C for 22 hours, and then reflux The temperature of the reaction mixture was reduced to 25℃, filtered with a 0.85μm filter membrane, washed with deionized water and filtered to a pH of 7, to obtain carbon nanotubes with carbonyl, hydroxyl, carboxyl and other functional groups introduced on the surface, and dried at 60℃ in the air Dry for 24 hours;

[0043] (2) Prepare ferrous sulfate into an aqueous solution with a concentration of 30%, and put the carbon nanotubes with carbonyl, hydroxyl, carboxyl and other functional groups on the surface obtained in step (1) into the ferrous sulfate aqueous solution, ultrasonically disperse for 30 minutes, and electromagnetically stir After 24 hours, filter with a filter membrane and dry in the air at 60°C for 12 hours to obtain carbon nanot...

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Abstract

The invention belongs to the technical field of preparation and application of nano composite material, and in particular relates to a method for preparing a magnetic nano metallic iron particle / carbon nano tube functional composite material. The invention discloses a method for filling a carbon nano tube with magnetic nano metallic iron particles. The method comprises the following steps: carrying out refluxing treatment on the carbon nano tube in concentrated nitric acid, introducing functional groups such as carbonyl, hydroxyl, carboxyl and the like on the surface of the carbon nano tube, carrying out ultrasonic dispersion and electromagnetic mixing on the treated carbon nano tube in aqueous solution of bivalent ferric salt, filling the bivalent ferric salt in the carbon nano tube through capillary action, thermally treating the carbon nano tube at inert atmosphere, decomposing the bivalent ferric salt filled inside the carbon nano tube into ferric oxide, and reducing the ferric oxide into the magnetic nano metallic iron particles by hydrogen to obtain the composite material for filling the magnetic nano metallic iron particles into the carbon nano tube, wherein the magnetic nano metallic iron particles can be filled in the carbon nano tubes the calibers of which are 10 to 100 nanometers and which have different structures, and the carbon nano tubes with different calibers as templates can accurately control the size of the magnetic nano metallic iron particles. The method has the advantages of simple process and good controllability, can make the magnetic nano metallic iron particles evenly filled in the carbon nano tube with high filling rate, and is convenient for industrialized production; and the prepared nano magnetic composite material has good application prospect in the fields of high-density magnetic recording materials, wave-absorbing materials, electromagnetic shielding materials, nuclear magnetic resonance imaging materials.

Description

Technical field [0001] The invention relates to a method for preparing nano composite materials, in particular to a method for filling carbon nanotubes with magnetic nano metal iron particles. Background technique [0002] Magnetic composite materials are widely used in the preparation of high-density magnetic recording materials for data storage, as well as in the preparation of absorbing materials, electromagnetic shielding materials, inks for electrophotographic printing, broadband domain transformers, noise filters, and medically directed heat collection treatment of tumors And targeted drug delivery. [0003] Since the discovery of carbon nanotubes, due to their many novel and unique characteristics, they have broad application prospects in many aspects, and researchers have paid great attention to them. Studies have shown that carbon nanotube composites prepared by filling carbon nanotubes exhibit more excellent physical and chemical properties, such as better optical prope...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F1/02
Inventor 赵东林李霞沈曾民
Owner BEIJING UNIV OF CHEM TECH
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