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Preparation method of ammonia-gas-free carbon-coated iron nitride nanopowder

A technology of nano-iron and nano-iron powder, which is applied in the direction of nitrogen-metal/silicon/boron binary compounds, can solve the problems of large ammonia consumption, long production time, environmental pollution, etc., and achieve simple equipment, environment-friendly, cost reduction effect

Inactive Publication Date: 2013-10-23
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the currently published patents and documents, most of the processes for preparing iron nitride powder or particles are based on the principle of gas nitriding of traditional steel, that is, using ammonia (NH 3 ) or ammonia (NH 3 ) and hydrogen (H 2 ) mixed gas, there are problems such as long production time, large ammonia consumption, high cost and environmental pollution

Method used

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  • Preparation method of ammonia-gas-free carbon-coated iron nitride nanopowder
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  • Preparation method of ammonia-gas-free carbon-coated iron nitride nanopowder

Examples

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Comparison scheme
Effect test

Embodiment 1

[0020] Example 1 Preparation of carbon-coated iron nitride nanopowder

[0021] Proceed as follows:

[0022] 100ml of acrylonitrile and 6g of itaconic acid were used as comonomers for polymerization, with 0.76g of azobisisobutyronitrile as an initiator and 260ml of DMSO as a solvent, at a constant temperature of 60°C for 24 hours, and the polymerization was completed to obtain a polyacrylonitrile solution. Add iron powder with a particle size of 50-200nm into the PVP aqueous solution with a concentration of 0.016g / ml under air-isolated conditions (the amount of the solution is based on completely submerging the nano-iron powder), and perform surface modification treatment for 10 minutes. The nanometer iron powder was dried and added to the polyacrylonitrile solution prepared above, and the mass ratio of iron powder to polyacrylonitrile was 0.4:1. Ultrasonic dispersion was used for 2 hours, and an appropriate amount of mixed solution was taken to form a film with a glass sheet,...

Embodiment 2

[0023] Example 2 Preparation of carbon-coated iron nitride nanopowder

[0024] Proceed as follows:

[0025] 100ml of acrylonitrile and 6g of itaconic acid were used as comonomers for polymerization, with 0.76g of azobisisobutyronitrile as an initiator and 260ml of DMSO as a solvent, at a constant temperature of 60°C for 24 hours, and the polymerization was completed to obtain a polyacrylonitrile solution. Add iron powder with a particle size of 50-200nm into oleic acid under air-isolated conditions (the amount of oleic acid is based on completely submerging the nano-iron powder), perform surface modification treatment for 20 minutes, and dry the nano-iron powder after treatment. Then add it to the polyacrylonitrile solution, the mass ratio of iron powder to polyacrylonitrile is 0.6:1. Stir mechanically for 2 hours, take an appropriate amount of mixed solution, press it on a glass sheet, wash and solidify with deionized water at 65°C, dry at 100°C, and grind to obtain the prec...

Embodiment 3

[0026] Example 3 Preparation of carbon-coated iron nitride nanopowder

[0027] Proceed as follows:

[0028] 100ml of acrylonitrile and 6g of itaconic acid were used as comonomers for polymerization, with 0.76g of azobisisobutyronitrile as an initiator and 260ml of DMSO as a solvent, at a constant temperature of 60°C for 24 hours, and the polymerization was completed to obtain a polyacrylonitrile solution. Add iron powder with a particle size of 50-200nm into oleic acid under air-isolated conditions (the amount of oleic acid is based on completely submerging the nano-iron powder), perform surface modification treatment for 30 minutes, and dry the nano-iron powder after treatment. Then add it to the polyacrylonitrile solution, the mass ratio of iron powder to polyacrylonitrile is 0.5:1. Use ultrasonic dispersion for 30 minutes, mechanical stirring for 30 minutes, take an appropriate amount of mixed liquid, press it on a glass sheet, wash and solidify with deionized water at 60°...

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Abstract

The invention discloses a preparation method of ammonia-gas-free carbon-coated iron nitride nanopowder. The preparation method comprises the following steps of: uniformly dispersing iron nanopowder in a nitrogenous high polymer solution, cleaning the iron nanopowder by using water and then carrying out solidification treatment to obtain a composite precursor; then, carrying out oxidation treatment on the precursor or not, and then, continuously raising the temperature from room temperature to 500-800 DEG C at the temperature rise speed of 4-20 DEG C / min at a high-pure nitrogen or argon atmosphere to obtain the carbon-coated iron nitride nanopowder, wherein ammonia gas is not needed in the whole process. The reaction principle is as follows: the carbon-coated iron nitride nanopowder is produced through reaction between active nitrogen atoms released in the process of treating nitrogenous high polymers at the high temperature of 500-800 DEG C and iron nanopowder subjected to surface treatment. High-pure nitrogen or argon is adopted to replace ammonia gas in the treatment process, and long-term heat insulation is not needed, so that the production time is shortened, the cost is reduced, and the preparation method has the advantages of simple equipment and environment friendliness.

Description

technical field [0001] The invention relates to a preparation method of carbon-coated iron nitride nano powder without ammonia gas, and belongs to the nano material preparation technology and field. Background technique [0002] Carbon-coated magnetic nanopowders or particles, as a new class of magnetic nanocomposites, have received extensive attention from researchers. So far, the methods for synthesizing carbon-coated magnetic metal nanopowders include arc discharge method, chemical vapor deposition method, pyrolysis method, energy concentration method and explosion method, etc. Although each method has advantages and disadvantages, most of these methods require Higher energy and complex experimental devices lead to cumbersome experimental operations and higher costs, which are greatly limited in practical applications. Carbon-coated iron nitride is a magnetic material with important application value and potential in magnetic recording, ferrofluid, biosensors, targeted d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/06C04B35/58C04B35/622
Inventor 于美杰王成国吕宇鹏白玉俊高瑞
Owner SHANDONG UNIV