Method for preparing chemical and magnetic ordered-phase nanoparticles

A magnetic nanoparticle and nanoparticle technology, which is applied in the manufacture of inductors/transformers/magnets, electrical components, circuits, etc., can solve the problems of increasing process steps and increasing the preparation cost, and achieves the advantages of avoiding agglomeration, low cost and good application prospects. Effect

Inactive Publication Date: 2016-03-30
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method is beneficial to prevent the agglomeration and growth of nanoparticles, it increases the process steps and increases the preparation cost.
In addition, some researchers use the subsequent heat treatment process of salt bed, but it is still necessary to first prepare nanoparticles by high temperature pyrolysis.

Method used

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  • Method for preparing chemical and magnetic ordered-phase nanoparticles
  • Method for preparing chemical and magnetic ordered-phase nanoparticles
  • Method for preparing chemical and magnetic ordered-phase nanoparticles

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Take 1mol NaCl, after drying in a vacuum drying oven, add 25ml of n-heptane and put it into a planetary ball mill for ball milling for 2 days to obtain NaCl powder with a particle size below 20 microns;

[0036] (2) the iron acetylacetonate of 0.75mmol and the platinum acetylacetonate of 0.5mmol are mixed with the NaCl powder that step (1) obtains together for 10h;

[0037] (3) Take out the mixed powder and dry it and put it into the ark, and then place it in a tube annealing furnace for calcination. The tube annealing furnace first uses Ar gas to remove the air, and then feeds Ar and H during heating. 2 Mixed gas of Ar and H 2 The volume percentage is 95:5, the mixed gas flow rate is 10ml-400ml / min, the temperature rise rate is controlled at 10°C / min, the temperature is raised to 750°C and then kept for 1 hour, and after the heat preservation is completed, it is cooled to room temperature under the protection of the atmosphere to obtain the calcined product ;

[...

Embodiment 2

[0041] (1) Take 1mol NaCl, after drying in a vacuum drying oven, add 25ml of n-heptane and put it into a planetary ball mill for ball milling for 2 days to obtain NaCl powder with a particle size below 20 microns;

[0042] (2) the iron acetylacetonate of 1mmol and the platinum acetylacetonate of 0.5mmol are mixed with the NaCl powder that step (1) obtains together for 10h;

[0043](3) Take out the mixed powder and dry it and put it into the ark, and then place it in a tube annealing furnace for calcination. The tube annealing furnace first uses Ar gas to remove the air, and then feeds Ar and H during heating. 2 Mixed gas of Ar and H 2 The volume percentage is 95:5, the mixed gas flow rate is 10ml-400ml / min, the temperature rise rate is controlled at 10°C / min, the temperature is raised to 650°C and then kept for 1 hour, and after the heat preservation is completed, it is cooled to room temperature under the protection of the atmosphere to obtain the calcined product ;

[0044...

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Abstract

The invention provides a method for preparing chemical and magnetic ordered-phase nanoparticles through a one-step solid-phase high-temperature sintering process. The method comprises the steps that a large amount of solid dispersing agent powder, such as NaCl and KCl, which can be dissolved in water easily and metal precursor powder are evenly mixed; high-temperature calcination is directly conducted on the mixed powder for the thermal decomposition reaction, so that other elements, except metal elements, in a precursor are removed; and the calcination temperature is controlled to be higher than the magnetic ordered-phase forming temperature, so that crystal-phase growth of prepared nanoparticles is promoted by using dispersing agents as carriers, and thus the chemical and magnetic ordered-phase nanoparticles are obtained. Compared with an existing preparation technique that chemical and magnetic ordered-phase nanoparticles can be obtained only after annealing of chemical disorder nanoparticles synthetized in liquid-phase mode, by the adoption of the method, the chemical and magnetic ordered-phase nanoparticles can be obtained through one-step synthesis without the annealing process, phenomena of agglomeration and growth of the nanoparticles in the high-temperature calcinations are avoided, and the method has good application prospects.

Description

technical field [0001] The invention belongs to the technical field of magnetic nanoparticle preparation, and in particular relates to a preparation method of chemically and magnetically ordered phase nanoparticle. Background technique [0002] At present, the mainstream method for preparing magnetic metal nanoparticles is the high-temperature liquid-phase chemical synthesis method. This method is to dissolve the metal precursor in the reaction solvent, add a dispersant, etc., mix uniformly, and heat up in a liquid-phase environment for chemical thermal decomposition. reaction, followed by centrifugation to separate the liquid phase to obtain magnetic nanoparticles, which are then annealed. For example, Sun, S. et al reported in the following documents 1 and 2 that in a certain reaction solvent, oleic acid and oleylamine were used as surfactants to prepare FePt monodisperse nanoparticles by thermally decomposing various metal salts. method. [0003] Document 1: Sun S. etal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/22H01F41/02
Inventor 杜娟边宝茹何江海夏卫星张健闫阿儒刘平
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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