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Method for preparing magnetic metal-metal core-shell nano particles

A magnetic metal nanometer and magnetic metal technology, applied in the coating and other directions, can solve the problems of low cladding rate, easy nucleation of shell metal, and difficulty in controlling the formation of shell metal. Wide, ensure the effect of effective coating

Active Publication Date: 2013-03-27
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of preparing core-shell magnetic metal nanoparticles by the aqueous phase method is that the magnetic metal salt is easily reduced and the reaction temperature is low, but due to the fast reduction speed, the size and shape of the nanoparticles are difficult to control, and the shell metal is easy to nucleate alone , the coverage rate is not high
If the organic liquid phase method is used, it is easy to prepare nanoparticles with relatively uniform size and good crystallization, but the generation control of the shell metal is a difficult point.
At present, there are still reports on the preparation of gold-coated magnetic metal nanoparticles with obvious core-shell structure by organic liquid phase method.

Method used

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  • Method for preparing magnetic metal-metal core-shell nano particles
  • Method for preparing magnetic metal-metal core-shell nano particles
  • Method for preparing magnetic metal-metal core-shell nano particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 0.5mmol nickel acetylacetonate and 6ml oleylamine into a three-necked flask, stir and mix under the protection of argon, then add a mixture of 0.012mmol chloroauric acid and 0.3ml anisole into the three-necked flask, stir for 10min and then heat to Hold at 50°C for 10 minutes, then heat to 200°C, hold for 20 minutes, and then cool to 150°C. Quickly inject a mixture of 0.5mmol of the pre-prepared gold organic compound and 2ml of chloroform, keep it at 140°C for 30 minutes and then cool it naturally, add acetone to precipitate the nanoparticles, take out the reaction mother liquor by centrifugation, and then use a mixed solution of ethanol, acetone and n-hexane Repeated washing, centrifugation three times, and finally vacuum drying to obtain a powder product. The electron micrograph and energy spectrum are as shown figure 1 with figure 2 Shown.

Embodiment 2

[0035] Add 0.5mmol nickel acetylacetonate and 6ml oleylamine into a three-necked flask, stir and mix under the protection of argon, then add a mixture of 0.012mmol chloroauric acid and 0.3ml ethanol into the three-necked flask, stir for 10min and then raise the temperature to 50℃ , Keep for 10min, then heat up to 200℃, keep for 20min, then cool to 150℃. Quickly inject a mixture of 0.5mmol of pre-prepared gold organic compound and 2ml of chloroform, keep it at 130°C for 30 minutes and then cool it naturally, add acetone to precipitate the nanoparticles, take out the reaction mother liquor by centrifugation, and then use a mixed solution of ethanol, acetone and n-hexane Repeated washing, centrifugation for 3 times, and finally vacuum drying to obtain a powder product. The electron microscope picture is as follows image 3 As shown, its energy spectrum and figure 2 similar.

Embodiment 3

[0037] Add 0.5mmol nickel acetylacetonate, 5ml oleylamine, 2ml dodecylamine into a three-necked flask, stir and mix under the protection of argon, then add a mixture of 0.012mmol chloroauric acid and 0.3ml toluene into the three-necked flask, and stir for 10min Then the temperature was raised to 50°C, the temperature was kept for 10 minutes, then the temperature was raised to 210°C, the temperature was kept for 20 minutes, and then it was cooled to 150°C. Quickly inject a mixture of 0.3mmol of the pre-prepared gold organic compound and 3ml of chloroform, keep it at 130°C for 30 minutes and then cool it naturally, add acetone to precipitate the nanoparticles, take out the reaction mother liquor by centrifugation, and then use a mixed solution of ethanol, acetone and n-hexane Repeated washing, centrifugation for three times, and finally vacuum drying to obtain a powder product. The electron microscope image is as follows Figure 4 As shown, its energy spectrum and figure 2 simila...

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Abstract

The invention discloses a method for preparing magnetic metal-metal core-shell nano particles, which relates to metal nano particles. The method comprises: dissolving chloroauric acid and triphenylphosphine in ethanol respectively, filtering, cleaning, drying, obtaining an organic compound formed by gold and triphenylphosphine, mixing the organic compound with alkylamine, obtaining solution A, mixing an organic solvent A with a noble metal salt, adding mixed solution A, rising the temperature to perform a reaction, cooling and obtaining magnetic metal nano particles; dissolving the obtained organic compound formed by gold and triphenylphosphine in an organic solvent B, injecting obtained magnetic metal nano particles, keeping the temperature between 120 and 160 DEG C for 20 minutes to 1 hour, reducing to obtain gold and wrapping gold on the formed magnetic metal nano particles and obtaining nano particles in which gold and magnetic metal are in a core-shell structure; and washing the nano particles in which gold and magnetic metal are in a core-shell structure, performing centrifugal separation, drying and obtaining powder product, namely magnetic metal-gold core-shell nano particles.

Description

Technical field [0001] The invention relates to a metal nano particle, in particular to a preparation method of a magnetic metal-gold core-shell type nano particle. Background technique [0002] Metal nanoparticles are gradually valued due to their small size, large specific surface area, and excellent properties that conventional bulk materials cannot match. However, their surface activity is high, they are easy to agglomerate, and are easily oxidized in the air, especially magnetic metals (Fe , Co, Ni) nanoparticles are more easily oxidized in the air, which greatly limits their performance and application range. If the inert layer covers the magnetic metal nanoparticles to form a core-shell structure, the oxidation problem of the nanoparticles can be solved, and the magnetic properties of the particles will not be significantly affected. Therefore, it is particularly important to prepare magnetic metal nanoparticles with a core-shell structure. [0003] As a precious metal, go...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24B22F1/02
Inventor 陈远志陈小真佘厚德彭栋梁岳光辉
Owner XIAMEN UNIV
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