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Method for preparing nanometer particles of nickel-carbide nickel core-shell structure

A nanoparticle, core-shell structure technology, applied in the field of preparation of magnetic nanoparticles, can solve the problems of uneven nanochains, thick shell thickness, serious problems, etc.

Inactive Publication Date: 2015-07-01
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, nickel nanoparticles with different crystal forms have been synthesized, such as fcc-Ni, hcp-Ni, and Ni3C, but there are few reports on the synthesis of Ni-Ni3C core-shell structure, Zhang et al. (Nano Lett.2008, 8, 1147 -1152) reported one-dimensional nickel-nickel carbide core-shell nanochains, using a chemical liquid phase method to synthesize particles between 30 and 50 nm in one step, with a shell thickness between 1 and 4 nm. The coercive force of the chain is enhanced compared with that of a single nickel nanowire, but the synthetic core-shell nanochain is not uniform, serious agglomeration occurs, and the thickness of the shell is thicker.

Method used

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  • Method for preparing nanometer particles of nickel-carbide nickel core-shell structure
  • Method for preparing nanometer particles of nickel-carbide nickel core-shell structure
  • Method for preparing nanometer particles of nickel-carbide nickel core-shell structure

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Example 1 A method for preparing nickel-nickel carbide core-shell nanoparticles, comprising the following steps:

[0034] (1) Mix the nickel precursor compound, octadecene and alkylamine uniformly to obtain the mixed solution A.

[0035] Wherein: the molar volume ratio of nickel precursor compound to octadecene is 0.5mmol:4mL, and the molar volume ratio of nickel precursor compound to alkylamine is 0.5mmol:0.6mL.

[0036] The precursor compound of nickel refers to nickel acetylacetonate.

[0037] Alkylamine refers to cetylamine.

[0038] (2) Stir the mixed solution A with inert gas argon at a flow rate of 40mL / min at room temperature for 10 minutes, then raise the temperature to 120°C, then inject trioctylphosphine into the mixed solution A under the protection of argon, and mix well to form Mixture B, that is, the ligand compound of nickel.

[0039] Wherein: the molar ratio of trioctylphosphine to nickel precursor compound is 1:1.

[0040] (3) After mixing octad...

Embodiment 2

[0047] Example 2 A method for preparing nickel-nickel carbide core-shell nanoparticles, comprising the following steps:

[0048] (1) Mix the nickel precursor compound, octadecene and alkylamine uniformly to obtain the mixed liquid A.

[0049] Wherein: the molar volume ratio of nickel precursor compound to octadecene is 1.5mmol:6mL, and the molar volume ratio of nickel precursor compound to alkylamine is 1.5mmol:1.2mL.

[0050] The precursor compound of nickel refers to nickel acetylacetonate.

[0051] Alkylamine refers to dodecylamine.

[0052] (2) Mixed solution A is stirred at room temperature with inert gas argon at a flow rate of 60mL / min for 20 minutes, then heated to 140°C, and then injected trioctylphosphine into mixed solution A under the protection of argon, and mixed evenly to form Mixture B, that is, the ligand compound of nickel.

[0053] Wherein: the molar ratio of the precursor compound of trioctylphosphine to nickel is 3:1.

[0054] (3) After mixing oct...

Embodiment 3

[0061] Example 3 A method for preparing nickel-nickel carbide core-shell nanoparticles, comprising the following steps:

[0062] (1) Mix the nickel precursor compound, octadecene and alkylamine uniformly to obtain the mixed liquid A.

[0063] Wherein: the molar volume ratio of the nickel precursor compound to octadecene is 1 mmol: 5 mL, and the molar volume ratio of the nickel precursor compound to alkylamine is 1 mmol: 0.9 mL.

[0064] The precursor compound of nickel refers to nickel acetylacetonate.

[0065] Alkylamine refers to oleylamine.

[0066] (2) Stir the mixed solution A with inert gas argon at a flow rate of 50mL / min at room temperature for 15 minutes, then raise the temperature to 130°C, then inject trioctylphosphine into the mixed solution A under the protection of argon, and mix well to form Mixture B, that is, the ligand compound of nickel.

[0067] Wherein: the molar ratio of trioctylphosphine to nickel precursor compound is 2:1.

[0068] (3) After mi...

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Abstract

The invention relates to a method for preparing nanometer particles of a nickel-carbide nickel core-shell structure. The method includes the following steps of firstly, evenly mixing nickel precursor compounds, octadecene and alkylamine to obtain mixed liquid A; secondly, injecting trioctylphosphine into the mixed liquid A under the protection of argon, and evenly mixing the trioctylphosphine with the mixed liquid A to obtain mixed liquid B; thirdly, after mixing the octadecene with the alkylamine, injecting inert gas argon into the mixture of the octadecene and the alkylamine and conducting stirring at the room temperature, injecting the trioctylphosphine and evenly conducting mixing to obtain mixed liquid C; fourthly, keeping the temperature of the mixed liquid B and packing the mixed liquid B into an injection pump; fifthly, continuously injecting the mixed liquid B into the heated mixed liquid C to react to obtain a solution of the nanometer particles of the nickel-carbide nickel core-shell structure; sixthly, cooling the solution of the nanometer particles of the nickel-carbide nickel core-shell structure, adding absolute ethyl alcohol into the solution, conducting centrifugal separation to obtain sediments, sequentially conducting washing, centrifugal separation and vacuum drying on the sediments until the weight of the sediments is constant, and then obtaining the nanometer particles of the nickel-carbide nickel core-shell structure. By means of the method, the thickness, the shape and the appearance of a shell can be controlled.

Description

technical field [0001] The invention relates to the preparation of a magnetic nano particle, in particular to a preparation method of a nickel-nickel carbide core-shell nano particle. Background technique [0002] Compared with bulk materials, metal nanomaterials exhibit unique electrical, optical, magnetic and chemical properties, which are mainly due to their surface effects, volume effects and quantum size effects. widespread attention. However, due to the high activity of the surface layer of metal particles, they are prone to agglomeration and are easily oxidized when exposed to the air, especially the magnetic metal nickel nanoparticles are more likely to be oxidized in the air, which greatly limits their performance and application range. If the magnetic metal nanoparticles are coated with an inactive layer to form a core-shell structure, the magnetic properties of the inner metal particles will not be significantly affected, and at the same time, the problem of easy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F1/02B22F9/24B82Y40/00
Inventor 佘厚德魏娟娟雷自强
Owner NORTHWEST NORMAL UNIVERSITY
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