Preparation method of nickel nanopowder

A technology of nano-nickel powder and nickel salt, which is applied in the field of liquid-phase chemical reduction preparation of nano-nickel powder, which can solve the problems of difficulty in controlling the particle size and shape of the liquid-phase reduction method, difficulty in realizing industrial production, and difficulty in preparing carbon-based nickel. , to achieve the effect of simple and easy-to-control preparation method, stable production quality and good dispersibility

Active Publication Date: 2014-08-06
YUCHEN ADVANCED ENERGY MATERIALS & TECH WUXI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The physical vapor deposition method is obtained by volatilizing or ionizing the metal nickel target by physical methods in a vacuum environment, and then controlling a certain condensation speed. It is characterized by simple process, easy operation, and no pollution of three wastes; High energy consumption, complex equipment, high technical requirements, and high cost, so it is difficult to realize industrial production
[0005] The chemical vapor deposition method uses carbon-based nickel as a raw material, and decomposes to obtain nano-nickel powder under a certain temperature and pressure. The production efficiency of the chemical vapor deposition method is high, and it is suitable for large-scale industrial production. The preparation of nickel is difficult, the nano-powder is difficult to collect, and the equipment requirements of the process are high.
[0006] The liquid-phase chemical reduction method uses nickel salt as the raw material such as hydrazine hydrate as the reducing agent to prepare nickel powder in the solution. The preparation of nano-nickel powder by the liquid-phase reduction method has the advantages of simple process, small equipment investment and high production efficiency, and is suitable for industrial scale. The production of nano-nickel powder, but the liquid phase reduction method is difficult to control in terms of particle size and shape

Method used

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  • Preparation method of nickel nanopowder
  • Preparation method of nickel nanopowder

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Embodiment 1

[0031] A preparation method of nano nickel powder, comprising:

[0032] (1) 0.075molNiCl 2 Dissolve 5g of PVP in water and mix evenly, then add 0.015mol of ammonia water and stir thoroughly to obtain 500ml of A solution; mix 0.5mol of N 2 h 4 ·H 2 O, 0.01mol sodium borohydride and 2.0mol NaOH are miscible in water to obtain 500ml B liquid;

[0033] (2) Heat liquid A to 90°C, add liquid B to liquid A, the feeding time is 30min, the temperature of the reaction system is maintained at 90°C and react for 50min, then add cold water to cool to room temperature (10-30°C); the reaction product is centrifuged Separation, the filter cake is washed with water to remove impurities in the filter cake, and the waste water is treated centrally; the washed filter cake is washed with absolute ethanol to remove water, and the absolute ethanol is recovered; the nickel powder filter cake washed with absolute ethanol is in the Ethanol and a small amount of water were removed in vacuum at 40°C ...

Embodiment 2

[0035] A preparation method of nano nickel powder, comprising:

[0036] (1) Add 0.1mol NiSO 4 Dissolve 10g of PVA in water and mix evenly, then add 0.02mol of ethylenediamine and stir thoroughly to obtain 300ml of A solution; add 0.7mol of N 2 h 4 ·H 2 O, 0.02mol potassium borohydride and 3.0mol KOH are miscible in water to obtain 700ml B liquid;

[0037] (2) Heat liquid A to 70°C, add liquid B to liquid A, the feeding time is 50min, the temperature of the reaction system is maintained at 70°C and react for 40min, then add cold water to cool to room temperature (10-30°C); the reaction product is centrifuged Separation, the filter cake is washed with water to remove impurities in the filter cake, and the waste water is treated centrally; the washed filter cake is washed with absolute ethanol to remove water, and the absolute ethanol is recovered; the nickel powder filter cake washed with absolute ethanol is in the Ethanol and trace moisture were removed under vacuum at 40°C...

Embodiment 3

[0039] A preparation method of nano nickel powder, comprising:

[0040] (1) Add 0.25molNi(NO 3 ) 2 Dissolve 20.0g PEG in water and mix evenly, then add 0.0125mol disodium edetate and stir well to obtain 250ml A solution; mix 1.2mol N 2 h 4 ·H 2 O, 0.03mol potassium borohydride and 5.0mol NaOH are miscible in water to obtain 750ml B liquid;

[0041](2) Heat liquid A to 60°C, add liquid B to liquid A, the feeding time is 60min, the temperature of the reaction system is maintained at 60°C and react for 40min, then add cold water to cool to room temperature (10-30°C); the reaction product is centrifuged Separation, the filter cake is washed with water to remove impurities in the filter cake, and the waste water is treated centrally; the washed filter cake is washed with absolute ethanol to remove water, and the absolute ethanol is recovered; the nickel powder filter cake washed with absolute ethanol is in the Ethanol and a small amount of water were removed in vacuum at 40° C...

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Abstract

The invention discloses a preparation method of nickel nanopowder. The method includes: dissolving nickel salt and surfactant in water, mixing well, adding complexing agent into obtained nickel slat solution, mixing for reaction to obtain complex nickel salt solution A, dissolving reducing agent and alkali in water to obtain solution B, heating the solution A, adding the solution B into the solution A to obtain mixture of the solutions A and B, cooling, subjecting a reaction product to solid-liquid separation to obtain nickel nanopowder filter cakes, washing to remove impurities in the filter cakes, washing the washed filter cakes with absolute ethyl alcohol to remove moisture, and removing ethyl alcohol and trace moisture from the filter cakes, washed with the absolute ethyl alcohol, in vacuum at the temperature of 40-60 DEG C so as to obtain spherical nickel nanopowder. The method has the advantages that the process is short and easy to control, production cost is low, reduction degree is high, production efficiency is high, and industrial production is easy.

Description

technical field [0001] The invention relates to the technical field of preparation of nanometer materials, in particular to a liquid phase chemical reduction preparation method of nanometer nickel powder. Background technique [0002] With the miniaturization, ultra-large, and integrated development of electronic technology, electronic components will become smaller and smaller, and the nickel powder used as electronic paste is also required to reach the nanometer level; at the same time, because nano-nickel powder has conventional In addition to the properties of nickel powder, it also has unusual properties such as small volume, high specific surface area and quantum properties. The uniformity and monodispersity of nano-nickel powder is one of the conditions for the miniaturization of electronic components. Nano-nickel powder has unique physical and chemical properties such as high surface activity, high surface purity, large specific surface area, magnetism, and no micro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24
Inventor 何爱山
Owner YUCHEN ADVANCED ENERGY MATERIALS & TECH WUXI
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