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Liquid phase fluidized reduction method for preparing nanometer nickel powder

A technology of nanometer nickel powder and reduction method, which is applied in the field of preparation of nanometer nickel powder, can solve the problems of difficulty in liquid phase reduction of particle size and morphology, difficulty in industrialization, generation of waste water, etc., and achieves reduction of production cost, simple equipment and low energy consumption. Effect

Inactive Publication Date: 2006-12-13
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The liquid phase reduction method is to use nickel salt as raw material and hydrazine hydrate etc. It is difficult to control the morphology, industrialization is more difficult, and waste water is produced

Method used

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  • Liquid phase fluidized reduction method for preparing nanometer nickel powder
  • Liquid phase fluidized reduction method for preparing nanometer nickel powder
  • Liquid phase fluidized reduction method for preparing nanometer nickel powder

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Example 1 Dissolve 14 g of nickel sulfate in 100 ml of distilled water, dissolve the theoretical ratio of NaOH in distilled water, mix the two solutions, and then add 0.1% CTAB solution to obtain Ni(OH) at pH 12 2 Colloid, the colloid was mixed with 5 mL of hydrazine hydrate, and flowed through the fluidized bed reactor at a speed of 1.5 L / min at a temperature of 60° C. After the reaction, it was cooled and filtered with suction to obtain a black solid powder. The solid is a ferromagnetic solid, and its surface morphology is shown in FIG. 1 . The nickel powder has a median diameter of 60nm measured by the small angle scattering method, an electron microscope statistical average particle diameter of 95nm, and a specific surface area of ​​8.8m 2 / g.

Embodiment 2

[0026] Example 2 Dissolve 14g of nickel sulfate in 100ml of distilled water, dissolve the theoretical ratio of NaOH in distilled water, mix the two solutions, and then add 0.1% CTAB solution to obtain Ni(OH) at pH 12 2 Colloid, 0.1% cobalt sulfate in the system, change the surfactant to SDS, and the reducing agent to NaBH 4 , the amount of reducing agent added is 0.8g, and the flow rate of 3L / min passes through the fluidized bed reactor at a reaction temperature of 90°C. After the reaction, black ferromagnetic powder is obtained. The scattering particle size is 28nm, and the electron microscope statistical particle size is 50nm , the specific surface area is 42.59m 2 / g, the morphology of nickel powder is shown in Figure 2.

Embodiment 3

[0027] Example 3 Dissolve 14g of nickel sulfate in 100ml of distilled water, dissolve the theoretical ratio of NaOH in distilled water, mix the two solutions, and then add 0.1% CTAB solution to obtain Ni(OH) at pH 12 2 Colloid; add 5ml of hydrazine hydrate and 0.2% ammonium tungstate to the pH12 colloid. The colloid was passed through a fluidized bed reactor at a flow rate of 0.8 L / min at a temperature of 100° C. After the reaction was completed, the black ferromagnetic powder was obtained by cooling, vacuum filtration, and water washing. The surface morphology of the black ferromagnetic powder is shown in Figure 3, the scattering median diameter is 78nm, the statistical average particle diameter is 92nm, and the specific surface area is 8.02m 2 / g.

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Abstract

The invention relates to a method for preparing nanometer nickel powder, especially for preparing spherical nanometer nickel powder with grain size being 30-100 nm and specific surface area being larger than 8 m2 / g. The invention is characterized in that: dissolving nickel nitrate or nickel sulfate with deionized water, adding proper amount of surface activator to prepare nickel hydroxide slurry; fastening reaction on rapid heat transmission and even temperature fluid bed with reducer and accelerant to control core formation of nickel powder and crystal growth, preparing spherical nanometer nickel powder; desalting reacting liquid and returning it to reactor, moderating temperature and retention time; returning washing liquid to batching process. The invention controls size of nanometer nickel powder by controlling crystal growth time, and prepares spherical nanometer nickel powder with size being 30-100 nm and specific surface area being larger than 8 m2 / g; the reacting liquid and washing liquid are reused in process, the wastewater discharge is reduced, and the production is lowered.

Description

Technical field: [0001] The invention relates to a preparation method of nano-nickel powder, especially the prepared particle size is 30-100nm, and the specific surface area is greater than 8m 2 / g of spherical nano-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 nanoscale particles; at the same time, due to the removal of nanoscale nickel powder In addition to the characteristics of conventional nickel powder, it also has unusual characteristics such as small size and quantum characteristics. The uniformity and monodispersity of nano-nickel powder is one of the conditions for the miniaturization of electronic components. Nano-nickel powder can also be used as petroleum cracking catalyst, fine organic synthesis catalyst, rocket fuel catalyst, cemented carbide...

Claims

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Application Information

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IPC IPC(8): B22F9/24
Inventor 金胜明袁良生周贤渭肖麦秋
Owner CENT SOUTH UNIV
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