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A kind of method for preparing superfine nickel powder by solid phase reduction

A technology of nickel powder and powder, which is applied in the field of solid-phase reduction to prepare ultra-fine nickel powder, which can solve the problems of large environmental pollution, complex equipment, and large particle size of nickel powder, and achieve simple process, low preparation cost and controllable parameters Effect

Inactive Publication Date: 2019-01-04
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for the existing method for industrialized production of ultrafine nickel powder, which has large particle size and poor dispersibility, or complex equipment, low production efficiency, or large environmental pollution and high production cost. A method for preparing superfine nickel powder by solid phase reduction, the method can control the particle size of the nickel powder obtained by reduction by adding a suitable metal halide to the nickel oxalate powder as a barrier agent, and prevent the agglomeration between the generated nickel powder particles , and at the same time, the halide barrier is effectively recovered, which has good environmental protection

Method used

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  • A kind of method for preparing superfine nickel powder by solid phase reduction
  • A kind of method for preparing superfine nickel powder by solid phase reduction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Select nickel oxalate powder with a powder particle size range of 0.1-1 mm as raw material, add 30wt% potassium chloride as a barrier agent, select absolute ethanol as the ball milling medium, put it into a ball mill, and mill for 12 hours. The ball-to-material ratio is 5:1. Set to 180 rpm. The mixed slurry was placed in an oven for drying at a temperature of 75° C. for 2 hours to obtain fully dried nickel oxalate and potassium chloride uniformly mixed raw materials. Then, put the dried mixture into a sintering boat, put it into a sintering furnace, and carry out reduction under a hydrogen atmosphere at a temperature of 500° C. and a holding time of 0.5 hours. The reduced powder was washed with distilled water 5 times to remove the potassium chloride blocking agent in the powder; then dried at 50° C. for 5 hours.

[0028] The nickel powder prepared in this example has an average particle size of 0.403 μm and a specific surface area of ​​3.31 μm 2 / g.

Embodiment 2

[0030] Select nickel oxalate powder with a particle size range of 0.1-1 mm as raw material, add 40wt% sodium chloride as a barrier agent, select absolute ethanol as the ball milling medium, put it into a ball mill, and mill for 18 hours. Set to 150 rpm. The mixed slurry was placed in an oven for drying at a temperature of 60° C. for 3 hours to obtain fully dried nickel oxalate and sodium chloride uniformly mixed raw materials. Then, put the dried mixture into a sintering boat, put it into a sintering furnace, and carry out reduction under a hydrogen atmosphere at a temperature of 460° C. and a holding time of 1 hour. The reduced powder was washed with distilled water five times to remove the sodium chloride blocking agent in the powder; then dried at 60° C. for 4 hours.

[0031] The nickel powder prepared in this example has an average particle size of 0.280 μm and a specific surface area of ​​3.73 μm 2 / g.

Embodiment 3

[0033] Select nickel oxalate powder with a particle size range of 0.1-1mm as raw material, add 50wt% sodium chloride as a barrier agent, select absolute ethanol as the ball milling medium, put it into a ball mill, and mill for 24 hours. Set to 120 rpm. The mixed slurry was placed in an oven for drying at a temperature of 50° C. for 4 hours to obtain fully dried nickel oxalate and sodium chloride uniformly mixed raw materials. Then, put the dried mixture into a sintering boat, put it into a sintering furnace, and carry out reduction under a hydrogen atmosphere at a temperature of 420° C. and a holding time of 2 hours. The reduced powder was washed with distilled water 5 times to remove the sodium chloride blocking agent in the powder; then dried at 75°C for 3 hours.

[0034] The nickel powder prepared in this example has an average particle size of 0.152 μm and a specific surface area of ​​4.42 μm 2 / g.

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Abstract

The invention provides a method for preparing superfine nickel powder by means of solid-phase reduction. The method for preparing the nickel powder at least comprises the following steps that (a) nickel oxalate powder is selected as a raw material, a proper metal halide blocking agent is added, absolute ethyl alcohol is selected as a ball-milling medium, and the materials are evenly mixed in a ball grinding mill; (b) mixed slurry of the nickel oxalate powder and the metal halide blocking agent is placed into an oven to be dried; (c) a dried mixed material is put into a combustion boat, and a solid-phase reduction reaction is carried out in the reducing atmosphere; and (d) heating is stopped, after the temperature is lowered to an indoor temperature, a powder sample is taken out to be washed with distilled water, the metal halide blocking agent capable of being dissolved into water is fully removed, and then powder obtained by washing is put into the oven to be dried so that superfine elementary substance nickel powder can be obtained. By the adoption of the method, proper metal halide is added into the nickel oxalate powder to be used as the blocking agent, and the grain size of the nickel powder obtained through reduction can be controlled; and meanwhile, the metal halide blocking agent can be effectively recovered and the environmental protection property is good.

Description

technical field [0001] The invention relates to the field of metal powder materials, in particular to a method for preparing superfine nickel powder by solid phase reduction with small particle size, low production cost and good environmental protection in the production process. Background technique [0002] Ultrafine nickel powder has been widely used in conductive paste, battery material, magnetic material and other fields because of its unique electromagnetic, catalytic, large surface effect and volume effect. At present, the methods used for industrial production of ultra-fine nickel powder in my country mainly include liquid phase reduction method, nickel carbonyl thermal decomposition method and evaporation-condensation method, among which the liquid phase reduction method is the most common. Chinese patent [CN 104889415A] dissolves nickel nitrate, urea and glucose in deionized water in a certain proportion, mixes it into a solution and heats it until a violent redox ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/22
CPCB22F9/22
Inventor 刘如铁王铸博陈洁何达熊翔林雪杨成凯
Owner CENT SOUTH UNIV
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