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Method for preparing monodisperse high-crystallinity silver powder

A high crystallinity, monodisperse technology, applied in the field of metal powder material preparation, can solve the problems of difficulty in meeting the market demand, low crystallinity of liquid phase powder, and low quality of silver powder products, and achieve rich product types, narrow particle size distribution, Use the effect of good performance

Inactive Publication Date: 2012-07-18
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (2) Wide particle size distribution or serious agglomeration
[0007] (3) The crystallinity is not high and the tap density is low, which is especially serious for the liquid phase process
Due to the low reaction temperature and fast crystal nucleus growth rate, the crystallinity of the liquid phase powder is low, which makes the performance of the silver powder poor.
[0008] In short, although scientific researchers have carried out extensive research and discussion on the preparation of silver powder, due to the defects of the technical route itself, the quality of the current silver powder products is low, and it is difficult to meet the needs of the market

Method used

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  • Method for preparing monodisperse high-crystallinity silver powder
  • Method for preparing monodisperse high-crystallinity silver powder
  • Method for preparing monodisperse high-crystallinity silver powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Precursor preparation

[0037] First prepare 100ml of silver nitrate solution A with a concentration of 1mol / L, and then prepare 100ml of 1.2mol / L NaOH mixed solution B, then control the reaction temperature at 80°C and the stirring speed at 200r / min, and feed solution B at a feeding speed of 5ml / min Added to solution A, after the addition was completed, aged for 1h. The precipitated product was washed 3 times with pure water, and vacuum-dried at 50°C to constant weight to obtain a precursor;

[0038] (2) Precursor reduction

[0039] First, the obtained precursor was dispersed by ball milling for 3 hours, the ball-to-material ratio was 10:1; the rotation speed was 400r / min, and then the precursor was added to the burning boat, put into the muffle furnace and calcined at 400°C for 2 hours to obtain the silver powder product. The resulting silver powder scanning electron microscope picture is as follows figure 2 As shown, the particle morphology is spherical or sp...

Embodiment 2

[0041] (1) Precursor preparation

[0042] First prepare 100ml of silver nitrate solution A with a concentration of 1.2mol / L, and then prepare 0.8mol / L Na 2 CO 3 Solution B 80ml, then control the reaction temperature at 60°C and the stirring speed at 200r / min, add solution B to solution A at a feeding speed of 30ml / min, and age for 1.5h after the addition. The precipitate was washed 3 times with pure water, and dried in vacuum at 50°C to constant weight to obtain the precursor;

[0043] (2) Precursor reduction

[0044] First, the obtained precursor was dispersed by ball milling for 4 hours, the ball-to-material ratio was 30:1; the rotation speed was 300r / min, and then the precursor was added to a burning boat, placed in a muffle furnace and calcined at 350°C for 4 hours to obtain a silver powder product. The resulting silver powder scanning electron microscope picture is as follows image 3 As shown, the particle morphology is spherical or spherical, and the average particl...

Embodiment 3

[0046] (1) Precursor preparation

[0047] First prepare 100ml of silver nitrate solution A with a concentration of 2mol / L, and then prepare 1mol / L Na 2 C 2 o 4 Solution B 120ml, then control the reaction temperature at 55°C and the stirring speed at 300r / min, add solution B to solution A at a feeding speed of 50ml / min, and age for 2h after the feeding is completed. The precipitate was washed three times with pure water, and vacuum-dried at 50° C. to constant weight to obtain the precursor.

[0048] (2) Precursor reduction

[0049] First, the obtained precursor was dispersed by ball milling for 5 hours, the ball-to-material ratio was 50:1; the rotation speed was 500r / min, and then the precursor was added to a burning boat, placed in a muffle furnace and calcined at 450°C for 2 hours to obtain a silver powder product. The resulting silver powder scanning electron microscope picture is as follows Figure 4 As shown, the particle morphology is spherical or spherical, and the av...

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Abstract

A method for preparing monodisperse high-crystallinity silver powder includes preparing a precursor and reducing the precursor. At least one of K+, Na+ and NH4+ hydroxide, carbonate and oxalate is selected to prepare precipitator liquor B; the liquor B is added into silver nitrate liquor A, the liquor is filtered after being aged for 1-2h, precipitates are washed with pure water, the precipitates are dried in a vacuum manner at the temperature of 50 DEG C to reach constant weight, and the precursor is obtained; and the obtained precursor is calcined after ball milling dispersion to obtain the silver powder. The process method is simple, operation is convenient, a wet process is combined with a pyrogenic process, the prepared silver powder is uniform in grain size, the mean grain size ranges from 0.5 micrometer to 4 micrometers, grains are spherical or similarly spherical, the silver powder is high in crystallinity, narrow in grain size distribution, high in tap density, high in quality and environment-friendly, special equipment is omitted, and industrialization is easily realized.

Description

technical field [0001] The invention discloses a preparation method of monodisperse silver powder with high crystallinity. The invention belongs to the technical field of metal powder material preparation. Background technique [0002] Silver powder is widely used in electronics, energy, biology and other fields because of its excellent thermal conductivity, electrical conductivity, antibacterial and catalytic properties. Silver powder is the most used precious metal powder in the electronics industry, and is the key material for the production of various electronic components. In particular, the rapid development of the solar energy industry in recent years has drawn much attention to the preparation of silver powder. As far as the reported method is concerned, the preparation method of silver powder is mainly based on wet process. The wet process is a method of adding a reducing agent to the liquid phase to reduce silver ions to prepare silver powder under certain condi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/04B22F9/20
Inventor 李玉虎刘志宏李启厚刘智勇陈建波李晏平
Owner CENT SOUTH UNIV
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