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Method for preparing monodisperse high-crystallinity copper powder

A high crystallinity, monodisperse technology, applied in the field of preparation of copper powder for conductive paste, can solve the problems of ineffective control of the reaction process, broadening of powder particle size distribution, unbalanced reaction process, etc., to achieve cheap raw material sources, structure The effect of dense and well-developed crystal lattice

Inactive Publication Date: 2010-01-20
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its shortcoming is that the reaction speed of this method depends on the dissolution rate of cuprous oxide, the reaction process cannot be effectively controlled, and its reaction process is unbalanced; moreover, its reducing agent is added after the system reaches the reaction temperature , this addition method is bound to cause local inhomogeneity of the system, and the secondary nucleation is more serious, which makes the powder particle size distribution wider and the powder surface rougher. At the same time, it is difficult to make the powder particles have high crystallinity due to too fast local reaction speed
In addition, the process uses expensive reagents, and the cost is also high

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] First prepare 0.5 L of alcohol-water solution of copper compound, wherein the addition amount of ethylene glycol is 0.5 mol, copper nitrate is 0.5 mol, then add 1 mol of sodium hypophosphite, sodium formate is added to the saturated amount, after mixing well, adjust the pH of the solution to 6.8°C, then raised to 95°C, introduced carrier gas Ar, the flow rate of the carrier gas was 200ml / min·L, and after 1 hour of heat preservation, the obtained product was separated from liquid to solid, washed, and dried in vacuum to obtain monodisperse and highly crystalline copper powder. The shape of the copper powder is spherical, and the average particle size is 3.2um. The X-ray pattern of copper powder is as follows figure 1 As shown, it can be seen from the figure that, except for the characteristic peak of copper, there is no other impurity phase, and the characteristic peak is narrow and sharp, indicating that the prepared copper powder grains are well developed and have hig...

Embodiment 2

[0024] First prepare 0.5 L of alcohol-water solution of copper compound, wherein the addition amount of triethylene glycol is 0.5 mol, copper chloride is 0.5 mol, then add 1 mol of formaldehyde, sodium chloride is added to the saturated amount, after fully mixing, adjust the pH of the solution to 6.5, then the temperature was raised to 65°C, and the carrier gas N 2 , the flow rate is 100ml / min·L, after 2 hours of heat preservation, the obtained product is separated from liquid to solid, washed, and dried in vacuum to obtain monodisperse copper powder with high crystallinity. The shape of the copper powder is spherical, and the average particle size is 4.7um. Scanning electron microscope photos as image 3 shown.

Embodiment 3

[0026] First prepare 0.5L of alcohol-water solution of copper compound, wherein the addition amount of 1,2-propanediol is 0.5mol / L, copper acetate is 0.25mol, then add 1mol of hydrazine hydrate, add sodium chloride to the saturated amount, and mix thoroughly, Adjust the pH of the solution to 7.2, then raise the temperature to 80°C, pass the carrier gas Ar, the flow rate of the carrier gas is 200ml / min·L, keep it warm for 3 hours, separate the liquid from the solid, wash it, and dry it in vacuum to obtain monodisperse High crystallinity copper powder. The shape of the copper powder is spherical, and the average particle size is 2.4um. Scanning electron microscope photos as Figure 4 shown.

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Abstract

A preparation method of monodisperse high crystallinity copper powder is provided, which relates to a method for preparing copper powder used in conductive paste by using cupreous compound, in particular to a preparation method of the copper powder used in the conductive paste that is applicable to ceramic electronic components with a plurality of layers. The method is characterized in that: cupric salt and copper oxide or copper hydroxide are taken as raw materials, a reductant and a reaction control agent are added into an alcohol-water system and fully mixed, reaction occurs under the conditions that the pH of the solution is 6.0 to 7.5 and the temperature is 50 to 95 DEG C, inert gas is used as carrier gas during the reaction process and the flux of the carrier gas is 50 to 500 ml / min question mark L, then solid-liquid separation, washing and drying are carried out to an obtained product after heat preservation for 1 to 6 h, and the monodisperse high crystallinity copper powder is obtained. The copper powder prepared by the invention is in spheroid shape or polyhedron shape, of which the grains are monodisperse and non-aggregating and have smooth surface, good crystallinity and certain antioxidant capacity. The size distribution of the copper powder is narrow and the average grain size can be regulated between 0.1 and 10 um.

Description

technical field [0001] The invention relates to a method for preparing copper powder for conductive paste with a copper compound, in particular to a preparation method for copper powder for conductive paste suitable for multilayer ceramic electronic components. Background technique [0002] The electronic information industry has put forward higher requirements for the development of base metallization of electronic pastes, among which the development of a new generation of high-performance copper powder is particularly urgent, especially for conductive pastes that need to undergo high-temperature processes such as sintering and roasting, such as multi-layer Copper powder for ceramic electronic components and electromagnetic shielding conductive paste should have spherical, monodisperse, non-agglomerated, high crystallinity and other characteristics in addition to particle size and particle size distribution. [0003] Among the preparation methods of copper powder for conduc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24
Inventor 刘志宏李玉虎李启厚张多默
Owner CENT SOUTH UNIV
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