Method for preparing ultrafine copper powder by secondary atmosphere reduction

A technology of ultra-fine copper powder and secondary atmosphere, applied in metal processing equipment, transportation and packaging, etc., can solve the problems of poor particle dispersion and sintering, and achieve good dispersion effect

Active Publication Date: 2020-06-05
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the products obtained by direct hydrogen reduction in this temperature range are prone to serious sintering and poor particle dispersion.

Method used

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  • Method for preparing ultrafine copper powder by secondary atmosphere reduction
  • Method for preparing ultrafine copper powder by secondary atmosphere reduction
  • Method for preparing ultrafine copper powder by secondary atmosphere reduction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] 1) The cuprous oxide powder and the process control agent (PCA) stearic acid are mixed by simple mechanical stirring. The amount of stearic acid added is 0.5% of the copper oxide powder mass;

[0058] 2) After weighing the above mixed powder, weigh the zirconia balls according to the ball-to-material ratio of 10:1, put them together into a ball mill jar, vacuumize to 15Pa, and then pass in a protective atmosphere of argon .

[0059] 3) Put the ball mill pot into a planetary ball mill for ball milling, the ball milling speed is 300r / min, and the ball milling time is 6h.

[0060] 4) Spread the ball-milled powder into the corundum boat, control the thickness within 2mm, then slowly put the corundum boat into the tube furnace, vacuumize until the ambient pressure in the tube does not exceed 15Pa; then fill it with nitrogen or inert gas to 1 atmosphere.

[0061] 5) When the temperature is raised to the holding temperature of 300°C at a heating rate of 6°C / min, a CO atmosp...

Embodiment 2

[0065] The preparation method is basically the same as in Example 1, except that the amount of stearic acid added is 2% of the mass of copper oxide powder, the ball milling speed is 250r / min, the ball milling time is 12h, and the ball-to-material ratio is 15:1. The heating rate was 4°C / min.

[0066] After reduction, the oxygen content is 0.08wt%, the powder shape is approximately spherical, there is no obvious sintering phenomenon between the particles, the particle size is 0.500-1 μm copper powder particles, and the color of the copper powder is rose red.

Embodiment 3

[0068] The preparation method is basically the same as in Example 1, except that the amount of stearic acid added is 1.2% of the mass of the copper oxide powder, the ball milling speed is 300r / min, the ball milling time is 6h, and the heating rate is 5°C / min. The reduction temperature is 350°C, and the holding time for the first stage of CO reduction is 0.5h.

[0069] After reduction, copper powder particles with an oxygen content of 0.05wt%, approximately spherical powder appearance and a particle size of 0.3-0.8 μm are obtained, but there is no obvious sintering phenomenon between the particles, and the color of the copper powder is rose red.

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Abstract

The invention discloses a method for preparing ultra-fine copper powder by secondary atmosphere reduction. Copper oxide powder and process control agent are mixed in proportion to obtain mixed powder; the mixed powder and zirconia balls are put into a ball mill jar; the ball mill jar is put into Carry out high-energy ball milling in a planetary ball mill; put the ball-milled powder into the crucible, then put the crucible into the tube furnace, and close the hatch; heat up and introduce reducing gas CO at the holding temperature point, and then keep warm; close CO venting valve, and then re-introduce H into the pipe 2 , and at the new holding temperature point, carry out isothermal reduction, and then keep warm; close the H 2 Vent valve, and close the outlet valve, and cool to room temperature with the furnace to obtain ultra-fine copper powder. The invention can prepare the superfine conductive powder material required by the superminiature chip and the conductive material of the contact, the process is simple, the cost is low, and the method is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of microelectronics manufacturing and 3D printing, and in particular relates to a method for preparing ultrafine copper powder through secondary atmosphere reduction. Background technique [0002] In recent years, as products and technologies such as flexible wearable devices, high-precision sensors, electronic printing, and 3D printing have attracted more and more attention from the capital market, microelectronics products are gradually moving towards lightweight, portable, space-saving, and ultra-precision develop. According to the 2017-2027 forecast report on electronic printing and organic flexible electrical appliances by IDTechEx in the United States, the global market for 3D electronic printing and flexible electronic devices will grow from US$29.28 billion in 2017 to US$73.43 billion in 2027. The conductive copper material in this type of microelectronic components will also develop in the directio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/22B22F1/00
CPCB22F9/22B22F1/065B22F1/054
Inventor 黄斐杨斌汪航廖涛王朝阳
Owner JIANGXI UNIV OF SCI & TECH
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