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Process for producing silver powder

A manufacturing method and technology of silver particles, applied in semiconductor/solid-state device manufacturing, nanotechnology for materials and surface science, transportation and packaging, etc., can solve problems such as unoptimized, and achieve good sinterability and high monodispersity Effect

Inactive Publication Date: 2013-01-23
DOWA ELECTRONICS MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the molecular weight of the mercaptan-based dispersant is as low as about 200, it can be easily removed by low-temperature firing when wiring is formed. However, it contains sulfur (S), which causes corrosion of wiring and other electronic parts. Unpreferable for wiring formation applications

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0156] Add 185.83 mL of oleylamine (Wako Pure Chemical Industries, Ltd. Mw=267) as an organic protective agent and silver nitrate as a silver compound to 140 mL of isobutanol (special grade manufactured by Wako Pure Chemical Industries, Ltd.) as a reaction medium and reducing agent. 19.218 g of crystals (manufactured by Kanto Chemical Co., Ltd.) were stirred with a magnetic stirrer to dissolve silver nitrate.

[0157] Move this solution to a container with a reflux device and place it in an oil bath. While blowing nitrogen as an inert gas into the container at a flow rate of 400 mL / min, while stirring with a magnetic stirrer, the reaction tank In order to maintain the flow of the Reynolds number of 3600-3800, set the stirring power to 1.17×10 4 ~1.28×10 4 W and heating, and reflux at a temperature of 108° C. for 5 hours. The heating rate was set at 2°C / min.

[0158] The slurry after the reaction is subjected to the washing, dispersion and classification described herein, an...

Embodiment 2

[0160] Except when stirring with a magnetic stirrer, in order to maintain a flow with a Reynolds number of 7300 to 7450, set the stirring power to 3.03×10 5 ~3.18×10 5 W, except that the solution in the reaction tank was stirred and heated, Example 1 was repeated.

[0161] After the reaction, the slurry was subjected to the washing, dispersion and classification described herein, and the TEM particle size was measured by the method described herein, and the reduction rate, monodispersion rate, and yield were calculated. As a result, the reduction rate was 96.7%, the monodispersity rate was 68.4%, and the yield was 66.1%. The single crystallinity is 1.19.

Embodiment 3

[0163] Example 1 was repeated except that natural convection was performed in such a manner as to maintain a flow having a Reynolds number of 400 or less without stirring.

[0164] After the reaction, the slurry was subjected to the washing, dispersion and classification described herein, and the method described herein was used to measure the TEM particle size and calculate the reduction rate, monodispersion rate, and yield. As a result, the reduction rate was 94.3%, the monodispersity rate was 88.8%, and the yield was 83.7%. In addition, the degree of single crystallinity was 0.52. Even if forced stirring is not performed as in this example, a flow formed by blowing nitrogen gas and repeated evaporation and condensation can be generated, thereby maintaining a flow with a Reynolds number of 400 or less, and good stirring can be obtained even in natural convection mixed effect.

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PUM

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Abstract

Provided is a method for producing a silver particle powder excellent in the dispersibility in a liquid organic medium having a low polarity, which comprises reducing a silver compound in an alcohol having a boiling point of from 80°C to 200°C or in a polyol having a boiling point of from 150 to 300°C, at a temperature of from 80°C to 200°C under reflux while maintaining the stream having a Reynolds number of not more than 3.70 × 10 4 . The stream having a Reynolds number of not more than 3.70 × 10 4 can be maintained by stirring with a stirring power of not more than 5.68 × 10 8 W. According to the method, a silver particle powder having good low-temperature sinterability and good dispersibility and suitable for use for microwiring formation can be obtained at a high yield.

Description

technical field [0001] The present invention relates to a method for producing fine (especially nanometer-sized) silver particle powder, and specifically relates to a wiring forming material suitable for forming a fine circuit pattern, for example, a wiring forming material using an inkjet method, etc. The manufacture method of the silver particle powder. Background technique [0002] Since the specific surface area becomes very large when the size of the solid substance is in the nm order (nanometer order), although it is a solid, its interface with gas and liquid becomes very large. Therefore, its surface properties largely affect the properties of solid substances. It is known that in the case of metal particle powder, its melting point is sharply lowered compared with that of a bulky state. Therefore, compared with μm-order particles, nm-order particle powder has the ability to draw fine wiring, and, It can be sintered at low temperature and so on. Among metal particl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24B22F1/00H01L21/28H01L21/288B22F1/0545
CPCB22F9/24H01L21/76838H01L21/288B22F1/0022B82Y30/00Y10T428/24413Y10T428/2982B22F1/0545B22F1/00H01L21/28
Inventor 佐藤王高久枝穰
Owner DOWA ELECTRONICS MATERIALS CO LTD
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