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Silver powder made of silver particles, each to which fine silver particles adhere and process of producing the same

a silver nanoparticle and silver powder technology, applied in the direction of printed circuit aspects, semiconductor/solid-state device details, transportation and packaging, etc., can solve the problem of difficult to meet the size-refinement of powder particles and the dispersibility meant by powder particles nearly in a mono-disperse state, and the low-temperature sintering performance of silver nanoparticles cannot be used to the full, so as to reduce the amount of impurities contained, improve the effect of low-temperature sintering

Inactive Publication Date: 2005-08-25
MITSUI MINING & SMELTING CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The present invention relates to a new process for producing a silver powder that overcomes the limitations of conventional methods. The new process involves coating the surface of each powder particle with finer silver particles, resulting in a silver powder with improved low-temperature sintering performance. The coated powder particles have high dispersibility and low agglomeration, making them useful for various applications such as forming wiring circuits and adhesives. The new silver powder also has low impurity content and high conductivity, making it ideal for use in power-supply circuits and low-resistance circuits. The process of producing the new silver powder involves using a wet reduction process and adding a reducing agent, resulting in a silver powder with low crystallinity and high dispersibility. Overall, the new process provides a solution for producing a high-quality silver powder with improved low-temperature sintering performance.

Problems solved by technology

However, in a metal powder such as a silver powder, it is generally said that both the size-refinement of powder particles and the dispersibility meant by that powder particles nearly in a mono-disperse state are hard to become satisfied.
In such a case, generally the decomposition temperature of the dispersant is higher than the sintering temperature of the silver nanoparticles, resulting in that the low-temperature sintering performance of the silver nanoparticles themselves cannot be used to the full.
Further, in case of the silver ink containing the silver nanoparticles, because the content of the filler is less than conventional, a thick film is difficult to form while a thin film is easy to form.
This makes it difficult to use such silver ink for application to form wiring circuits having a large cross-sectional area sufficient to be usable for power-supply circuit such carries a relatively large amount of current or for application to form a low-resistance circuit.
Further, in the use of the silver ink for adhesives for mounting components thereon, not only its conductivity, but also its adhesive strength is required severely.
Thus, there remain many problems that cannot be overcome by conventional silver-nanoparticles-containing silver ink.
In the meantime, it goes without saying that silver powder used for commonly-used silver pastes has had a limitation in terms of its low-temperature sintering performance judging from its particle size.
Thus, the conventional silver powder has been unsuitable when forming recent circuits where fine-pitched wiring patterns are drawn.
As a result, a silver powder has been merely obtained such that its crystallinity is low, and additionally its agglomeration significantly occurs easily.

Method used

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  • Silver powder made of silver particles, each to which fine silver particles adhere and process of producing the same
  • Silver powder made of silver particles, each to which fine silver particles adhere and process of producing the same
  • Silver powder made of silver particles, each to which fine silver particles adhere and process of producing the same

Examples

Experimental program
Comparison scheme
Effect test

example 1

Process for Producing Silver Powder Used as a Core Material:

[0068] In this example, first silver powder (whose particle is spherical) used as a core material was produced. The production process was as follows.

[0069] First, 63.3 g of silver nitrate was dissolved in 9.7 liter of deionized water to prepare an aqueous solution of silver nitrate. Then, 235 ml of 25% by weight aqueous ammonia was added for a very short time to the aqueous solution of silver nitrate and stirred to give an aqueous solution of a silver ammine complex.

[0070] The aqueous solution of a silver ammine complex was introduced into a first pass a having an inner diameter 13 mm, shown in FIG. 2, at a flow rate of 1500 ml / sec and a reducing agent was allowed to flow through a second pass b at a flow rate of 1500 ml / sec so that the solution and the agent came into contact with each other at a juncture m while being kept at 20° C. to precipitate fine silver powder through reduction. The reduction agent used here wa...

example 2

Process for Producing Silver Powder Used as a Core Material:

[0077] In this example, first silver powder (which is substantially spherical) used as a core material was produced. The production conditions were as described below.

[0078] Silver powder was produced under production conditions different from those of Example 1 and the powder characteristics of the resultant silver powder were determined. Then, a silver paste was prepared using the above silver powder and a test circuit was formed using the silver paste. Then, the specific resistance of the conductor and sinterable temperature were measured for the formed test circuit.

[0079] First, 63.3 g of silver nitrate was dissolved in 3.1 liter of deionized water to prepare an aqueous solution of silver nitrate. Then, 235 ml of 25% by weight aqueous ammonia was added for a very short time to the aqueous solution of silver nitrate and stirred to give an aqueous solution of a silver ammine complex.

[0080] The aqueous solution of a s...

example 3

Process for Producing Silver Powder Used as a Core Material:

[0087] In this example, first silver powder (of nearly spherical shape) having a large crystallite size was produced using the process shown below, and the powder characteristics of the resultant silver powder were determined. Then, a silver paste was prepared using the above silver powder and a test circuit was formed using the silver paste. Then the specific resistance and sinterable temperature were measured for the formed test circuit.

[0088] First, 20 g of polyvinyl pyrrolidone was dissolved in 260 ml of deionized water and 50 g of silver nitrate was dissolved to prepare an aqueous solution of silver nitrate. Then, 25 g of nitric acid was added for a very short time to the above solution and stirred to yield a silver-containing nitric acid solution. At the time of completion of the mixing, the concentration of ascorbic acid was about 36.0 g / l.

[0089] A reducing solution was prepared by adding and dissolving 35.8 g of...

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Abstract

This invention is a silver powder having a low-temperature sintering performance and dispersibility, which allows the powder particles to be agglomerated to a small degree and be nearly in the monodisperse state. Employed is silver powder of fine silver particles each to which fine silver particles adhere, wherein fine silver particles of nano-order particle size are adhered to the surface of each silver powder particle. The powder particles of the silver powder of fine silver particles each to which fine silver particles adhere have excellent dispersibility. In the production of the silver powder of fine silver particles each to which fine silver particles adhere, a process of including the steps of: adding a silver nitrate and a neutralizing agent into a slurry of silver powder in a dispersing medium; dissolving the mixture while stirring to allow fine silver oxide particles to be precipitated on the surface of each silver powder particle; washing the resultant silver powder; and exposing the fine silver oxide particles to UV rays to reduce the same to fine silver particles.

Description

TECHNICAL FIELD [0001] The present invention relates to a silver powder made of silver particles, each to which fine silver particles adhere and a process of producing the same. BACKGROUND ART [0002] Silver ink (silver paste) has been conventionally used not only for forming circuit boards by co-firing it with a ceramic substrate at a relatively high temperature but also for forming a wiring circuit on a printed wiring board, via-hole-fillers through such a board and adhesives for mounting electrical parts thereon by mixing and curing the silver ink (silver paste) with various types of resin ingredients, as described in the Patent Document 1. In the latter application, in general, an electrical conductivity has been obtained simply by mutually having the particles of silver powder touched, as a conductive filler without mutually sintering the particles. [0003] However, there have been a demand in recent years for lowering an electrical resistance for conductor portions formed using ...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B22F1/052B22F1/148B22F9/24C22B3/44C22B11/00H01L23/498H05K1/09
CPCB22F1/0014B22F1/0096B22F9/24B22F2999/00H01L2924/0002C22B11/04H01L23/49883H05K1/095H05K2201/0218C22B3/44B22F9/20B22F2202/11H01L2924/00Y02P10/20B22F1/052B22F1/148
Inventor SASAKI, TAKUYAKATO, MASASHIFUJIMOTO, TAKUSAKAUE, TAKAHIKOYOSHIMARU, KATSUHIKO
Owner MITSUI MINING & SMELTING CO LTD
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