Fine silver particle ink, fine silver particle sintered body, and method for producing fine silver particle ink

Patent metadata

Field	Value
Publication number	US-9674953-B2
Application number	US-201314614196-A
Country	US
Kind code	B2
Filing date	Jul 11, 2013
Priority date	Aug 7, 2012
Publication date	Jun 6, 2017
Grant date	Jun 6, 2017

Abstract

Provided are a fine silver particle ink composed of hexylamine, dodecylamine, oleic acid, fine silver particles and a solvent, in which the volume resistivity of a sintered body at 100° C. obtained after the ink is applied on a substrate by spin coating is 8 to 25 μΩcm, a sintered body thereof, and a method for producing a fine silver particle ink. When a fine silver particle ink containing coated fine silver particles is produced by a silver-amine complex decomposition method, production can be carried out smoothly. The fine silver particle ink can be sintered even at a low temperature, and a sintered body thereof has a mirror surface and low volume resistance.

First claim

The invention claimed is:

1. A method for producing a silver particle ink, the method comprising:
a first step of kneading silver oxalate and N,N-dimethyl-1,3-diaminopropane;
a second step of kneading the kneading product obtained in the first step with hexylamine, dodecylamine and oleic acid, and thereby forming a silver complex;
a third step of heating and stirring the silver complex, and thereby producing fine silver particles; and
a dispersion step of dispersing the fine silver particles obtained in the third step in a solvent to form an ink, wherein the silver oxalate is wetted with 30 to 200 wt % of a solvent in advance.

2. The method for producing a silver particle ink according to claim 1 , wherein the silver oxalate comprises, as a silver raw material, a silver oxalate that has been wetted with an organic solvent which has a boiling point of 60° C. to 230° C. and does not contain a halogen compound, in an amount in the range of 30 to 200 wt %.

3. The method for producing a silver particle ink according to claim 1 , wherein the heating and stirring in the third step is continued until the silver complex turns black, and gas bubbles are no longer generated from the reaction system.

4. The method for producing a silver particle ink according to claim 1 , the method comprising a centrifugation step that includes at least two iterations of a process of separating the N, N-dimethyl-1, 3-diaminopropane, hexylamine, dodecylamine and oleic acid that are not adsorbed to the fine silver particles as protective agents, by adding an alcohol to a matrix containing the fine silver particles produced in the third step, centrifuging the matrix, and then removing the supernatant.

5. The method for producing a silver particle ink according to claim 3 , the method comprising a centrifugation step that includes at least two iterations of a process of separating the N, N-dimethyl-1, 3-diaminopropane, hexylamine, dodecylamine and oleic acid that are not adsorbed to the fine silver particles as protective agents, by adding an alcohol to a matrix containing the fine silver particles produced in the third step, centrifuging the matrix, and then removing the supernatant.

6. The method of producing a silver particle ink according to claim 2 , the method comprising a centrifugation step that includes at least two iterations of a process of separating the N, N-dimethyl-1, 3-diaminopropane, hexylamine, dodecylamine and oleic acid that are not adsorbed to the fine silver particles as protective agents, by adding an alcohol to a matrix containing the fine silver particles produced in the third step, centrifuging the matrix, and then removing the supernatant.

Assignees

• Tanaka Precious Metal Ind

Inventors

• Kubo Hitoshi
• Ohshima Yusuke
• Nakamura Noriaki
• Noguchi Hiroshi
• Taniuchi Junichi
• Makita Yuichi

Classifications

• B22F1/102 Primary

  Metallic powder coated with organic material · CPC title

• B22F1/103

  containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent · CPC title

• C09D11/52 Primary

  Electrically conductive inks · CPC title

• H05K1/097 Primary

  Inks comprising nanoparticles and specially adapted for being sintered at low temperature (H05K1/095 takes precedence) · CPC title

• B22F2001/0066

  Operations & Transport · mapped topic