Coated silver nanoparticles and manufacturing method therefor

• US 9,496,068 B2
• Filed: 03/31/2010
• Issued: 11/15/2016
• Est. Priority Date: 04/17/2009
• Status: Active Grant

• Current Assignee: National University Corporation Yamagata University
• Original Assignee: National University Corporation Yamagata University
• Inventors: Sakamoto, Masaomi, Kurihara, Masato
• Primary Examiner(s): Kopec, Mark
• Application Number:
  US13/264,204
• Publication Number:
  US 20120043510A1
• Time in Patent Office: 2,421 Days
• Field of Search: 252500-5216
• US Class Current: 1/1
• CPC Class Codes: B05D 5/12 to obtain a coating with specific electrical properties
• CPC Class Codes: B22F 1/0545 Dispersions or suspensions of nanosized particles
• CPC Class Codes: B22F 1/102 Metallic powder coated with organic material
• CPC Class Codes: B22F 2301/255 Silver or gold
• CPC Class Codes: B22F 2304/054 Particle size between 1 and 100 nm
• CPC Class Codes: B22F 2998/00 Supplementary information concerning processes or compositions relating to powder metallurgy
• CPC Class Codes: B22F 2999/00 Aspects linked to processes or compositions used in powder metallurgy
• CPC Class Codes: B22F 9/30 with decomposition of metal compounds, e.g. by pyrolysis
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C09D 5/24 Electrically-conducting paints conductive materials H01B1/00
• CPC Class Codes: H01B 1/22 the conductive material comprising metals or alloys
• CPC Class Codes: H05K 1/097 Inks comprising nanoparticles and specially adapted for being sintered at low temperature H05K1/095 takes precedence

Abstract

The present invention provides coated silver nanoparticles for use as an electrically conductive material capable of sintering at lower temperatures that is able to be used even with flexible printed substrates having low heat resistance, and a manufacturing method therefor. The coated silver nanoparticles of the present invention have a mean particle diameter of 30 nm or less and are coated with protective molecules amine, and are characterized in that the weight loss rate when heated to 160° C. in thermogravimetric measurement is 30% or more. The coated silver nanoparticles of the present invention are also characterized in that a silver-colored sintered film can be formed by sintering at a temperature of 100° C. or lower for 1 hour or less. These coated silver nanoparticles are manufactured by mixing a silver compound that forms metallic silver when decomposed by heating, an alkylamine and an alkyldiamine to prepare a complex compound, and by thermally decomposing the silver compound by heating the complex compound.

Claims

1. Coated silver nanoparticles having a mean particle diameter of 30 nm or less and coated with protective molecules, wherein the protective molecules contain as main components thereof a medium- to short-chain alkylamine having a boiling point within the range of 100°

C. to 250°

C. and a medium- to short-chain alkyldiamine having a boiling point within the range of 100°

C. to 250°

C., and

one of the amino groups possessed by the medium- to short-chain alkyldiamine is a tertiary amine.

2. A coated silver nanoparticle dispersion, comprising the coated silver nanoparticles according to claim 1 dispersed in a dispersion medium.

3. Coated silver nanoparticles having a mean particle diameter of 30 nm or less and coated with protective molecules, wherein the protective molecules contain as main components thereof a medium- to short-chain alkylamine having a boiling point within the range of 100°

C. to 250°

C. and a medium- to short-chain alkyldiamine having a boiling point within the range of 100°

C. 250°

C., and the protective molecules further contain a fatty acid.

4. A coated silver nanoparticle dispersion, comprising the coated silver nanoparticles according to claim 3 dispersed in a dispersion medium.

5. A method of manufacturing coated silver nanoparticles, comprising:

mixing a silver compound that forms metallic silver when decomposed by heating, a medium- to short-chain alkylamine having a boiling point of 100°

C. to 250°

C. and a medium- to short-chain alkyldiamine having a boiling point of 100°

C. to 250°

C. to prepare a complex compound; and

thermally decomposing the silver compound by heating the complex compound.

6. The manufacturing method of according to claim 5, wherein the silver compound that forms metallic silver when decomposed by heating is silver oxalate.

7. The manufacturing method of according to claim 5, wherein the content ratio of the alkyldiamine to the total amount of amines in the alkylamine and alkyldiamine mixed with the silver compound is 10 mol % to 90 mol %.

8. The manufacturing method according to claim 5, wherein further comprising admixing a fatty acid with the silver compound, alkylamine and alkyldiamine, wherein the amount of the fatty acid is at 5 mol % or less based on the silver atoms contained in the reaction system.