Method for producing silver nanoparticles, silver nanoparticles, and silver coating composition

Patent metadata

Field	Value
Publication number	US-9860983-B2
Application number	US-201314371462-A
Country	US
Kind code	B2
Filing date	Jan 7, 2013
Priority date	Jan 11, 2012
Publication date	Jan 2, 2018
Grant date	Jan 2, 2018

Abstract

The present invention provides silver nano-particles with excellent stability and conductivity by low-temperature calcining, a producing method for same, and a silver coating composition. A method for producing silver nano-particles comprising: preparing an amine mixture liquid comprising: an aliphatic hydrocarbon monoamine (A) with an aliphatic hydrocarbon group and one amino group, the aliphatic hydrocarbon group having 6 or more carbon atoms in total; an aliphatic hydrocarbon monoamine (B) with an aliphatic hydrocarbon group and one amino group, the aliphatic hydrocarbon group having 5 or less carbon atoms in total; and an aliphatic hydrocarbon diamine (C) with an aliphatic hydrocarbon group and two amino groups, the aliphatic hydrocarbon group having 8 or less carbon atoms in total; mixing a silver compound and the amine mixture liquid to form a complex compound; and thermally decomposing the complex compound by heating to form silver nano-particles.

First claim

The invention claimed is:

1. Coated silver nano-particles produced by a method comprising:
(a) preparing an amine mixture liquid comprising:
(i) an aliphatic hydrocarbon monoamine (A) comprising an aliphatic hydrocarbon group and one amino group, said aliphatic hydrocarbon group having 6 or more carbon atoms in total,
(ii) an aliphatic hydrocarbon monoamine (B) comprising an aliphatic hydrocarbon group and one amino group, said aliphatic hydrocarbon group having 2 or more and 4 or less carbon atoms in total, and
(iii) an aliphatic hydrocarbon diamine (C) comprising an aliphatic hydrocarbon group and two amino groups, said aliphatic hydrocarbon group having 7 or less carbon atoms in total wherein aliphatic hydrocarbon diamine (C) is represented by a structural formula:
R 1 R 2 N—R—NH 2

wherein R represents a bivalent ethylene or propylene group, R 1 and R 2 may be the same or different from each other and each represent a methyl or an ethyl group, and the total number of carbon atoms of R, R 1 , and R 2 is 7 or less,
(b) mixing a silver compound and the amine mixture liquid to form a complex compound comprising the silver compound and the amines; and
(c) thermally decomposing the complex compound by heating to form coated silver nano-particles,
wherein each of the aliphatic hydrocarbon amine (A), the aliphatic hydrocarbon amine (B), and the aliphatic hydrocarbon diamine (C) does not have, on its hydrocarbon group, a hetero atom, and
wherein a surface of the coated silver nano-particles comprises a protective agent, comprising the aliphatic hydrocarbon monoamine (A), the aliphatic hydrocarbon monoamine (B) and the aliphatic hydrocarbon diamine (C).

2. The coated silver nano-particles according to claim 1 , wherein the silver compound is silver oxalate.

3. The coated silver nano-particles according to claim 1 , wherein the aliphatic hydrocarbon monoamine (A) is contained in the amine mixture liquid in step (a) in an amount of 10 mol % to 65 mol % of a total of the aliphatic hydrocarbon monoamine (A), the aliphatic hydrocarbon monoamine (B), and the aliphatic hydrocarbon diamine (C).

4. The coated silver nano-particles according to claim 1 , wherein the aliphatic hydrocarbon monoamine (B) is contained in the amine mixture liquid in step (a) in an amount of 5 mol% to 50 mol % of a total of the aliphatic hydrocarbon monoamine (A), the aliphatic hydrocarbon monoamine (B), and the aliphatic hydrocarbon diamine (C).

5. The coated silver nano-particles according to claim 1 , wherein the aliphatic hydrocarbon diamine (C) is contained in the amine mixture liquid in step (a) in an amount of 15 mol % to 50 mol % of a total of the aliphatic hydrocarbon monoamine (A), the aliphatic hydrocarbon monoamine (B), and the aliphatic hydrocarbon diamine (C).

6. The coated silver nano-particles according to claim 1 , wherein the aliphatic hydrocarbon monoamine (A), the aliphatic hydrocarbon monoamine (B), and the aliphatic hydrocarbon diamine (C) are used in step (a) in a total amount of 1 to 20 moles per mole of silver atoms in the silver compound.

7. The coated silver nano-particles according to claim 1 , wherein an aliphatic carboxylic acid (D) is added to the amine mixture liquid in step (a), and wherein the protective agent comprised on the surface of the coated silver nano-particles further comprises the aliphatic carboxylic acid (D).

8. A silver coating composition comprising the coated silver nano-particles of claim 1 , and an organic solvent.

9. A silver coating composition comprising the coated silver nano-particles of claim 7 , and an organic solvent.

10. The coated silver nano-particles according to claim 1 ,
wherein the aliphatic hydrocarbon diamine (C) comprises an aliphatic hydrocarbon group and two amino groups, said aliphatic hydrocarbon group having 6 or less carbon atoms in total wherein aliphatic hydrocarbon diamine (C) is represented by a structural formula:
R 1 R 2 N—R—NH 2

 wherein R represents a bivalent ethylene or propylene group, R 1 and R 2 may be the same or different from each other and each represent a methyl or an ethyl group, and the total number of carbon atoms of R, R 1 , and R 2 is 6 or less.

11. A silver coating composition comprising the coated silver nano-particles of claim 10 , and an organic solvent.

12. Coated silver nano-particles produced by a method comprising:
(a) preparing a mixture liquid comprising:
(i) an aliphatic hydrocarbon monoamine (A) comprising a saturated aliphatic hydrocarbon group and one primary amino group, said aliphatic hydrocarbon group having 6 or more and 18 or less carbon atoms in total,
(ii) an aliphatic hydrocarbon monoamine (B) comprising an aliphatic hydrocarbon group and one primary amino group, said aliphatic hydrocarbon group having 3 or more and 4 or less carbon atoms in total, and
(iii) an aliphatic hydrocarbon diamine (C) comprising an aliphatic hydrocarbon group and two amino groups, said aliphatic hydrocarbon group having 6 or less carbon atoms in total wherein aliphatic hydrocarbon diamine (C) is represented by a structural formula:
R 1 R 2 N—R—NH 2

 wherein R represents a bivalent ethylene or propylene group, R 1 and R 2 may be the same or different from each other and each represent a methyl or an ethyl group, and the total number of carbon atoms of R, R 1 , and R 2 is 6 or less,
(iv) an aliphatic carboxylic acid (D) that is a saturated or unsaturated monocarboxylic acid having 8 to 18 carbon atoms;
(b) mixing a silver compound and the mixture liquid to form a complex compound comprising the silver compound and the amines; and
(c) thermally decomposing the complex compound by heating to form coated silver nano-particles,
wherein each of the aliphatic hydrocarbon amine (A), the aliphatic hydrocarbon amine (B), and the aliphatic hydrocarbon diamine (C) does not have, on its hydrocarbon group, a hetero atom, and
wherein a surface of the coated silver nano-particles comprises a protective agent, comprising the aliphatic hydrocarbon monoamine (A), the aliphatic hydrocarbon monoamine (B), the aliphatic hydrocarbon diamine (C) and the aliphatic carboxylic acid (D).

Assignees

• Univ Yamagata Nat Univ Corp
• Daicel Corp

Inventors

• Kurihara Masato
• Okamoto Kazuki
• Iguchi Yuki

Classifications

• B22F1/142

  Thermal or thermo-mechanical treatment · CPC title

• B22F1/054

  Nanosized particles · CPC title

• B22F1/0545

  Dispersions or suspensions of nanosized particles · CPC title

• B22F1/107

  containing organic material comprising solvents, e.g. for slip casting · CPC title

• B22F1/102

  Metallic powder coated with organic material · CPC title