IP Library Granted Patent US 8,765,862
Granted Patent B2
US 8,765,862 · App. 13/581,800 · Granted Jul 1, 2014

Metal nanoparticle composite and production method thereof

Inventors: Yasufumi Matsumura (Chiba, JP); Ryuzo Shinta (Chiba, JP); Yasushi Enomoto (Chiba, JP)
Assignee: Nippon Steel & Sumikin Chemical Co., Ltd.
C08J7/00C08J7/08C08J7/14C08K3/08C08L79/08Y10S977/90Y10S977/778
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Quick Facts
Patent No.
US 8,765,862
App. No.
13/581,800
Granted
Jul 1, 2014
Kind
B2
Abstract

A metal nanoparticle composite is provided, in which a matrix resin layer and metal nanoparticles are immobilized on the matrix resin layer. The metal nanoparticle composite has the following characteristics: a) the metal nanoparticles are obtained by heat-reducing metal ions or metal salts contained in the matrix resin layer or a precursor resin layer thereof; b) the metal nanoparticles exist within a region from the surface of the matrix resin layer to a depth of at least 50 nm; c) particle diameters of the metal nanoparticles are in the range of 1 nm to 100 nm with the mean particle diameter of greater than and equal to 3 nm; and d) a spacing between adjacent metal nanoparticles is greater than and equal to the particle diameter of a larger one of the adjacent metal nanoparticles.

Claims (24)

1. A metal nanoparticle composite, comprising:

a matrix resin layer and metal nanoparticles immobilized on the matrix resin layer, the metal nanoparticles are formed by metals selected from the group consist of gold (Au), silver (Ag), copper (Cu), palladium (Pd), platinum (Pt), tin (Sn), rhodium (Rh), and iridium (Ir) and the metal nanoparticle composite comprising following structures a to e:

a) the metal nanoparticles obtained through heat-reducing metal ions or metal salts contained in the matrix resin layer or a precursor resin layer thereof;

b) the metal nanoparticles being present within a range from a surface of the matrix resin layer to a depth of at least 50 nm;

c) particle diameters (D) of the metal nanoparticles in a range of 1 nm to 100 nm with a mean particle diameter of greater than and equal to 3 nm; and

d) a spacing between adjacent metal nanoparticles is greater than and equal to the particle diameter of a larger one of the adjacent metal nanoparticles;

e) the metal nanoparticles interact with light of a wavelength greater than and equal to 380 nm, for generating a local surface plasmon resonance.

2. The metal nanoparticle composite according to claim 1 , wherein a volume fraction of the metal nanoparticles relative to the metal nanoparticle composite is in a range of 0.05% to 23%.

3. The metal nanoparticle composite according to claim 1 , wherein the matrix resin layer further comprises a polyimide resin.

4. The metal nanoparticle composite according to claim 3 , wherein the polyimide resin is transparent or colorless.

5. The metal nanoparticle composite according to claim 3 , wherein the matrix resin layer is obtained by coating a polyamic acid resin solution on a substrate and drying to form a polyamic acid resin film, and imidizing the polyamic acid resin film.

6. The metal nanoparticle composite according to claim 5 , wherein the polyamic acid resin solution contains a metal compound to be used as a raw material of the metal nanoparticles.

7. The metal nanoparticle composite according to claim 6 , wherein the particle diameters of the metal nanoparticles are in a range of 30 nm to 100 nm.

8. The metal nanoparticle composite according to claim 5 , wherein the polyamic acid resin film is impregnated with a solution containing the metal ions or a metal compound to be used as a raw material of the metal nanoparticles, and is imidized to form the metal nanoparticle composite.

9. The metal nanoparticle composite according to claim 3 , wherein the matrix resin layer is obtained by performing alkali modification on a surface of a polyimide film to form a polyamic acid resin layer, and imidizing the polyamic acid resin layer.

10. The metal nanoparticle composite according to claim 9 , wherein the polyamic acid resin layer is impregnated with a solution containing the metal ions or a metal compound to be used as a raw material of the metal nanoparticles, and is imidized to form the metal nanoparticle composite.

11. The metal nanoparticle composite according to claim 1 where, a specified pattern is formed on a substrate to form the metal nanoparticle composite.

12. A production method of a metal nanoparticle composite, wherein metal nanoparticles interacting with light of a wavelength greater than and equal to 380 nm for generating a local surface plasmon resonance, and metal nanoparticles with a mean particle diameter in a polyimide resin in a range of 20 nm to 30 nm do not contact with each other, and are independently dispersed in the metal nanoparticle composite, the metal nanoparticles are formed by metals selected from the group consist of gold (Au), silver (Ag), copper (Cu), palladium (Pd), platinum (Pt), tin (Sn), rhodium (Rh), andiridium (Ir), the production method of a metal nanoparticle composite comprising following Step A and Step B:

A) performing a step of coating a coating liquid containing polyamic acid resin and a metal compound on a substrate, wherein a content of a metal component is in a range of 1 μg/cm 2 to 30 μg/cm 2 , and drying to form a dried coating film with a thickness in a range of 30 nm to 1.7 μm; and

B) performing a step of heat treatment on the coating film at a temperature in the range of 200° C. to 450° C., precipitating the metal nanoparticles by reducing metal ions (or metal salts) in the coating film to disperse the metal nanoparticles in the coating film, and imidizing the polyamic acid resin in the coating film to form a polyimide resin layer with a thickness in a range of 25 nm to 1 μm.

13. The production method of a metal nanoparticle composite according to claim 12 , wherein a spacing between two adjacent metal nanoparticles is greater than and equal to a particle diameter of a larger one of the two adjacent metal nanoparticles.

14. The production method of a metal nanoparticle composite according to claim 12 , wherein a volume fraction of the metal nanoparticles relative to the metal nanoparticle composite is in a range of 1% to 10%.

15. The production method of a metal nanoparticle composite according to claim 12 , where the Step B is performed in an inert gas atmosphere.

16. The production method of a metal nanoparticle composite according to claim 12 , the metal compound is a precursor of Au.

Assignments (3)
MERGER Recorded Oct 21, 2020
From: NIPPON STEEL & SUMIKIN MATERIALS CO., LTD.; NIPPON STEEL & SUMIKIN CHEMICAL CO., LTD.
To: NIPPON STEEL CHEMICAL & MATERIAL CO., LTD.
Reel/Frame 054145/0400 →
CHANGE OF NAME Recorded Mar 20, 2013
From: NIPPON STEEL CHEMICAL CO., LTD.
To: NIPPON STEEL & SUMIKIN CHEMICAL CO., LTD.
Reel/Frame 030049/0771 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 31, 2012
From: MATSUMURA, YASUFUMI; SHINTA, RYUZO; ENOMOTO, YASUSHI
To: NIPPON STEEL CHEMICAL CO., LTD.
Reel/Frame 028879/0975 →
Priority Claims (2)
JP 2010-044108 · Mar 1, 2010 · national
JP 2010-083118 · Mar 31, 2010 · national
Continuity (1)
Related Publication 20120329935A1 · Dec 27, 2012