IP Library Granted Patent US 7,648,557
Granted Patent B2
US 7,648,557 · App. 11/809,486 · Granted Jan 19, 2010

Process for making highly dispersible spherical silver powder particles and silver particles formed therefrom

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Quick Facts
Patent No.
US 7,648,557
App. No.
11/809,486
Granted
Jan 19, 2010
Kind
B2
Abstract

Disclosed is an improved process for making highly dispersible, spherical silver particles. In particular, the invention is directed to a process for making silver particles, which are very high solids and highly ordered. The silver particles formed are particularly useful in electronic applications.

Claims (36)

1. A method for the formation of very high solids, highly ordered, finely divided, and controlled morphology silver powder particles comprising the sequential steps of:

(a) preparing an aqueous solution of a silver salt wherein said aqueous solution comprises a silver salt dissolved in de-ionized water;

(b) preparing a reducing solution comprising:

(i) de-ionized water;

(ii) nitric acid;

(iii) a reducing agent consisting of ascorbic acid;

(iv) a particle surface morphology modifier chosen from the group consisting of potassium sulfate, sodium sulfate, potassium phosphate, sodium phosphate, potassium carbonate and sodium carbonate;

(v) a surface modifier chosen from the group consisting of gum arabic, ammonium stearate, stearate salts, salts of polynaphthalene sulfonate formaldehyde condensate, polyetheylene glycol with molecular weight 2100 to 8000, and mixtures of these surfactants;

(vi) a particle modifier chosen from the group consisting of gold colloid, silver colloid and sodium borohydride; and

(c) mixing together the aqueous solution of silver salt and said reducing solution to form silver powder particles in a final aqueous solution wherein said final aqueous solution has a pH of less than or equal to 6.

2. The method of claim 1 further comprising the steps of:

d) separating said silver powder particles from said final aqueous solution;

e) providing deionized water;

f) washing the silver powder particles with said deionized water; and

g) drying said silver powder particles.

3. The method of claim 1 wherein said silver salt is silver nitrate.

4. The method of claim 1 wherein step (c) is performed at a temperature in the range of 10° C. to 35° C.

5. The method of claim 1 wherein step (c) is performed at a temperature in the range of 36° C. to 44° C.

6. The method of claim 1 wherein step (c) is performed at a temperature of greater than 45° C. and the silver powder particles are predominantly two dimensional flakes.

7. The method of claim 1 wherein said particle surface morphology modifier is potassium sulfate.

8. The method of claim 1 wherein said particle size modifier is a metal colloid.

9. The method of claim 1 wherein said surface modifier for making finely divided silver particles is gum arabic.

10. The method of claim 1 wherein the pH of said final aqueous solution is less than or equal to 2.

11. The use of the silver powder particles formed by the method of claim 1 , as electrically functional materials in a paste in thick film applications comprising:

forming a thick film consisting of electrically functional materials, inorganic binders, and solvents;

coating said paste on a substrate; and

firing said coated substrate to form a conductive circuit.

12. A method for the formation of very high solids, highly ordered, finely divided, and controlled morphology silver powder particles comprising the sequential steps of:

(a) preparing an aqueous nitric acid solution of a silver salt wherein said aqueous nitric acid solution comprises a silver salt;

(b) preparing a reducing solution comprising:

(i) de-ionized water;

(i) a reducing agent consisting of ascorbic acid;

(iii) a particle surface morphology modifier chosen from the group consisting of potassium sulfate, sodium sulfate, potassium phosphate, sodium phosphate, potassium carbonate and sodium carbonate;

(iv) a surface modifier chosen from the group consisting of gum arabic, ammonium stearate, stearate salts, salts of polynaphthalene sulfonate formaldehyde condensate, polyetheylene glycol with molecular weight 2100 to 8000, and mixtures of these surfactants;

(v) a particle modifier chosen from the group consisting of gold colloid, silver colloid and sodium borohydride; and

(c) mixing together the aqueous nitric acid solution of silver salt and said reducing solution to form silver powder particles in a final aqueous solution wherein said final aqueous solution has a pH of less than or equal to 6.

Assignments (3)
CHANGE OF NAME Recorded Mar 20, 2025
From: DU PONT CHINA LIMITED
To: CELANESE MERCURY HOLDINGS INC.
Reel/Frame 070567/0231 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 20, 2022
From: DUPONT ELECTRONICS, INC.
To: DU PONT CHINA LIMITED
Reel/Frame 062173/0299 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 25, 2019
From: E. I. DU PONT DE NEMOURS AND COMPANY
To: DUPONT ELECTRONICS, INC.
Reel/Frame 049583/0269 →