Granted Patent B2

US 8,834,965 · App. 12/369,861 · Granted Sep 16, 2014

Abstract

Claims (37)

1. A process for producing organoamine-stabilized silver nanoparticles, comprising:

forming a heated solution at a first temperature comprising an organic solvent and a first amount of organoamine;

adding silver salt particles to the heated solution;

adding a second amount of organoamine to the heated solution containing the organic solvent, first amount of organoamine, and the silver salt particles, wherein the weight ratio of the first amount of organoamine to the second amount of organoamine is about 1:1;

cooling the heated solution to a second temperature that is lower than the first temperature;

adding an organohydrazine to the heated solution containing the organic solvent, first amount of organoamine, silver salt particles, and the second amount of organoamine; and

reacting the solution containing the organic solvent, first amount of organoamine, silver salt particles, second amount of organoamine, and organohydrazine to form organoamine-stabilized silver nanoparticles;

wherein the organoamine is hexadecylamine, the silver salt is silver acetate, and the organic solvent is toluene;

wherein the organoamine-stabilized silver nanoparticles have a silver content of 81 wt % to 84 wt %; and

wherein when a film is made by annealing a solution containing the organoamine-stabilized silver nanoparticles and having a shelf life of 30 days or more at 140° C. for 10 minutes, the film has a conductivity of from 27560 S/cm to 29350 S/cm.

2. The process of claim 1 , wherein the molar ratio of total organoamine to silver salt is from about 1:1 to about 15:1.

3. The process of claim 1 , wherein the first temperature is from about 50° C. to about 80° C.

4. The process of claim 1 , wherein the solution is cooled over a period of about 30 minutes or more.

5. The process of claim 1 , wherein the second temperature is from about 45° C. to about 60° C.

6. The process of claim 1 , wherein the weight ratio of organic solvent to the first amount of organoamine is about 1:1.

7. The process of claim 1 , wherein the organohydrazine is of the formula:

R 6 R 7 N—NR 8 R 9

wherein R 6 , R 7 , R 8 and R 9 are independently selected from hydrogen, alkyl, and aryl; and wherein at least one of R 6 , R 7 , R 8 and R 9 is not hydrogen.

8. The process of claim 1 , wherein the resulting nanoparticles have an average diameter of from about 2 nanometers to about 8 nanometers.

9. The process of claim 1 , wherein the resulting nanoparticles have a particle size distribution of about 10 nanometers.

10. The process of claim 1 , further comprising:

separating the silver nanoparticles from the solution by adding isopropanol and a non-solvent to the solution; and

washing the silver nanoparticles.

11. The process of claim 10 , wherein the non-solvent comprises acetone, methanol, ethanol, propanol, methyl ethyl ketone, acetonitrile, isobutyl alcohol, and combinations thereof.

12. The process of claim 10 , wherein the volume ratio of isopropanol to non-solvent is about 0.4:1.

13. A process for producing organoamine-stabilized silver nanoparticles, comprising:

forming a solution comprising an organic solvent and a first amount of organoamine and having a first temperature of from about 50° C. to about 80° C.;

adding silver salt particles to the solution;

adding a second amount of organoamine to the solution, wherein the weight ratio of the first amount of organoamine to the second amount of organoamine is about 1:1;

cooling the solution containing the organic solvent, first amount of organoamine, silver salt particles, and second amount of organoamine down to a second temperature of from about 45° C. to about 60° C.;

adding an organohydrazine to the solution;

reacting the solution containing the organic solvent, first amount of organoamine, silver salt particles, second amount of organoamine, and organohydrazine to form organoamine-stabilized silver nanoparticles for a time period of from about 5 minutes to about 2 hours;

cooling the solution down to a third temperature of from about 35° C. to about 50° C.;

adding isopropanol to the solution;

adding a non-solvent to the solution to separate the silver nanoparticles from the solution; and

washing the silver nanoparticles;

wherein the organoamine is hexadecylamine, the silver salt is silver acetate, and the organic solvent is toluene.

Assignments (10)