Safe method for manufacturing silver nanoparticle inks
View Patent ↗In an embodiment, there is a method of preparing a conductive ink formulation. The method can include dissolving a stabilizer in a first solvent, adding a reducing agent to the first solvent, adding a metal salt to the first solvent and forming a slurry by precipitating stabilized metal nanoparticles in the first solvent. The method can also include forming a wet cake of the stabilized metal nanoparticles and adding the wet cake to a second solvent. The second solvent can include at least one of a polyvinyl alcohol derivative. The wet cake may not be actively dried prior to being added to the second solvent.
1. A method of preparing a conductive ink formulation, the method comprising:
dissolving a stabilizer in a first solvent;
adding a reducing agent to the first solvent;
adding a metal salt to the first solvent;
forming a slurry by precipitating stabilized metal nanoparticles in the first solvent;
forming a wet cake of the stabilized metal nanoparticles from at least a portion of the slurry, the wet cake comprising from about 8 wt % to about 25 wt % of volatiles; and
adding the wet cake to a second solvent, the second solvent comprising at least one of a polyvinyl alcohol derivative,
wherein the wet cake is not actively dried prior to being added to the second solvent.
2. The method of preparing a conductive ink formulation of claim 1 , wherein the metal nanoparticles comprise at least one metal selected from the group consisting of Al, Au, Pt, Pd, Cu, Co, Cr, In, and Ni nanoparticles.
3. The method of preparing a conductive ink formulation of claim 1 , wherein the wet cake added to the second solvent forms an ink composition comprising a viscosity of from about 2 cps to about 200 cps.
4. The method of preparing a conductive ink formulation of claim 1 , wherein the metal nanoparticles comprise at least one selected from the group consisting of Au—Ag, Ag—Cu, Ag—Ni, Au—Cu, Au—Ni, Au—Ag—Cu, and Au—Ag—Pd metal nanoparticles composites.
5. The method of preparing a conductive ink formulation of claim 1 , wherein the metal nanoparticles are not stored as a powder prior to being added to the second solvent.
6. The method of preparing a conductive ink formulation of claim 1 , wherein the reducing agent comprises a phenylhydrazine.
7. The method of preparing a conductive ink formulation of claim 1 , wherein the metal salt comprises a silver salt.
8. The method of preparing a conductive ink formulation of claim 1 , wherein the metal salt comprises silver acetate.
9. The method of preparing a conductive ink formulation of claim 1 , wherein the stabilized nanoparticles are organoamine stabilized silver nanoparticles.
10. The method of preparing a conductive ink formulation of claim 1 , wherein the stabilizer comprises dodecylamine.
11. The method of preparing a conductive ink formulation of claim 1 , wherein at least one of the first and the second solvent comprise a mixed solvent composition.
12. The method of preparing a conductive ink formulation of claim 1 , wherein at least one of the first and the second solvent comprises a mixture comprised of a solvent selected from the group consisting of terpineol, hexanol, heptanol, cyclohexanol, 3,7-dimethylocta-2,6-dien-1ol, 2-(2-propyl)-5-methyl-cyclohexane-1-ol, and at least one hydrocarbon solvent selected from the group consisting of decalin, hexadecane, hexadecene, and 1,2,4-trimethylbenzene.
13. The method of preparing a conductive ink formulation of claim 1 , wherein at least one of the first and the second solvent consists essentially of decalin and methanol.
14. The method of preparing a conductive ink formulation of claim 1 , wherein the metal salt is added to the first solvent before the reducing agent is added to the first solvent.
15. The method of preparing a conductive ink formulation of claim 1 , wherein the reducing agent is added to the first solvent before the metal salt is added to the first solvent.
16. A method of preparing a conductive ink formulation, comprising:
reacting a metal salt with a reducing agent in a first solvent that contains a stabilizer to form a stabilized metal nanoparticle slurry;
forming a wet cake of stabilized metal nanoparticles from at least a portion of the stabilized metal nanoparticle slurry, wherein the wet cake of stabilized metal nanoparticles comprises from about 8 wt % to about 25 wt % of volatiles; and
adding the wet cake to a second solvent that contains a polyvinyl alcohol derivative,
wherein the wet cake is not actively dried prior to being added to the second solvent.
17. The method of preparing a conductive ink formulation of claim 16 further comprising dispersing the metal nanoparticles of the metal nanoparticle wet cake in decalin.
18. The method of preparing a conductive ink formulation of claim 16 , wherein the nanoparticle ink comprises from about 30 wt % to about 40 wt % silver.
19. The method of preparing a conductive ink formulation of claim 1 , wherein the wet cake comprises from about 10 wt % to about 17 wt % of volatiles.
20. The method of preparing a conductive ink formulation of claim 1 , wherein the wet cake comprises from about 13 wt % to about 15 wt % of volatiles.