A process for producing sub-micron-sized copper powder comprising the steps of: providing a precursor composition comprising a solution of copper monoethanolamine complex; and heating the precursor composition to a temperature wherein copper monoethanolamine complex is converted to copper powder. A
A process for producing sub-micron-sized copper powder comprising the steps of: providing a precursor composition comprising a solution of copper monoethanolamine complex; and heating the precursor composition to a temperature wherein copper monoethanolamine complex is converted to copper powder. A process for producing nickel powder comprising the steps of: providing a precursor composition comprising a solution of nickel monoethanolamine complex; and heating the precursor composition to a temperature wherein nickel monoethanolamine complex is converted to nickel powder.
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The invention claimed is: 1. A process for producing micron-sized to sub-micron-sized copper powder comprising the steps of: 1) providing an aqueous precursor composition comprising a solution of more than 5% copper ions, more than 10% water, and more than 20% monoethanolamine, by weight, with the
The invention claimed is: 1. A process for producing micron-sized to sub-micron-sized copper powder comprising the steps of: 1) providing an aqueous precursor composition comprising a solution of more than 5% copper ions, more than 10% water, and more than 20% monoethanolamine, by weight, with the proviso that there is less than 0.8 moles of a low molecular weight organic acid selected from the group consisting of formic acid, acetic acid, and oxalic acid per mole of copper ions; and 2) heating the precursor composition to a temperature wherein the copper ions are converted to copper powder, said powder having greater than 90% by weight copper and having a mean diameter of between about 0.02 microns and about 5 microns. 2. The process of claim 1 wherein the temperature is between 130° C. and 155° C. 3. The process of claim 1 wherein the composition comprises less than 0.4 moles of low molecular weight organic acid selected from the group consisting of formic acid, acetic acid, and oxalic acid per mole of copper ions. 4. The process of claim 1 wherein the composition comprises less than 0.4 moles total of a low molecular weight organic acid selected from the group consisting of formic acid and oxalic acid and of hydrazine per mole of copper ions. 5. The process of claim 1 wherein the composition is substantially free of a low molecular weight organic acid selected from the group consisting of formic acid, acetic acid, and oxalic acid and of hydrazine. 6. The process of claim 1 wherein at least a portion of the copper ions in the precursor composition are in the form of particles of copper salts, copper hydroxides, copper oxides, or mixtures or combinations thereof. 7. The process of claim 1 wherein the mole ratio of monoethanolamine to copper ions is at least 1.5:1 and wherein the aqueous precursor composition comprises between 15% and 60% of water. 8. The process of claim 1 wherein the powder has a mean diameter of between about 0.2 microns and about 1.3 microns. 9. The process of claim 1 wherein there is less than 0.4 moles hydrazine is present per mole of copper ions in the precursor composition. 10. The process of claim 1 wherein the precursor composition comprises less than 0.1 moles of a low molecular weight organic acid selected from the group consisting of formic acid, acetic acid, and oxalic acid per mole of copper ions and wherein the aqueous precursor composition comprises between 15% and 60% of water. 11. The process of claim 1 wherein the precursor composition is substantially free of low a molecular weight organic acid selected from the group consisting of formic acid and oxalic acid. 12. The process of claim 1 wherein the heating is to a temperature between about 95° C. and about 150° C. 13. The process of claim 1 wherein at least one mole of monoethanolamine is consumed by the reduction process per mole of copper powder formed. 14. The process of claim 1, wherein the precursor composition comprises more than 12% copper, more than 25% monoethanolamine, between 15% and 60% of water, and more than 0.2% of a counterion, wherein less than one half the equivalents of the counterion are low molecular weight organic acids selected from the group consisting of formic acid, acetic acid, and oxalic acid. 15. A process for producing micron-sized to sub-micron-sized copper powder comprising the steps of: 1) providing a precursor composition comprising at least 10% water by weight, copper ions and monoethanolamine, with the proviso that the mole ratio of ethanolamine to copper ions is at least 1 and there is less than 0.4 moles total of a low molecular weight organic acid and hydrazine per mole of copper ions, wherein the low molecular weight organic acid has a molecular weight equal to or less than that of oxalic acid ; and 2) heating the precursor composition to a temperature wherein the copper ions are converted to copper powder, said powder having greater than 90% by weight copper and having a mean diameter of between about 0.02 microns and about 5 microns. 16. The process of claim 15 wherein no common reducing agents selected from the group consisting of formic acid, oxalic acid, and hydrazine are added to the precursor composition. 17. The process of claim 15 wherein the precursor composition comprises less than 0.1 moles of low molecular weight organic acid having a molecular weight equal to or less than that of oxalic acid per mole of dissolved copper ions. 18. The process of claim 15 wherein the precursor composition is substantially free of low molecular weight organic acid having a molecular weight equal to or less than that of oxalic acid. 19. The process of claim 15 wherein the heating is to a temperature between about 95° C. and about 150° C. 20. The process of claim 15 wherein at least one mole of monoethanolamine is consumed by the reduction process per mole of copper powder formed. 21. A process for producing micron-sized to sub-micron-sized copper powder comprising the steps of: 1) providing a precursor composition consisting essentially of copper ions, monoethanolamine, an inorganic counterion, at least 10% by weight of water, and optionally an reducing sugar, wherein the mole ratio of monoethanolamine to copper ions is at least 1:1; and 2) heating the precursor composition to a temperature wherein copper ions are converted to copper powder, said powder having greater than 90% by weight copper and having a mean diameter of between about 0.02 microns and about 5 microns. 22. The process of claim 21 wherein no common reducing agents selected from the group consisting of formic acid, oxalic acid, and hydrazine are added to the precursor composition. 23. The process of claim 22 wherein the precursor composition comprises less than 0.1 moles of a low molecular weight organic acid per mole of copper ions, wherein the low molecular weight organic acid has a molecular weight equal to or less than that of oxalic acid. 24. The process of claim 22 wherein the precursor composition is substantially free of low molecular weight organic acid selected from the group consisting of formic acid, acetic acid, and oxalic acid. 25. The process of claim 22 wherein the heating is to a temperature between about 95° C. and about 150° C. 26. The process of claim 22 wherein the precursor composition comprises between 2.5 and about 4 moles of monoethanolamine per mole of copper, and wherein at least one mole of monoethanolamine is consumed by the reduction process per mole of copper powder formed. 27. The process of claim 22 wherein the mole ratio of monoethanolamine to copper ions is at least 1.5:1. 28. A process for producing micron-sized to sub-micron-sized metal powder comprising the steps of: 1) providing a precursor composition comprising at least 10% by weight of water, monoethanolamine-reducible metal ions and monoethanolamine, wherein the monoethanolamine-reducible metal ions each have a standard reduction potential from about-0.30 volts to about 0.6 volts in water solution at 25° C., and wherein the mole ratio of monoethanolamine to monoethanolamine-reducible metal ions is at least 1:1, with the proviso that the precursor composition comprises less than 0.8 moles total of metal-reducing-organic acids and of hydrazine per mole of monoethanolamine-reducible metal ions; and 2) heating the precursor composition to a temperature wherein the metal ions are converted to metal powder, said powder having a mean diameter of between about 0.02 microns and about 5 microns. 29. The process of claim 28 wherein the temperature is between 130° C. and about 150° C. 30. The process of claim 28 wherein the composition comprises less than 0.8 moles of metal-reducing-organic acids per mole of monoethanolamine-reducible metal ions. 31. The process of claim 28 wherein the composition comprises less than 0.4 moles total of metal-reducing-organic acids and of hydrazine per mole of monoethanolamine-reducible metal ions. 32. The process of claim 28 wherein at least half of the moles of monoethanolamine-reducible metal ions comprise copper ions, nickel ions, or both. 33. The process of claim 28 wherein at least a portion of the monoethanolamine-reducible metal ions in the precursor composition are in the form of particles of metal salts, metal hydroxides, metal oxides, or mixtures or combinations thereof 34. The process of claim 28 wherein the mole ratio of monoethanolamine to monoethanolamine-reducible metal ions is at least 1.5:1 and wherein the precursor composition comprises from 15% to 60% water. 35. The process of claim 28 wherein the powder has a mean diameter of between about 0.2 microns and about 1.3 microns. 36. A process for producing micron-sized to sub-micron-sized nickel powder comprising the steps of: 1) providing a precursor composition comprising more than 10% by weight of water, nickel ions and monoethanolamine, wherein the mole ratio of monoethanolamine to nickel ions is at least 1:1, with the proviso that the precursor composition comprises less than 0.8 moles total of nickel-reducing-organic acids and of hydrazine per mole of monoethanolamine-reducible nickel ions and 2) heating the precursor composition to a temperature wherein the nickel monoethanolamine complex is converted to nickel powder. 37. The process of claim 36 wherein the temperature is between 130° C. and about 155° C. 38. The process of claim 36 wherein the composition comprises less than 0.8 moles of nickel-reducing-organic acids per mole of nickel ions. 39. The process of claim 36 wherein the composition comprises less than 0.4 moles total of nickel-reducing-organic acids and of hydrazine per mole of nickel ions. 40. The process of claim 36 wherein at least a portion of the nickel ions in the precursor composition are in the form of particles of metal salts, metal hydroxides, metal oxides, or mixtures or combinations thereof. 41. The process of claim 36 wherein the mole ratio of monoethanolamine to nickel ions is at least 1.5:1. 42. The process of claim 36 wherein the powder has a mean diameter of between about 0.2 microns and about 1.3 microns.
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이 특허에 인용된 특허 (9)
Parr William J. E. (Naperville IL) Hutton Ronald E. (Faversham IL GB2) Moy Paul Y. Y. (Des Plaines IL) Frank Dieter (Naperville IL) Strawser David A. (Prospect Heights IL), Conductive metallization of substrates via developing agents.
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