Method of producing fine-particle copper powders
View Patent ↗Methods for producing finely divided copper or copper alloy powders are described, from compositions containing metal ions and an alkanolamine, preferably monoethanolamine, wherein the alkanolamine acts as a primary reducing agent. In preferred embodiments the methods for producing micron and submicron copper powder utilize precursor compositions containing copper ions in the form of submicron particles of copper carbonate, copper hydroxide, copper oxides, or any combination thereof, and utilize monoethanolamine (or optionally but less preferably hydrazine), and preferably additionally containing caustic and a reducing sugar.
1. A method of making finely divided copper or copper alloy powder, said method comprising adding monoethanolamine to a slurry comprising finely divided particles of a solid copper-containing precursor compound selected from the group consisting of a copper salt, copper carbonate, copper hydroxide, cupric oxide, cuprous oxide, or any combination thereof, said monoethanolamine being present in an amount between 1.5 to 2 grams of monoethanolamine per gram of copper, wherein the temperature is between 90° C. and 150° C., for a time sufficient to convert the precursor compound to a copper powder.
2. The method of making finely divided copper or copper alloy powder of claim 1 , said slurry additionally comprising caustic and a reducing sugar.
3. The method of making finely divided copper or copper alloy powder of claim 2 , said caustic being present in an amount to raise the pH of the slurry to a value between 10.5 and 11.5.
4. The method of making finely divided copper or copper alloy powder of claim 3 , wherein said slurry further comprises water.
5. The method of making finely divided copper or copper alloy powder of claim 2 , said monoethanolamine being present in an amount between 1.6 to 2 grams of monoethanolamine per gram of copper.
6. The method of making finely divided copper or copper alloy powder of claim 4 , wherein said slurry further comprises water.
7. The method of making finely divided copper or copper alloy powder of claim 2 , said monoethanolamine being present in an amount between 1.7 to 1.8 grams of monoethanolamine per gram of copper.
8. The method of making finely divided copper or copper alloy powder of claim 2 , wherein the copper powder has an average particle size of between 0.04 and 0.07 microns.
9. The method of making finely divided copper or copper alloy powder of claim 2 , wherein the copper powder has an average particle size of between 0 0.07 and 0.095 microns.
10. The method of making finely divided copper or copper alloy powder of claim 2 , wherein the copper powder has an average particle size of between 0.1 and 0.2 microns.
11. The method of making finely divided copper or copper alloy powder of claim 2 , wherein said slurry further comprises water.
12. The method of making finely divided copper or copper alloy powder of claim 1 , wherein the solid copper-containing precursor compound is cuprous oxide.
13. The method of making finely divided copper or copper alloy powder of claim 1 , additionally comprising adding caustic and a reducing sugar before reacting the copper-containing precursor compound with the monoethanolamine.
14. The method of making finely divided copper or copper alloy powder of claim 1 , said slurry additionally comprising caustic and a reducing sugar.
15. The method of making finely divided copper or copper alloy powder of claim 1 , wherein said copper-containing precursor compound is cuprous oxide, said method further comprising wet milling the cuprous oxide prior to reacting the cuprous oxide with the monoethanolamine.
16. The method of making finely divided copper or copper alloy powder of claim 1 , wherein said copper-containing precursor compound is cuprous oxide having an average particle size between 0.05 and 0.4 microns, said slurry additionally comprising caustic and a reducing sugar.
17. The method of making finely divided copper or copper alloy powder of claim 1 , wherein said copper-containing precursor compound is cuprous oxide, and wherein the cuprous oxide is converted to copper powder in 10 minutes or less from the time of adding the monoethanolamine.
18. The method of making finely divided copper or copper alloy powder of claim 1 , wherein said slurry further comprises water.