IP Library Granted Patent US 11,296,313
Granted Patent B2
US 11,296,313 · App. 15/960,178 · Granted Apr 5, 2022

Carbon dioxide treatment of cathodes

Inventors: Ozgenur Kahvecioglu (Naperville, IL); Gregory K. Krumdick (Homer Glen, IL)
Assignee: UCHICAGO ARGONNE, LLC
H01M4/366C01D15/08C01G53/50H01M4/505H01M4/525H01M4/5825H01M10/0525C01P2004/80C01P2006/40H01M2004/028
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Quick Facts
Patent No.
US 11,296,313
App. No.
15/960,178
Granted
Apr 5, 2022
Kind
B2
Abstract

A method for producing water resistant cathodes is discussed. The method uses mixing cathode powder with solid carbon dioxide to create a mixture and heating the mixture to a temperature. The heating occurs for a time sufficient to cause lithium carbonate coatings to form on the powder. A method for coating lithium-containing cathode surfaces is also discussed. This method uses simultaneously sublimating solid CO 2 and condensing atmospheric water vapor onto surfaces. Afterwards allowing the lithium to react with the sublimated CO 2 for a time sufficient to create a lithium carbonate film on the surface.

Claims (28)

1. A method for producing water resistant cathodes, the method comprising:

a) contacting solid phase cathode powder containing lithium with solid phase carbon dioxide to create a mixture wherein a weight ratio of the powder to the carbon dioxide is between 1:10 and 1:20; and

b) heating the mixture to a temperature between 250 and 700° C. and for between 1 and 8 hours to cause a conformal coating of lithium carbonate to form on the powder.

2. The method as recited in claim 1 wherein the method is conducted in atmospheric conditions.

3. The method as recited in claim 1 wherein the mixture is heated to between 300 and 500° C.

4. The method as recited in claim 1 wherein the powder is an NMC type cathode material selected from the group consisting of nickel, cobalt, manganese, lithium, oxygen, and combinations thereof.

5. A method for producing water resistant cathodes, the method comprising:

a) mixing cathode powder containing lithium with solid carbon dioxide to create a mixture; and

b) heating the mixture to a temperature between 250 and 700° C. and for a time between 1 and 8 hours to cause lithium carbonate to form on the powder, wherein mixing occurs in an atmosphere having between 1 percent and 30 percent humidity.

6. The method as recited in claim 5 wherein the mixing establishes an equilibrium between solid dry ice and gaseous water to form carbonic acid.

7. The method as recited in claim 6 wherein the carbonic acid reacts with lithium contained in the powder.

8. The method as recited in claim 7 wherein the reaction occurs at between −30° C. and 0° C.

9. A method for producing water resistant cathodes, the method comprising:

a) mixing cathode powder containing lithium with solid carbon dioxide to create a mixture; and

b) heating the mixture to a temperature between 250 and 700° C. and for a time between 1 and 8 hours to cause lithium carbonate to form on the powder wherein the mixture is buried under additional solid carbon dioxide before heating.

10. A method for coating lithium-containing solid cathode surfaces, the method comprising:

a) simultaneously sublimating solid CO 2 and condensing atmospheric water vapor onto the surfaces; and

b) allowing the lithium to react with the sublimated CO 2 for a time between 1 to 8 hours to create a lithium carbonate film on the surface.

11. The method as recited in claim 10 wherein a pH of the surface is less than 11.

12. The method as recited in claim 10 wherein the simultaneous step comprises mixing solid dry ice with cathode powder.

13. The method as recited in claim 10 wherein a weight ratio of dry ice to cathode powder ranges from 10:1 to 20:1.

14. A method for coating lithium-containing cathode surfaces, the method comprising:

a) simultaneously sublimating solid CO 2 and condensing atmospheric water vapor onto the surfaces; and

b) allowing the lithium to react with the sublimated CO 2 for a time between 1 to 8 hours to create a lithium carbonate film on the surface, and further comprising removing excess water from the surface.

15. The method as recited in claim 10 further comprising heating the film.

16. The method as recited in claim 11 wherein the simultaneous step results in the production of carbonic acid.

17. The method as recited in claim 16 wherein the carbonic acid reacts with the lithium.

18. The method as recited in claim 10 wherein the condensed water dissolves the lithium prior to the creation of the film.

Assignments (2)
CONFIRMATORY LICENSE Recorded Jun 21, 2022
From: UCHICAGO ARGONNE, LLC
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 060450/0845 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 24, 2019
From: FERIDUN, OZGENUR KAHVECIOGLU; KRUMDICK, GREGORY K.
To: UCHICAGO ARGONNE, LLC
Reel/Frame 050471/0305 →
Continuity (1)
Related Publication 20190326591A1 · Oct 24, 2019