IP Library Granted Patent US 11,414,749
Granted Patent B1
US 11,414,749 · App. 17/207,375 · Granted Aug 16, 2022

Formation of lithium-metal-carbon protecting layer and removal of lithium carbonate on lithium metal

Inventors: Donghyeon Kang (Willowbrook, IL); Jeffrey W. Elam (Elmhurst, IL); Anil U. Mane (Naperville, IL)
Assignee: UChicago Argonne, LLC
C23C16/18C23C16/455
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Quick Facts
Patent No.
US 11,414,749
App. No.
17/207,375
Granted
Aug 16, 2022
Kind
B1
Abstract

A process for forming a lithium-metal-carbon film on a lithium metal structure. A metal-ligand complex is exposed to the metal ligand, such as for 5-30 seconds in a chemical vapor transfer reactor at a temperature of 100-180° C.

Claims (25)

1. A method, comprising:

placing a lithium metal structure in a reactor, the lithium metal structure having an exposed coating of lithium carbonate;

flowing a metal-ligand precursor vapor in a carrier gas, the metal-ligand precursor vapor comprising a metal selected from Al, In, Ga, and Zn and an alkyl ligand through the reactor at a temperature of 100-180° C. for a flow time of 5-30 seconds; and

reacting the metal-ligand precursor vapor with the exposed coating of lithium carbonate of the lithium metal structure, removing the lithium carbonate from the lithium metal structure;

reacting the metal-ligand precursor vapor with lithium metal of the lithium metal structure, forming a lithium-metal-carbon film on the lithium metal structure.

2. The method of claim 1 , wherein the temperature is 130-160° C.

3. The method of claim 2 , wherein the carrier gas has a flow velocity of 0.1-20 m/s.

4. The method of claim 2 , wherein reacting the metal-ligand complex with lithium metal is under a high vacuum condition of 10 −6 -10 −10 Torr.

5. The method of claim 1 , wherein the metal of the metal-ligand precursor vapor is aluminum.

6. The method of claim 4 , wherein the lithium-metal-carbon film is a lithium-aluminum-carbon film.

7. The method of claim 1 , wherein the lithium-metal-carbon film is a composite comprising up to 90% Li—Al—C and up to 10% oxygen.

8. A method, comprising:

placing a lithium metal structure in a reactor, the lithium metal structure having an exposed coating of lithium carbonate;

flowing a metal-ligand complex precursor vapor in a carrier gas, the metal-ligand complex precursor vapor comprising a metal selected from Al, In, Ga, and Zn and an alkyl ligand, through the reactor at a temperature of 100-150° C. for a flow time of 5-30 seconds; and

reacting the metal-ligand complex precursor vapor with the exposed coating of lithium carbonate of the lithium metal structure, removing a portion of the lithium carbonate from the lithium metal structure.

9. The method of claim 8 , further comprising forming a lithium-metal-carbon film on the lithium metal structure.

10. The method of claim 9 , wherein the metal of the metal-ligand complex precursor vapor is aluminum.

11. The method of claim 10 , wherein the lithium-metal-carbon film is a lithium-aluminum-carbon film.

12. The method of claim 11 , wherein the lithium-metal-carbon film is a composite comprising up to 90% Li—Al—C and up to 10% oxygen.

13. The method of claim 12 , wherein the metal-ligand complex precursor vapor is trimethylaluminum.

14. The method of claim 8 , wherein the temperature is 130-160° C.

15. The method of claim 14 wherein the carrier gas has a flow velocity of 0.1-20 m/s.

16. The method of claim 14 , wherein reacting the metal-ligand complex with lithium metal is under a high vacuum condition of 10 −6 -10 −10 Torr.

17. The method of claim 8 , wherein alkyl ligand of the metal-ligand complex precursor vapor is a methyl, ethyl, or propyl ligand.

18. The method of claim 8 , wherein the metal-ligand vapor has a partial pressure of 0.001-10 Torr.

Assignments (2)
CONFIRMATORY LICENSE Recorded May 27, 2022
From: UCHICAGO ARGONNE, LLC
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 060037/0452 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 12, 2022
From: ELAM, JEFFREY W.; KANG, DONGHYEON; MANE, ANIL U.
To: UCHICAGO ARGONNE, LLC
Reel/Frame 059574/0679 →
Cited By (1)
US 12,334,562