IP Library Granted Patent US 12,270,101
Granted Patent B2
US 12,270,101 · App. 17/207,445 · Granted Apr 8, 2025

Formation of lithium-metal-oxygen layer and removal of lithium carbonate on solid state electrolytes

Inventors: Donghyeon Kang (Willowbrook, IL); Jeffrey W. Elam (Elmhurst, IL); Joseph A. Libera (Clarendon Hills, IL); Yujia Liang (Lisle, IL); HackSung Kim (Naperville, IL); Anil U. Mane (Naperville, IL)
Assignees: UCHICAGO ARGONNE, LLC; NORTHWESTERN UNIVERSITY
C23C16/18C23C16/455H01M10/0562H01M2300/0068
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Quick Facts
Patent No.
US 12,270,101
App. No.
17/207,445
Granted
Apr 8, 2025
Kind
B2
Abstract

A process for forming a lithium-metal-oxygen film on a lithium SSE. A metal-ligand complex is exposed to the SSE such as for 30-600 seconds in a chemical vapor transfer reactor at a temperature of 200-350° C.

Claims (24)

1. A method, comprising:

placing a lithium metal structure in a reactor;

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 a ligand selected from the group consisting of an alkyl, through the reactor at a temperature of 250-350° C. for a continuous flow time of 30-600 seconds; and

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

2. The method of claim 1 , wherein the temperature is 280-320° 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 precursor vapor with lithium metal is under a high vacuum condition of 10 −6 -10 −10 Torr.

5. The method of claim 1 , wherein the metal is aluminum.

6. The method of claim 5 , wherein the lithium-metal-oxygen film is a lithium-aluminum-oxygen film.

7. A method, comprising:

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

flowing a metal-ligand complex precursor vapor in a carrier gas, the precursor comprising a metal selected from Al, In, Ga, and Zn and an alkyl ligand, through the reactor at a temperature of 250-350° C. for a continuous flow time of 30-600 seconds; and

reacting the metal-ligand complex with the lithium carbonate of the lithium SSE, removing a portion of the lithium carbonate from the lithium SSE.

8. The method of claim 7 , further comprising forming a lithium-metal-oxygen film on the lithium SSE.

9. The method of claim 8 , wherein all of the lithium carbonate is removed from the lithium SSE.

10. The method of claim 8 , wherein the temperature is 280-320° C.

11. The method of claim 8 , wherein the lithium-metal-oxygen film comprises a lithium-aluminum-oxygen film.

12. The method of claim 11 , wherein the metal-ligand complex is trimethylaluminum.

13. The method of claim 7 , wherein the carrier gas has a flow velocity of 0.1-20 m/s.

14. The method of claim 7 , wherein reacting the metal-ligand complex with lithium metal is under a high vacuum condition of 10 −6 -10 −10 Torr.

15. The method of claim 14 , wherein the metal is aluminum.

16. The method of claim 7 , wherein the metal-ligand complex is a methyl, ethyl, or propyl ligand.

17. The method of claim 7 , wherein the metal-ligand vapor has a partial pressure of 0.001-10 Torr.

18. The method of claim 7 , wherein the continuous flow time is 60 seconds to 600 seconds.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 8, 2024
From: KIM, HACKSUNG
To: NORTHWESTERN UNIVERSITY
Reel/Frame 066055/0397 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 20, 2023
From: KANG, DONGHYEON; ELAM, JEFFREY W.; LIANG, YUJIA; LIBERA, JOSEPH A.; MANE, ANIL U.
To: UCHICAGO ARGONNE, LLC
Reel/Frame 063995/0407 →
CONFIRMATORY LICENSE Recorded May 7, 2021
From: UCHICAGO ARGONNE LLC
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 056169/0481 →
Continuity (1)
Related Publication 20220298626A1 · Sep 22, 2022
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