Method for manufacturing an interfacial lithium fluoride layer for an electrochemical cell

Patent metadata

Field	Value
Publication number	US-12040505-B2
Application number	US-202217880521-A
Country	US
Kind code	B2
Filing date	Aug 3, 2022
Priority date	Aug 3, 2022
Publication date	Jul 16, 2024
Grant date	Jul 16, 2024

Abstract

A method for manufacturing an interfacial lithium fluoride layer for an electrochemical cell that cycles lithium ions is disclosed. In the method, a substrate is positioned in a reaction chamber of an atomic layer deposition reactor and a lithium fluoride (LiF) precursor is introduced into the reaction chamber such that the LiF precursor contacts and chemically reacts with functional groups on the substrate. Then, an oxidant is introduced into the reaction chamber to form a single molecular layer of lithium fluoride on the substrate. The lithium fluoride layer is formed on the substrate at a temperature of greater than or equal to about 110 degrees Celsius to less than or equal to about 250 degrees Celsius.

First claim

What is claimed is:

1. A method for manufacturing an interfacial lithium fluoride layer for an electrochemical cell that cycles lithium ions, the method comprising:
(a) positioning a substrate in a reaction chamber of an atomic layer deposition reactor, the substrate having functional groups on a major surface thereof;
(b) introducing a lithium fluoride (LiF) precursor into the reaction chamber such that the LiF precursor contacts and chemically reacts with the functional groups on the major surface of the substrate, the LiF precursor comprising a lithium- and fluorine-containing acetylacetonate compound; and
(c) after step (b), introducing an oxidant into the reaction chamber to form a single molecular layer of lithium fluoride on the major surface of the substrate,
wherein steps (b) and (c) are performed at a temperature of greater than or equal to about 110 degrees Celsius to less than or equal to about 250 degrees Celsius.

2. The method of claim 1 , wherein step (c) further comprises:
introducing plasma into the reaction chamber.

3. The method of claim 1 , wherein steps (b) and (c) are performed at a temperature of less than or equal to about 200 degrees Celsius.

4. The method of claim 1 , wherein the LiF precursor has a sublimation temperature of greater than or equal to about 80 degrees Celsius to less than or equal to about 90 degrees Celsius.

5. The method of claim 1 , wherein the LiF precursor comprises lithium hexafluoroacetylacetonate.

6. The method of claim 1 , wherein the oxidant comprises water, oxygen, ozone, oxygen plasma, ozone plasma, trimethyl phosphate, or a combination thereof.

7. The method of claim 1 , wherein the LiF precursor and the oxidant are the only reactants used to form the layer of lithium fluoride.

8. The method of claim 1 , wherein the substrate comprises silicon, carbon nanotubes, lithium metal, an electrically insulating polymer, or an electroactive positive electrode material.

9. The method of claim 8 , wherein the functional groups on the major surface of the substrate comprise hydroxyl groups.

10. The method of claim 1 , further comprising:
purging unreacted LiF precursor compounds and reaction byproducts from the reaction chamber prior to step (c).

11. The method of claim 10 , further comprising:
purging unreacted oxidant and reaction byproducts from the reaction chamber after step (c).

12. The method of claim 1 , wherein at least one of the LiF precursor or the oxidant are introduced into the reaction chamber along with an inert carrier gas.

13. The method of claim 1 , wherein a reductant is not introduced into the reaction chamber before, during, or after steps (b) and (c).

14. A method for manufacturing an interfacial lithium fluoride layer for an electrochemical cell that cycles lithium ions, the method comprising:
(a) positioning a substrate in a reaction chamber of an atomic layer deposition reactor, the substrate having functional groups on a major surface thereof;
(b) introducing a lithium fluoride (LiF) precursor into the reaction chamber such that the LiF precursor contacts and chemically reacts with the functional groups on the major surface of the substrate, the LiF precursor comprising lithium hexafluoroacetylacetonate; and
(c) after step (b), introducing an oxidant into the reaction chamber to form a single molecular layer of lithium fluoride on the major surface of the substrate, the oxidant comprising water, oxygen, ozone, oxygen plasma, ozone plasma, trimethyl phosphate, or a combination thereof,
wherein steps (b) and (c) are performed at a temperature of greater than or equal to about 110 degrees Celsius to less than or equal to about 250 degrees Celsius.

15. The method of claim 14 , wherein step (c) further comprises:
introducing plasma into the reaction chamber.

16. The method of claim 14 , wherein steps (b) and (c) are performed at a temperature of less than or equal to about 200 degrees Celsius.

17. The method of claim 14 , wherein the LiF precursor and the oxidant are the only reactants used to form the layer of lithium fluoride.

18. The method of claim 14 , wherein the substrate comprises lithium metal, an electrically insulating polymer, or an electroactive positive electrode material.

Assignees

• Gm Global Tech Operations Llc

Inventors

• Wang Biqiong
• He Meinan
• Cai Mei
• Galant Andrew J
• Osad William

Classifications

• H01M4/382

  Lithium (H01M4/405 takes precedence) · CPC title

• H01M4/139

  Processes of manufacture · CPC title

• H01M50/449 Primary

  having a layered structure · CPC title

• C23C16/45553

  characterized by the use of precursors specially adapted for ALD · CPC title

• C23C16/30

  Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides · CPC title