IP Library Granted Patent US 11,142,824
Granted Patent B2
US 11,142,824 · App. 16/391,876 · Granted Oct 12, 2021

Method of producing thin layer of large area transition metal dichalcogenides MoS

Inventors: Anil U. Mane (Naperville, IL); Devika Choudhury (Naperville, IL); Jeffrey W. Elam (Elmhurst, IL); Steven Payonk Letourneau (Naperville, IL)
Assignee: UChicago Argonne, LLC
C23C16/56C23C16/14C23C16/45527C23C16/45553
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Quick Facts
Patent No.
US 11,142,824
App. No.
16/391,876
Granted
Oct 12, 2021
Kind
B2
Abstract

An ultra-thin film transition metal dichalcogenide (“TMD”) supported on a support. The TMD is formed from a metal grown by atomic layer deposition (“ALD”) on a substrate. The metal is sulphurized to produce a TMD ultra-thin layer.

Claims (27)

1. A method of preparing a substrate comprising:

depositing a seed layer on the substrate, the seed layer comprising AlMoF;

forming an ultra-thin transition metal layer by:

performing a atomic layer deposition cycles of transition metal precursor at a first deposition temperature between 100° C. and 300° C., and

performing b atomic layer deposition cycles of a second precursor at a second deposition temperature between 50° C. and 300° C., and

forming a transition metal dichalcogenide by sulphurization of the ultra-thin transition metal layer by exposure to a sulfur precursor.

2. The method of claim 1 , wherein sulphurization further comprises thermally annealing the ultra-thin transition metal layer at a sulphurization temperature.

3. The method of claim 1 , wherein the transition metal precursor for a atomic layer deposition is MoF 6 and, the precursor for b atomic layer deposition is Si 2 H 6 and the sulfur precursor is H 2 S further wherein the transition metal dichalcogenide is MoS 2 .

4. The method of claim 1 , wherein the a cycles each comprise: a 1 second dose followed by a gas purge.

5. The method of claim 2 , wherein the b cycle depositions each comprise: a 1 second dose followed by a 1 second gas purge.

6. The method of claim 2 , wherein the sulphurization temperature is greater than 300° C. and less than 600° C.

7. The method of claim 5 , wherein sulphurization further comprises exposing the transition metal layer to H 2 S.

8. The method of claim 5 , wherein the ultra-thin transition metal layer is deposited on a substrate before sulphurization.

9. The method of claim 1 , wherein the seed layer comprises a material different from the ultra-thin transition metal layer and the substrate and wherein the seed layer is lnm thick.

10. A method of preparing a substrate comprising:

depositing a seed layer on the substrate, the seed layer comprising AlMoF;

forming a transition metal layer of x atomic layers by repeating x times a atomic layer deposition process having the steps of:

performing a atomic layer deposition cycles of transition metal precursor at a first deposition temperature between 100° C. and 300° C., and

performing b atomic layer deposition cycles of a second precursor at a second deposition temperature between 50° C. and 300° C., and

converting the transition metal layer to dichalcogenide by sulphurization of the transition metal layer at a temperature of at least greater than or equal to 300° C. by exposure to at least one dose of a sulfur precursor,

wherein x is between 1 and 8.

11. The method of claim 10 , wherein the transition metal precursor is MoF 6 and Si 2 H 6 further, the transition metal dichalcogenide is MoS 2 , and the sulfur precursor is H 2 S.

12. The method of claim 10 , wherein the a cycles each comprise: a 1 second dose followed by a gas purge.

13. The method of claim 10 , wherein the b cycle depositions each comprise: a 1 second dose followed by a second gas purge.

14. The method of claim 10 , wherein the sulfur precursor comprises H 2 S.

15. The method of claim 10 , wherein the sulphurization temperature is between 300° C. and 600° C.

16. The method of claim 15 wherein the sulphurization is by 10 second doses of H 2 S exposure at a pressure of at least 1.5 Torr.

Assignments (2)
CONFIRMATORY LICENSE Recorded May 19, 2021
From: UCHICAGO ARGONNE, LLC
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 056290/0061 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 30, 2019
From: ELAM, JEFFREY W.; LETOURNEAU, STEVEN; MANE, ANIL U.; CHOUDHURY, DEVIKA
To: UCHICAGO ARGONNE, LLC
Reel/Frame 049318/0061 →
Continuity (1)
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