Method of producing thin layer of large area transition metal dichalcogenides MoS2 and others

Patent metadata

Field	Value
Publication number	US-11142824-B2
Application number	US-201916391876-A
Country	US
Kind code	B2
Filing date	Apr 23, 2019
Priority date	Apr 23, 2019
Publication date	Oct 12, 2021
Grant date	Oct 12, 2021

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.

First claim

What is claimed:

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.

Assignees

• Uchicago Argonne Llc

Inventors

• Mane Anil U
• Choudhury Devika
• Elam Jeffrey W
• Letourneau Steven Payonk

Classifications

• C23C16/45527

  characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations · CPC title

• C23C16/56 Primary

  After-treatment · CPC title

• C23C16/0272

  Deposition of sub-layers, e.g. to promote the adhesion of the main coating · CPC title

• C23C16/14

  Deposition of only one other metal element · CPC title

• C23C16/45553

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