Growth methods for controlled large-area fabrication of high-quality graphene analogs

Patent metadata

Field	Value
Publication number	US-9580834-B2
Application number	US-201414203958-A
Country	US
Kind code	B2
Filing date	Mar 11, 2014
Priority date	Mar 11, 2013
Publication date	Feb 28, 2017
Grant date	Feb 28, 2017

Abstract

In some embodiments, the present disclosure pertains to methods of growing chalcogen-linked metallic films on a surface in a chamber. In some embodiments, the method comprises placing a metal source and a chalcogen source in the chamber, and gradually heating the chamber, where the heating leads to the chemical vapor deposition of the chalcogen source and the metal source onto the surface, and facilitates the growth of the chalcogen-linked metallic film from the chalcogen source and the metal source on the surface. In some embodiments, the chalcogen source comprises sulfur, and the metal source comprises molybdenum trioxide. In some embodiments, the growth of the chalcogen-linked metallic film occurs by formation of nucleation sites on the surface, where the nucleation sites merge to form the chalcogen-linked metallic film. In some embodiments, the formed chalcogen-linked metallic film includes MoS 2 .

First claim

What is claimed is:

1. A method of growing a chalcogen-linked metallic film on a surface in a chamber, said method comprising:
(a) patterning the surface to form a pattern on the surface, wherein the pattern comprises edges;
(b) placing a metal source, a chalcogen source, and the surface in the chamber; and
(c) heating the chamber,
wherein the heating leads to the deposition of the chalcogen source and the metal source onto the surface,
wherein the heating facilitates growth of the chalcogen-linked metallic film from the chalcogen source and the metal source on the surface, and
wherein the growth of the chalcogen-linked metallic film follows the edges of the pattern.

2. The method of claim 1 , wherein the surface is a silicon wafer.

3. The method of claim 1 , wherein the surface is coated with silicon-oxide.

4. The method of claim 1 , wherein the patterning of the surface occurs by photolithography.

5. The method of claim 1 , wherein the chalcogen source is selected from the group consisting of oxygen, sulfur, selenium, tellurium, and combinations thereof.

6. The method of claim 1 , wherein the chalcogen source comprises sulfur.

7. The method of claim 1 , wherein the chalcogen source comprises sulfur and selenium.

8. The method of claim 1 , wherein the metal source is selected from the group consisting of metals, metal oxides, transition metals, transition metal oxides, and combinations thereof.

9. The method of claim 1 , wherein the metal source is selected from the group consisting of molybdenum, tungsten, titanium, and combinations thereof.

10. The method of claim 1 , wherein the metal source is molybdenum trioxide.

11. The method of claim 1 , wherein the chalcogen source and the metal source are deposited onto the surface by chemical vapor deposition.

12. The method of claim 1 , wherein the heating of the chamber occurs by heating the chamber to about 850° C.

13. The method of claim 1 , wherein the heating of the chamber occurs by heating the chamber at a rate of between about 1° C. per minute to about 50° C. per minute.

14. The method of claim 1 , wherein the heating of the chamber occurs by:
heating the chamber from room temperature to about 550° C. at a rate of about 20° C./min; and
heating the chamber from about 550° C. to about 850° C. at a rate of about 5° C./min.

15. The method of claim 1 , wherein the growth of the chalcogen-linked metallic film occurs by formation of nucleation sites on the edges of the pattern, wherein the nucleation sites merge to form the chalcogen-linked metallic film.

16. The method of claim 1 , further comprising a step of cooling the chamber after heating the chamber.

17. The method of claim 16 , wherein the chamber is cooled to room temperature over a period of one hour.

18. The method of claim 1 , wherein the chamber is a furnace.

19. The method of claim 1 , wherein the chamber is under a flow of an inert gas.

20. The method of claim 19 , wherein the inert gas is selected from the group consisting of argon, nitrogen, helium, and combinations thereof.

21. The method of claim 20 , wherein the inert gas comprises nitrogen.

22. The method of claim 1 , further comprising a step of controlling a morphology of the chalcogen-linked metallic film, wherein the controlling comprises adjusting a growth parameter.

23. The method of claim 22 , wherein the morphology comprises at least one of shape, size, or thickness.

24. The method of claim 22 , wherein the growth parameter is selected from the group consisting of chalcogen source concentration, chamber pressure, metal source concentration, chamber temperature, type of surface, and combinations thereof.

25. The method of claim 1 , wherein the chalcogen-linked metallic film comprises a single layer.

26. The method of claim 1 , wherein the chalcogen-linked metallic film comprises multiple layers.

27. The method of claim 1 , wherein the chalcogen-linked metallic film is a single-crystalline film.

28. The method of claim 1 , wherein the chalcogen-linked metallic film is a sulfated metallic film.

29. The method of claim 1 , wherein the chalcogen-linked metallic film is selected from the group consisting of MoS 2 , MoSe 2 , MoS 1 Se 1 , WS 2 , WSe 2 , TiS 2 , and combinations thereof.

30. The method of claim 1 , wherein the chalcogen-linked metallic film comprises MoS 2(1-x) Se 2x .

31. The method of claim 30 , wherein x is at least one of 0.1, 0.3, 0.50 and 0.75.

32. The method of claim 1 , wherein the chalcogen-linked metallic film is a transition metal dichalcogenide.

33. The method of claim 1 , further comprising a step of transferring the chalcogen-linked metallic film to a new surface.

Assignees

• Najmaei Sina
• Liu Zheng
• Ajayan Pulickel M
• Lou Jun
• Univ Rice William M

Inventors

• Najmaei Sina
• Liu Zheng
• Ajayan Pulickel M
• Lou Jun

Classifications

• C30B25/00

  Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth · CPC title

• C30B25/10

  Heating of the reaction chamber or the substrate · CPC title

• C30B25/04 Primary

  Pattern deposit, e.g. by using masks · CPC title

• C23C16/305

  Sulfides, selenides, or tellurides · CPC title

• C30B29/46

  Sulfur-, selenium- or tellurium-containing compounds · CPC title