Method for manufacturing two-dimensional transition metal dichalcogemide thin film

Patent metadata

Field	Value
Publication number	US-10309011-B2
Application number	US-201615562545-A
Country	US
Kind code	B2
Filing date	Jul 28, 2016
Priority date	Jul 29, 2015
Publication date	Jun 4, 2019
Grant date	Jun 4, 2019

Abstract

The present invention relates to a method for preparing a two-dimensional transition metal dichalcogenide and, more particularly, to a method for preparing a highly uniform two-dimensional transition metal dichalcogenide thin film. More specifically, the present invention is directed to a preparation method for a highly uniform two-dimensional transition metal dichalcogenide thin film at low temperature of 500° C. or below.

First claim

What is claimed is:

1. A method for preparing a two-dimensional transition metal dichalcogenide, comprising:
pre-treating a substrate in a deposition chamber; and
introducing a chalcogen-containing precursor and a transition-metal-containing precursor into the deposition chamber to deposit a two-dimensional transition metal dichalcogenide on the substrate,
wherein the deposition step includes further adding an inhibitor for preventing the creation of a two-dimensional transition metal dichalcogenide bilayer.

2. The method as claimed in claim 1 , wherein the transition-metal-containing precursor comprises a transition metal selected from the group consisting of Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Nb, Ta, Mo, W, Tc, Re, Ru, Os, Rh, Ir, Pt, Ag, Au, Cd, In, Tl, Sn, Pb, Sb, Bi, Zr, Te, Pd, Hf, and a combination thereof.

3. The method as claimed in claim 1 , wherein a partial pressure ratio of the chalcogen-containing precursor to the transition-metal-containing precursor is 1:2 or greater.

4. The method as claimed in claim 1 , wherein the chalcogen-containing precursor comprises an S-containing organic compound or an S-containing inorganic compound.

5. The method as claimed in claim 1 , wherein the deposition is performed at a low temperature of 600° C. or below.

6. The method as claimed in claim 1 , wherein the deposition is performed according to a chemical vapor deposition method.

7. The method as claimed in claim 6 , wherein the chemical vapor deposition method comprises low pressure chemical vapor deposition, atmospheric pressure chemical vapor deposition, metal organic chemical vapor deposition, plasma-enhanced chemical vapor deposition, inductively coupled plasma chemical vapor deposition, atomic-layer chemical vapor deposition, or plasma-enhanced atomic layer deposition.

8. The method as claimed in claim 1 , wherein the pretreatment of the substrate is performed to control a nucleation site of the transition metal dichalcogenide to be deposited on the substrate.

9. The method as claimed in claim 1 , wherein a partial pressure ratio of the chalcogen-containing precursor to the transition-metal-containing precursor is adjusted to control a surface energy and the size of a cluster formed by gas phase reaction during the deposition process of the transition metal dichalcogenide, thereby inducing a two-dimensional growth of the transition metal dichalcogenide.

10. The method as claimed in claim 1 , wherein in the deposition process, the internal pressure of the deposition chamber is adjusted to control the amounts of the chalcogen-containing precursor and the transition-metal-containing precursor to be introduced into the deposition chamber, thereby controlling a partial pressure ratio of the chalcogen-containing precursor to the transition-metal-containing precursor.

11. A method for preparing a two-dimensional transition metal dichalcogenide thin film, comprising:
performing a surface treatment on a substrate in a deposition chamber to reduce the surface energy of the substrate; and
introducing a chalcogen-containing precursor, a transition-metal-containing precursor, and a precursor-decomposition-accelerating catalyst into the deposition chamber to deposit a two-dimensional transition metal dichalcogenide monolayer on the substrate,
wherein the deposition step includes further adding an inhibitor for preventing the creation of a two-dimensional transition metal dichalcogenide bilayer.

12. The method as claimed in claim 11 , wherein the inhibitor has an adsorption energy higher on the edge planes of the substrate and the transition metal dichalcogenide monolayer rather than on the basal plane of the two-dimensional transition metal dichalcogenide monolayer,
wherein the chalcogen has an adsorption energy higher on the basal planes of the substrate and the transition metal dichalcogenide monolayer than on the edge plane of the transition metal dichalcogenide monolayer.

13. The method as claimed in claim 11 , wherein the precursor-decomposition-accelerating catalyst speeds up the decomposition of the chalcogen-containing precursor to take the ligand off from the chalcogen atom in the chalcogen-containing precursor, and/or the decomposition of the transition-metal-containing precursor containing a ligand bonded to a transition metal atom to take the ligand off from the transition metal atom in the transition-metal-containing precursor.

14. The method as claimed in claim 11 , wherein the surface treatment of the substrate is performed by a wet surface treatment method selected from the group consisting of piranha solution treatment, sulfuric acid (H 2 SO 4 ) solution treatment, hydrochloric acid (HCl) solution treatment, and alkali metal hydroxide solution treatment; or a dry surface treatment method selected from the group consisting of O 2 plasma thermal treatment and water vapor thermal treatment.

15. The method as claimed in claim 11 , wherein the substrate is selected from the group consisting of SiO 2 , Al 2 O 3 , HfO 2 , LiAlO 3 , MgO, Si, Ge, GaN, AlN, GaP, InP, GaAs, SiC, glass, quartz, sapphire, graphite, graphene, plastic, polymer, boron nitride (h-BN), and a combination thereof.

16. The method as claimed in claim 11 , wherein the substrate is selected from the group consisting of SiO 2 , Al 2 O 3 , HfO 2 , LiAlO 3 , MgO, and a combination thereof,
wherein the surface treatment of the substrate is performed by a wet surface treatment method selected from the group consisting of piranha solution treatment, sulfuric acid (H 2 SO 4 ) solution treatment, hydrochloric acid (HCl) solution treatment, and alkali metal hydroxide solution treatment; or a dry surface treatment method selected from the group consisting of O 2 plasma thermal treatment and water vapor thermal treatment.

17. The method as claimed in claim 11 , wherein a partial pressure ratio of the chalcogen-containing precursor to the transition-metal-containing precursor is at least 2.

18. A method for preparing a two-dimensional transition metal dichalcogenide thin film, comprising:
(1) performing a surface treatment on a substrate in a deposition chamber to reduce the surface energy of the substrate;
(2) introducing a chalcogen-containing precursor and a transition-metal-containing precursor into the deposition chamber at a temperature of 500° C. or below and a first pressure of 0.001 to 760 Torr to create crystals of the two-dimensional transition metal dichalcogenide on the substrate;
(3) introducing the chalcogen-containing precursor and the transition-metal-containing precursor into the deposition chamber at a second pressure higher than the first pressure of the step (2) to increase the crystal size of the two-dimensional transition metal dichalcogenide on the substrate; and
(4) introducing the chalcogen-containing precursor and the transition-metal-containing precursor into the deposition chamber at a third pressure higher than the second pressure of the step (3) to form a two-dimensional transition metal dichalcogenide monolayer on the substrate,
wherein an inhibitor for preventing the creation of a two-dimensional transition metal dichalcogenide bilayer is further added into the deposition chamber in the steps (2), (3) and (4).

19. The method as claimed in claim 18 , wherein a precursor-decomposition-accelerating catalyst is further added into the deposition chamber in the steps (2), (3) and (4).

Assignees

• Korea Res Inst Standards & Sci

Inventors

• Kang Sang Woo
• Mun Ji Hun

Classifications

• C30B29/64

  Flat crystals, e.g. plates, strips or discs · CPC title

• C30B29/46

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

• C30B25/186

  being specially pre-treated by, e.g. chemical or physical means · CPC title

• C30B25/16

  Controlling or regulating (controlling or regulating in general G05) · CPC title

• C23C16/0227

  by cleaning or etching · CPC title