IP Library Granted Patent US 9,914,647
Granted Patent B2
US 9,914,647 · App. 14/520,358 · Granted Mar 13, 2018

Two-dimensional transition metal dichalcogenide sheets and methods of preparation and use

Inventor: Arockiadoss Thevasahayam (Madurai, IN)
Assignee: EMPIRE TECHNOLOGY DEVELOPMENT LLC
C01G39/06C01B19/007C01B21/0768C01G1/12H01G11/24H01G11/28H01G11/30H01G11/68H01G11/86C01P2002/01C01P2002/20C01P2004/04C01P2004/20C01P2004/24C01P2006/40Y02E60/13
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Quick Facts
Patent No.
US 9,914,647
App. No.
14/520,358
Filed
Oct 22, 2014
Granted
Mar 13, 2018
Kind
B2
Examiner
HA, NGUYEN T
Art Unit
2848
USPC
361/502
Abstract

Methods of forming two-dimensional transition metal dichalcogenide sheets are provided. The methods include adding a cross-linking agent to an activating agent to form a solution and mixing a two-dimensional transition metal dichalcogenide with the solution to form a mixture. The methods also include adding a cleaving agent to the mixture to form one or more contiguous sheets of transition metal dichalcogenide.

Claims (21)

1. A method of forming two-dimensional transition metal dichalcogenide sheets, the method comprising:

adding a cross-linking agent to an activating agent to form a solution;

mixing a two-dimensional transition metal dichalcogenide with the solution to form a mixture;

adding a cleaving agent to the mixture;

stirring the mixture comprising the cleaving agent to form one or more contiguous sheets of transition metal dichalcogenide;

removing any particulate matter; and

exfoliating the one or more contiguous sheets of transition metal dichalcogenide by exposing the one or more contiguous sheets of transition metal dichalcogenide to electromagnetic radiation to form a plurality of two-dimensional transition metal dichalcogenide sheets.

2. The method of claim 1 , further comprising:

adding a solvent to the one or more contiguous sheets of transition metal dichalcogenide; and

sonicating to remove unreacted agents.

3. The method of claim 2 , wherein adding the solvent comprises adding ethanol, methanol, isopropyl alcohol, or combinations thereof.

4. The method of claim 2 , further comprising:

filtering the solvent and the one or more contiguous sheets of transition metal dichalcogenide to produce a filtrate; and heating the filtrate to a temperature of about 50° C. for about 10 minutes to separate the one or more contiguous sheets.

5. The method of claim 1 , wherein exposing the one or more contiguous sheets of transition metal dichalcogenide to electromagnetic radiation comprises exposing the one or more contiguous sheets of transition metal dichalcogenide to thermal radiation, solar radiation, microwave radiation, or combinations thereof.

6. The method of claim 1 , wherein exfoliating the one or more contiguous sheets of transition metal dichalcogenide comprises heating the one or more contiguous sheets of transition metal dichalcogenide sheets to a temperature of about 150° C. at a pressure of about 1 atmosphere to about 2 atmosphere.

7. The method of claim 1 , wherein mixing the two-dimensional transition metal dichalcogenide comprises mixing molybdenum disulphide (MoS 2 ), tungsten disulphide (WS 2 ), titanium disulphide (TiS 2 ), tantalum (IV) sulphide (TaS 2 ), zirconium disulphide (ZrS 2 ), bismuth telluride (Bi 2 Te 3 ), bismuth selenide (Bi 2 Se 3 ), titanium nitride chloride (TiNCI), antimony telluride (Sb 2 Te 3 ), melonite (NiTe 2 ), or combinations thereof.

8. The method of claim 1 , wherein forming the two-dimensional transition metal dichalcogenide sheets comprises forming MX 2 , where M is Mo, W, Bi, Sb, Ti, Pt, Nb, Ta, Ni, Zr, Hf, V, Ta, and Pd; and X is S, Se, Te, and NCI.

9. The method of claim 1 , wherein adding the cross-linking agent comprises adding 1-ethyl-3-[3-dimethylaminopropyl]carbodiimide hydrochloride (EDC), cystamine (C 14 H 12 N 2 S 2 .2HCl), N,N′-dicyclohexylcarbodiimide (DCC), 3,3′-dithiobis(sulfosuccinimidylpropionate) (DTSSP), tris(2-carboxyethyl) phosphine hydrochloride (TCEP-HCl), dithiothreitol (DTT), or combinations thereof.

10. The method of claim 1 , wherein adding the activating agent comprises adding ammonia (NH 3 ), tetramethyl ammonium hydroxide (TMAH), or combinations thereof, at a pH of 6.8 to 7.1.

11. The method of claim 1 , wherein adding the cleaving agent comprises adding N-hydroxysuccinimide (NHS), N-hydroxysulfosuccinimide (Sulfo-NHS), or combinations thereof.

12. The method of claim 1 , wherein the stirring is carried out at a temperature of about 125° C. to about 200° C.

Assignments (4)
RELEASE OF SECURITY INTEREST IN PATENTS, RECORDED ON JANUARY 29, 2019, AT REEL/FRAME 048373/0217 Recorded Jun 22, 2026
From: CRESTLINE DIRECT FINANCE, L.P., AS COLLATERAL AGENT
To: EMPIRE TECHNOLOGY DEVELOPMENT LLC
Reel/Frame 075799/0053 →
RELEASE OF SECURITY INTEREST IN PATENTS, RECORDED ON JANUARY 29, 2019 AT REEL 048373 FRAME 0217 Recorded Sep 22, 2025
From: CRESTLINE DIRECT FINANCE, L.P., AS COLLATERAL AGENT
To: EMPIRE TECHNOLOGY DEVELOPMENT LLC
Reel/Frame 072936/0464 →
SECURITY INTEREST Recorded Jan 29, 2019
From: EMPIRE TECHNOLOGY DEVELOPMENT LLC
To: CRESTLINE DIRECT FINANCE, L.P.
Reel/Frame 048373/0217 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 23, 2014
From: THEVASAHAYAM, AROCKIADOSS
To: EMPIRE TECHNOLOGY DEVELOPMENT LLC
Reel/Frame 034011/0783 →
Priority Claims (1)
IN 4799/CHE/2013 · Oct 24, 2013 · national
Continuity (1)
Related Publication 20150116906A1 · Apr 30, 2015