IP Library Granted Patent US 9,725,332
Granted Patent B2
US 9,725,332 · App. 14/522,577 · Granted Aug 8, 2017

Transition metal dichalcogenide aerogels and methods of preparation and use

Inventor: Arockiadoss Thevasahayam (Madurai, IN)
Assignee: EMPIRE TECHNOLOGY DEVELOPMENT LLC
C01G39/06C01B19/007C01B21/0768C01G1/12H01G11/00H01G11/30H01G11/86C01P2002/20C01P2004/20C01P2004/24C01P2006/10C01P2006/12C01P2006/40Y02E60/13
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Quick Facts
Patent No.
US 9,725,332
App. No.
14/522,577
Granted
Aug 8, 2017
Kind
B2
Abstract

Methods of forming transition metal dichalcogenide aerogels are provided. Some methods include adding at least one solvent to one or more two-dimensional transition metal dichalcogenide sheets to form a transition metal dichalcogenide solution and freeze drying the transition metal dichalcogenide solution to form frozen transition metal dichalcogenide. The methods also include heating the frozen transition metal dichalcogenide to form a transition metal dichalcogenide aerogel.

Claims (17)

1. A method of forming a transition metal dichalcogenide aerogel, the method comprising:

adding a cleaving agent to a transition metal dichalcogenide mixture to form one or more two-dimensional transition metal dichalcogenide sheets;

adding at least one solvent to the one or more two-dimensional transition metal dichalcogenide sheets to form a transition metal dichalcogenide solution;

freeze drying the transition metal dichalcogenide solution to form a frozen transition metal dichalcogenide; and

heating the frozen transition metal dichalcogenide to form the transition metal dichalcogenide aerogel.

2. The method of claim 1 , wherein adding the at least one solvent to the one or more two-dimensional transition metal dichalcogenide sheets comprises adding the at least one solvent to 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 (TiNCl), antimony telluride (Sb 2 Te 3 ), melonite (NiTe 2 ), or combinations thereof.

3. The method of claim 1 , wherein adding at least one solvent to the one or more two-dimensional transition metal dichalcogenide sheets comprises adding the at least one solvent to 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 NCl.

4. The method of claim 1 , further comprising sonicating the transition metal dichalcogenide solution prior to freeze drying the solution.

5. The method of claim 4 , wherein the sonicating is carried out for about 30 minutes to about 45 minutes, at a power of about 170 Watts (W) and a duty cycle of about 180 s/cycle.

6. The method of claim 1 , wherein adding the at least one solvent comprises adding ethanol, methanol, isopropyl alcohol, or combinations thereof.

7. The method of claim 6 , wherein adding the at least one solvent comprises adding the at least one solvent in a concentration of about 10% to about 15%.

8. The method of claim 1 , wherein heating the frozen transition metal dichalcogenide is carried out in an inert atmosphere at a temperature of about 175° C. to about 250° C. for about 20 minutes to about 45 minutes.

9. The method of claim 1 , wherein freeze drying the transition metal dichalcogenide solution comprises freezing the solution using ice bath and salt, lyophilization, or combinations thereof.

10. The method of claim 1 , further comprising forming the transition metal dichalcogenide mixture by reacting a transition metal dichalcogenide with a cross-linking agent and an activating agent.

11. The method of claim 1 , further comprising adding at least one inorganic oxide to the two-dimensional transition metal dichalcogenide sheets prior to freeze drying the transition metal dichalcogenide solution.

12. The method of claim 11 , wherein adding the at least one inorganic oxide comprises adding boric oxide, barium oxide (BaO), praseodymium oxide (Pr 2 O 3 ), lanthanide oxide (Ln 2 O 3 ), manganese dioxide (MnO 2 ), or combinations thereof.

13. An aerogel made by the method of claim 1 .

Assignments (3)
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 24, 2014
From: THEVASAHAYAM, AROCKIADOSS
To: EMPIRE TECHNOLOGY DEVELOPMENT LLC
Reel/Frame 034024/0178 →
Priority Claims (1)
IN 4797/CHE/2013 · Oct 24, 2013 · national
Continuity (1)
Related Publication 20150118467A1 · Apr 30, 2015