IP Library Granted Patent US 9,853,284
Granted Patent B2
US 9,853,284 · App. 15/498,113 · Granted Dec 26, 2017

Graphene oxide as a sulfur immobilizer in high performance lithium/sulfur cells

Inventors: Yuegang Zhang (Cupertino, CA); Elton J. Cairns (Walnut Creek, CA); Liwen Ji (Richland, WA); Mumin Rao (El Cerrito, CA)
Assignee: The Regents of the University of California
H01M4/364C01B31/043C01B31/26C07D303/38H01M4/382H01M4/587H01M10/0525H01M10/0566C01P2002/72C01P2002/82C01P2002/85C01P2002/88C01P2004/03C01P2004/04C01P2006/40H01M2300/0045
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Quick Facts
Patent No.
US 9,853,284
App. No.
15/498,113
Granted
Dec 26, 2017
Kind
B2
Abstract

The loss of sulfur cathode material as a result of polysulfide dissolution causes significant capacity fading in rechargeable lithium/sulfur cells. Embodiments of the invention use a chemical approach to immobilize sulfur and lithium polysulfides via the reactive functional groups on graphene oxide. This approach obtains a uniform and thin (˜tens of nanometers) sulfur coating on graphene oxide sheets by a chemical reaction-deposition strategy and a subsequent low temperature thermal treatment process. Strong interaction between graphene oxide and sulfur or polysulfides demonstrate lithium/sulfur cells with a high reversible capacity of 950-1400 mAh g −1 , and stable cycling for more than 50 deep cycles at 0.1 C.

Claims (15)

1. A method of preparing a graphene oxide-sulfur (GO—S) nanocomposite comprising:

providing a graphene oxide (GO) dispersion;

adding a sodium polysulfide solution to the GO dispersion to form a blended solution;

titrating the GO/sodium polysulfide blended solution into a HCOOH solution to form a precipitate; and

heat treating, for a specified time and temperature, the precipitate in a sealed vessel utilizing a flowing gas at a specified gas flow rate.

2. The method of claim 1 , wherein the flowing gas is argon.

3. The method of claim 1 , wherein the gas flow rate is approximately 200 cc S −1 .

4. The method of claim 1 , wherein the temperature is approximately 155° C.

5. The method of claim 1 , wherein the time is approximately 12 hours.

6. The method of claim 1 , wherein the sodium polysulfide solution is added to the GO dispersion in the presence of 5 wt % surfactant cetyl trimethylammonium bromide (CTAB).

7. The method of claim 1 , wherein the sodium polysulfide solution is prepared by adding Na 2 S into a flask that has been filled with distilled water to form a Na 2 S solution, then elemental S is suspended in the Na 2 S solution, wherein the ratios of Na 2 S and elemental S, are adjusted to determine a value of x in Na 2 S x of the sodium polysulfide solution.

8. The method of claim 7 , wherein the GO after the heat treatment comprises approximately 50-90 wt % S.

9. The method of claim 8 , wherein the GO after the heat treatment comprises approximately 60-70 wt % S.

10. The method of claim 1 , wherein the graphene oxide (GO) dispersion is prepared by exfoliating GO from a graphite oxide.

11. The method of claim 10 , wherein the graphite oxide was prepared using a modified Hummers method.

Assignments (3)
CONFIRMATORY LICENSE Recorded Apr 5, 2018
From: UNIVERSITY OF CALIF-LAWRENC BERKELEY LAB
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 045450/0456 →
CONFIRMATORY LICENSE Recorded May 17, 2017
From: THE REGENTS OF THE UNIVERSITY OF CALIFORNIA
To: ENERGY, UNITED STATES DEPARTMENT OF
Reel/Frame 042522/0356 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 26, 2017
From: ZHANG, YUEGANG; CAIRNS, ELTON J.; JI, LIWEN; RAO, MUMIN
To: THE REGENTS OF THE UNIVERSITY OF CALIFORNIA
Reel/Frame 042155/0571 →
Continuity (3)
Division 14347600
Provisional Application 61541374 · Sep 30, 2011
Related Publication 20170294646A1 · Oct 12, 2017