IP Library Granted Patent US 9,919,264
Granted Patent B2
US 9,919,264 · App. 15/187,305 · Granted Mar 20, 2018

Enhanced graphene oxide membranes and methods for making same

Inventors: Yongsoon Shin (Richland, WA); David W. Gotthold (Richland, WA); Leonard S. Fifield (Richland, WA); Wei Liu (Richland, WA)
Assignee: BATTELLE MEMORIAL INSTITUTE
B01D53/228B01D67/0048B01D67/0093B01D69/02B01D71/021B01D53/268B01D2323/48B01D2325/04
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Quick Facts
Patent No.
US 9,919,264
App. No.
15/187,305
Granted
Mar 20, 2018
Kind
B2
Abstract

A method for making a graphene oxide membrane and a resulting free-standing graphene oxide membrane that provides desired qualities of water permeability and selectivity at larger sizes, thinner cross sections, and with increased ruggedness as compared to existing membranes and processes.

Claims (11)

1. A method for making a graphene oxide membrane, comprising the step of:

casting a gel dispersion comprising graphene oxide (GO) flakes having an average diameter greater than or equal to about 100 micrometers at a substantially neutral pH onto a receiving surface.

2. The method of claim 1 , further including the step of air drying the gel dispersion on the receiving surface to form the membrane.

3. The method of claim 1 , wherein the gel dispersion includes a pH selected from about 5 to about 7.5.

4. The method of claim 1 , wherein the graphene oxide (GO) flakes in the gel has a concentration between about 1% to about 3% by weight.

5. The method of claim 1 , wherein the gel dispersion is formed by a process including placing a graphite solid with a particle size greater than about 150 micrometers into a concentrated acid solution without sonicating or stirring the graphite for a time sufficient to form a quantity of graphite oxide.

6. The method of claim 5 , further comprising the step of adding KMnO 4 powder to the concentrated acid solution to form individual layers of graphene oxide (GO) therein.

7. The method of claim 6 , further comprising the step of adding the individual layers of graphene oxide (GO) to a H 2 O 2 /H 2 O solution to neutralize unreacted KMnO 4 .

8. The method of claim 7 , further including washing the individual layers of graphene oxide (GO) in the neutral solution without stirring or rotating the GO and acidifying the neutral solution to remove reduced metal as metal ions therefrom.

9. The method of claim 8 , further including iteratively rinsing and centrifuging the individual layers of graphene oxide (GO) in the previously acidified solution with distilled H 2 O to obtain a solution with a pH between about 5 and about 7.5 and removing GO flakes of a diameter less than about 5 micrometers therefrom.

10. The method of claim 1 , further comprising using a draw-bar to draw the dispersion down to the selected thickness.

Assignments (2)
CONFIRMATORY LICENSE Recorded Jul 18, 2016
From: BATTELLE MEMORIAL INSTITUTE, PACIFIC NORTHWEST DIVISION
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 039176/0543 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 29, 2016
From: SHIN, YONGSOON; GOTTHOLD, DAVID W.; FIFIELD, LEONARD S.; LIU, WEI
To: BATTELLE MEMORIAL INSTITUTE
Reel/Frame 039042/0803 →
Continuity (2)
Provisional Application 62201478 · Aug 5, 2015
Related Publication 20170036172A1 · Feb 9, 2017