Method for preparing graphene oxide films and fibers

Patent metadata

Field	Value
Publication number	US-9284193-B2
Application number	US-201414519937-A
Country	US
Kind code	B2
Filing date	Oct 21, 2014
Priority date	Oct 21, 2013
Publication date	Mar 15, 2016
Grant date	Mar 15, 2016

Abstract

We report a method of preparation of highly elastic graphene oxide films, and their transformation into graphene oxide fibers and electrically conductive graphene fibers by spinning. Methods typically include: 1) oxidation of graphite to graphene oxide, 2) preparation of graphene oxide slurry with high solid contents and residues of sulfuric acid impurities. 3) preparation of large area films by bar-coating or dropcasting the graphene oxide dispersion and drying at low temperature. 4) spinning the graphene oxide film into a fiber, and 5) thermal or chemical reduction of the graphene oxide fiber into an electrically conductive graphene fiber. The resulting films and fiber have excellent mechanical properties, improved morphology as compared with current graphene oxide fibers, high electrical conductivity upon thermal reduction, and improved field emission properties.

First claim

The invention claimed is:

1. A method for preparing a graphene oxide fiber, comprising:
a) preparing a graphene oxide film by:
preparing a graphene oxide gel slurry by concentration of a graphite oxide aqueous slurry:
depositing the graphene oxide slurry on a low friction surface;
spreading the graphene oxide slurry on the low-friction surface by bar coating; and
drying the graphene oxide slurry, thereby preparing graphene oxide film;

b) cutting the graphene oxide film into strips; and
c) dry-spinning the graphene oxide film strips into a fiber.

2. The method of claim 1 , wherein the diameter of the fiber is between 40 μm to 2500 μm.

3. A method for preparing a reduced graphene oxide fiber, comprising:
a) preparing a graphene oxide fiber according to the method of claim 1 ; and
b) reducing the graphene oxide fiber by at least one of thermal reduction and chemical reduction.

4. The method of claim 3 , wherein the graphene oxide fiber is reduced by chemical reduction, and wherein the chemical reduction is accomplished by a chemical reducing agent selected from the group consisting of hydrazine, sodium borohydride, hydroiodic acid (IA), ascorbic acid, and cysteamine.

5. The method of claim 3 , wherein the graphene oxide fiber is reduced by thermal reduction, said thermal reduction occurring at temperatures between 180 °C. and 3000°C.

6. The method of claim 3 , further comprising treating the graphene oxide fiber by a combination of heat treatment, followed by joule heating under inert or reducing atmosphere in which the conductivity reached range from 0.0001 Ωcm to 400 Ωcm.

7. A method for preparing a graphene oxide weave, comprising:
preparing a plurality of graphene oxide fibers by:
preparing a graphene oxide gel slurry by concentration of a graphite oxide aqueous slurry;
depositing the graphene oxide slurry on a low friction surface;
spreading the graphene oxide slurry on the low-friction surface by bar coating;
drying the graphere oxide slurry, thereby preparing graphene oxide film; and
applying a second layer to the graphene oxide film, wherein the second layer is selected from the group consisting of carbon nanotubes, grapheme nanoplatelets,

molybdenum disulfide, tungsten disulfide, polymer nanofiber, carbon fibers, and metallic nanowires; and
weaving the graphene oxide fibers to form a graphene oxide weave.

Assignees

• Penn State Res Found
• Univ Shinshu

Inventors

• Cruz-Silva Rodolfo
• Morelos Aaron
• Terrones Mauricio
• Elias Ana Laura
• Perea-Lopez Nestor
• Endo Morinobu

Classifications

• C09D5/24 Primary

  Electrically-conducting paints {(conductive materials H01B1/00)} · CPC title

• Y10T442/2984

  Coated or impregnated carbon or carbonaceous fiber fabric · CPC title

• Y10T442/277

  Coated or impregnated cellulosic fiber fabric · CPC title

• Y10T428/31678

  Of metal · CPC title

• C01B31/043 Primary

  Chemistry & Metallurgy · mapped topic