[미국특허]
METHOD FOR PREPARING GRAPHENE OXIDE FILMS AND FIBERS
원문보기
IPC분류정보
국가/구분
United States(US) Patent
공개
국제특허분류(IPC7판)
C01B-031/04
B01D-039/20
C09D-005/24
H01B-001/04
H01B-013/00
출원번호
US-0519937
(2014-10-21)
공개번호
US-0111449
(2015-04-23)
발명자
/ 주소
Cruz-Silva, Rodolfo
Morelos, Aaron
Terrones, Mauricio
Elias, Ana Laura
Perea-Lopez, Nestor
Endo, Morinobu
출원인 / 주소
Cruz-Silva, Rodolfo
인용정보
피인용 횟수 :
0인용 특허 :
0
초록▼
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 h
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.
대표청구항▼
1. A method for preparing graphene oxide film, comprising: a) preparing a graphene oxide gel slurry by concentration of a graphite oxide aqueous slurry;b) depositing the graphene oxide slurry on a surface;c) spreading the graphene oxide slurry on the low-friction surface by bar coating; andd) drying
1. A method for preparing graphene oxide film, comprising: a) preparing a graphene oxide gel slurry by concentration of a graphite oxide aqueous slurry;b) depositing the graphene oxide slurry on a surface;c) spreading the graphene oxide slurry on the low-friction surface by bar coating; andd) drying the graphene oxide slurry, thereby preparing graphene oxide film. 2. The method of claim 1, further comprising preparing graphene oxide by oxidation of graphite with at least one chemical selected from the group consisting of potassium permanganate, sodium permanganate, ammonia permanganate, potassium chromate, sodium chromate, potassium persulfate, sodium persulfate, ammonia persulfate, potassium nitrate, ammonia nitrate, sodium nitrate, sodium chlorate, potassium chlorate, and ammonium chlorate. 3. The method of claim 1, wherein the graphene oxide slurry is between 0.1 and 1.5% solids by weight, and has a pH between 1.0 and 5.0. 4. The method of claim 1, wherein the surface is a low-friction surface selected from the group consisting of polytetrafluoroethylene, fluorinated ethylene propylene copolymer (FEP), high density polyethylene (HDPE), perfluorinated alkoxy polymer resin (PFA), and fluorosilane treated glass. 5. The method of claim 1, wherein the solvent comprises at least one acid selected from the group consisting of sulfuric acid, phosphoric acid, nitric acid, perchloric acid, trichloroacetic acid, and dichloroacetic acid. 6. The method of claim 1, wherein the slurry comprises a plasticizer. 7. A method for preparing a dual-layer graphene-oxide film, comprising: a) preparing a graphene oxide film according to the method of claim 1; andb) applying a second layer to the graphene oxide film, wherein the second layer is selected from the group consisting of carbon nanotubes, graphene nanoplatelets, molybdenum disulfide, tungsten disulfide, polymer nanofiber, carbon fibers, and metallic nanowires. 8. A method for preparing a graphene oxide fiber, comprising: a) preparing a graphene oxide film according to the method of claim 1;b) cutting the graphene oxide film into strips; andc) dry-spinning the graphene oxide film strips into a fiber. 9. The method of claim 8, wherein the diameter of the fiber is between 40 μm to 2500 μm. 10. A method for preparing a reduced graphene oxide fiber, comprising: a) preparing a graphene oxide fiber according to the method of claim 8; andb) reducing the graphene oxide fiber by at least one of thermal reduction and chemical reduction. 11. The method of claim 10, 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. 12. The method of claim 10, wherein the graphene oxide fiber is reduced by thermal reduction, said thermal reduction occurring at temperatures between 180° C. and 3000° C. 13. The method of claim 10, 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 Ω·cm to 400 Ω·cm. 14. A method for preparing a graphene oxide weave, comprising preparing a plurality of graphene oxide fibers according to the method of claim 7; and weaving the graphene oxide fibers to form a graphene oxide weave. 15. A supported graphene oxide film, comprising: a graphene oxide film, said graphene oxide film bound to a support. 16. The film of claim 15, wherein said support is a textile support selected from the group consisting of paper, polymer fiber non-woven mat, cellulose nanofiber paper, non-woven carbon nanotube paper, and carbon fiber. 17. The film of claim 15, wherein said support is a non-textile support selected from the group consisting of metallic foil and polymer film.
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