IP Library › Granted Patent US 9,352,500
Granted Patent B2
US 9,352,500 · App. 14/396,000 · Granted May 31, 2016

Synthesis of three-dimensional graphene foam: use as supercapacitors

Inventors: Jonghak Lee (Singapore, SG); Barbaros Ozyilmaz (Singapore, SG); Orhan Kahya (Singapore, SG)
Assignee: National University of Singapore
B29C43/003C01B31/0438H01G11/26H01G11/28H01G11/34H01G11/36H01G11/48H01G11/68H01G11/70H01G11/86B29K2105/04B29L2031/00Y02E60/13Y10T29/43Y10T428/24997
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Quick Facts
Patent No.
US 9,352,500
App. No.
14/396,000
Granted
May 31, 2016
Kind
B2
Abstract

The application discloses methods of fabricating three-dimensional (3D) graphene crystalline foam, based on mixing a carbon source with a skelet (scaffold) powder. In one embodiment heat and pressure are used to compact the carbon and a metal powder into a close packed structure. In another embodiment a 3D crystalline graphene foam is fabricated with a large surface area (550 m 2 /g) from a 3D metal foam, depositing a layer of graphene using chemical vapor deposition (CVD), depositing a polymer support and removing the metal via wet chemical etching, such that the graphene retains the configuration, and then finally removing the polymer. A method of fabricating the metal foam framework and coating the metal with graphene are also disclosed.

Claims (26)

1. A method of fabricating a three-dimensional graphene crystalline foam, comprising:

a) mixing a carbon source and a skelet powder together to obtain a uniform mixture, wherein the carbon source is optionally coated on a group IV-B element;

b) applying pressure to the uniform mixture obtained in step (a) to obtain a closed packed structure;

c) applying temperature and pressure to the closed packed structure to form a graphene sheet layered around the skelet powder and the group IV-B element if present; and

d) removing the skelet powder from the closed packed structure using a chemical bath to dissolve the skelet powder away from the closed packed structure leaving voids, resulting in a three-dimensional crystalline foam comprising graphene and optionally a group IV-B element.

2. The method of claim 1 , wherein the carbon source is carbon black, amorphous carbon, or a combination thereof.

3. The method of claim 1 , wherein the optional group IV-B element is silicon (Si), germanium (Ge), tin (Sn), lead (Pb), or a combination thereof.

4. The method of claim 1 , wherein the carbon-coated group IV-B element is carbon-coated silicon nanoparticle.

5. The method of claim 1 , wherein the skelet powder is silicon dioxide (SiO2), aluminum oxide (A12O3), sodium chloride (NaCl), magnesium oxide (MgO), hafnium oxide (HfO2), zirconium dioxide (ZrO2), or a combination thereof.

6. The method of claim 1 , wherein the skelet powder has a particle size of between about 1 nm to 10 μm.

7. The method of claim 1 , wherein the pressure is applied in a uniform direction.

8. The method of claim 1 , wherein the chemical bath is aqueous potassium hydroxide or aqueous sodium hydroxide.

9. A method of fabricating a three-dimensional crystalline graphene foam, comprising:

a) providing a three-dimensional metal foam framework having a surface area of at least about 500 m2/g, for fabricating a three-dimensional graphene foam;

b) depositing a layer of graphene onto the metal foam of step (a) by template-directed chemical vapor deposition (CVD);

c) depositing a polymer support onto the graphene layer;

d) removing the three-dimensional metal foam framework via wet chemical etching, such that the graphene layer and the polymer support retain the three-dimensional configuration provided by the metal foam framework; and

e) removing the polymer support using a solvent to thereby obtain the three-dimensional crystalline graphene foams wherein the metal foam framework of step (a) is fabricated by:

i) mixing a metal powder and a skelet powder together to obtain a uniform mixture;

ii) applying pressure to the uniform mixture of the metal powder and the skelet powder to obtain a closed packed structure;

iii) applying temperature and pressure to the closed packed structure obtained in step (ii) to melt the metal powder around the skelet powder; and

iv) removing the skelet powder using a chemical bath to dissolve the skelet powder away from the closed packed structure leaving voids, resulting in a metal foam.

10. The method of claim 9 , wherein the metal powder is composed of nickel (Ni), cobalt (Co), copper (Cu), iron (Fe), platinum (Pt), or a combination thereof.

11. The method of claim 9 , wherein the skelet powder is silicon dioxide (SiO2), aluminum oxide (A12O3), sodium chloride (NaCl), magnesium oxide (MgO), hafnium oxide (HfO2), zirconium dioxide (ZrO2), or a combination thereof.

12. The method of claim 9 , wherein the skelet powder has a particle size of between about 1 nm to 10 gm.1.

13. The method of claim 9 , wherein the pressure is applied in a uniform direction.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 21, 2014
From: LEE, JONGHAK; OZYILMAZ, BARBAROS; KAHYA, ORHAN
To: NATIONAL UNIVERSITY OF SINGAPORE
Reel/Frame 033995/0951 →
Continuity (5)
Provisional Application 61654171 · Jun 1, 2012
Provisional Application 61657143 · Jun 8, 2012
Provisional Application 61810419 · Apr 10, 2013
Provisional Application 61810425 · Apr 10, 2013
Related Publication 20150104634A1 · Apr 16, 2015