Graphene/graphite polymer composite foam derived from emulsions stabilized by graphene/graphite kinetic trapping

Patent metadata

Field	Value
Publication number	US-9646735-B2
Application number	US-201514724499-A
Country	US
Kind code	B2
Filing date	May 28, 2015
Priority date	May 30, 2014
Publication date	May 9, 2017
Grant date	May 9, 2017

Abstract

The present disclosure provides advantageous graphene/graphite stabilized composites (e.g., graphene/graphite stabilized emulsion-templated foam composites), and improved methods for fabricating such graphene/graphite stabilized composites. More particularly, the present disclosure provides improved methods for fabricating pristine, graphene/graphite/polymer composite foams derived from emulsions stabilized by graphene/graphite kinetic trapping. In exemplary embodiments, the present disclosure provides that, instead of viewing the insolubility of pristine graphene/graphite as an obstacle to be overcome, it is utilized as a means to create or fabricate water/oil emulsions, with graphene/graphite stabilizing the spheres formed. These emulsions are then the frameworks used to make foam composites that have shown bulk conductivities up to about 2 S/m, as well as compressive moduli up to about 100 MPa and breaking strengths of over 1200 psi, with densities as low as about 0.25 g/cm 3 .

First claim

What is claimed is:

1. A method for fabricating a composite comprising:
a) providing a phase separated system of two non-mixing solvents, the phase separated system including: (i) a first solvent and a second solvent, and (ii) an interface between the first and second solvents;
b) introducing a substantially pristine layered material to the interface of the phase separated system wherein the substantially pristine layered material includes pristine graphene or graphite;
c) forming an emulsion of the first and second solvents, at least a portion of the substantially pristine layered material stabilizing the emulsion; and
d) adding a monomer and polymerizing the first solvent phase of the emulsion to form a matrix material having cavities lined with portions of the substantially pristine layered material.

2. The method of claim 1 , wherein the first solvent is an oil and the second solvent is water;
wherein the emulsion is a water/oil emulsion;
wherein the oil phase of the emulsion is the continuous phase of the emulsion; and
wherein after step c), the water/oil emulsion includes spheres of water surrounded by oil, the spheres of water coated and stabilized by layers or sheets of the layered material.

3. The method of claim 2 , wherein the oil is styrene and the substantially pristine layered material is substantially pristine graphite;
wherein the emulsion is formed via mixing and sonication; and
wherein after step d), the matrix material includes polystyrene.

4. The method of claim 1 , wherein the first solvent phase of the emulsion includes monomers selected from the group consisting of styrene, isoprene, butyl acrylate, divinylbenzene, methyl acrylate, tetra(ethylene glycol) diacrylate, and butyl methacrylate.

5. The method of claim 1 , wherein the cavities of the matrix material include substantially spherical cavities.

6. The method of claim 1 , wherein step d) includes a thermally initiated free-radical polymerizing step/process.

7. The method of claim 1 , wherein after step d), the second solvent is removed from the matrix material;
wherein the second solvent is removed from the matrix material via an evaporation step/process; and
wherein after the second solvent is removed from the matrix material, the matrix material has an open pore foam structure.

8. The method of claim 1 , wherein the portions of the substantially pristine layered material lining the cavities include individual sheets or layers of graphene or graphite.

9. The method of claim 7 , wherein after the second solvent is removed from the matrix material, the matrix material has a bulk conductivity of about 2 S/m, a compressive modulus of about 100 MPa, a breaking strength of at least about 1200 psi, and a density of about 0.25 g/cm 3 .

10. The method of claim 1 , wherein the first solvent is an oil and the second solvent is water; and
wherein the emulsion is a water/oil emulsion.

11. The method of claim 1 , wherein the first solvent phase of the emulsion is the continuous phase of the emulsion; and
wherein the matrix material is a polymeric matrix material.

12. The method of claim 1 , wherein the second solvent phase of the emulsion is also polymerized to form the matrix material; and
wherein prior to polymerization, the second solvent phase of the emulsion includes monomers.

13. The method of claim 1 , wherein after step d) the matrix material is electrically conductive.

14. The method of claim 1 , wherein prior to step d) the second solvent includes poly(3,4-ethylenedioxythiophene) poly(styrenesulfonate); and
wherein after step d) the poly(3,4-ethylenedioxythiophene) poly(styrenesulfonate) forms a conductive coating on at least a portion of the cavities of the matrix material.

15. The method of claim 7 , wherein after the second solvent is removed from the matrix material, the matrix material is contacted with a solution containing poly(3,4-ethylenedioxythiophene) poly(styrenesulfonate); and
wherein after contacting the matrix material with the solution containing poly(3,4-ethylenedioxythiophene) poly(styrenesulfonate), the matrix material is dried and the poly(3,4-ethylenedioxythiophene) poly(styrenesulfonate) forms a conductive coating on at least a portion of the cavities of the matrix material.

16. A method for fabricating a composite comprising:
a) providing a phase separated system, wherein the phase separated system is an oil and water based system having an interface between the oil and water;
b) introducing substantially pristine graphene or substantially pristine graphite to the interface of the oil and water based system wherein the substantially pristine layered material includes pristine graphene or graphite;
c) forming a water/oil emulsion with the oil phase of the emulsion including monomers, the water/oil emulsion including spheres of water surrounded by oil, the spheres of water coated and stabilized by layers or sheets of the substantially pristine graphene or substantially pristine graphite;
d) polymerizing the oil phase of the emulsion to form a polymeric matrix material having substantially spherical cavities lined with layers or sheets of the substantially pristine graphene or substantially pristine graphite, the oil phase of the emulsion the continuous phase of the emulsion; and
e) removing the water from the polymeric matrix material;
wherein after step e), the polymeric matrix material has an open pore foam structure, and is electrically conductive.

Assignees

• Univ Connecticut

Inventors

• Adamson Douglas H
• Woltornist Steven
• Dobrynin Andrey V

Classifications

• B01J20/3272

  Polymers obtained by reactions otherwise than involving only carbon to carbon unsaturated bonds · CPC title

• B01J20/321

  consisting of a polymer obtained by reactions involving only carbon to carbon unsaturated bonds · CPC title

• B01J20/28095

  Shape or type of pores, voids, channels, ducts · CPC title

• B01J20/28026

  Particles within, immobilised, dispersed, entrapped in or on a matrix, e.g. a resin · CPC title

• B01J20/262

  obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation (macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds per se C08G) · CPC title