IP Library Granted Patent US 9,441,076
Granted Patent B2
US 9,441,076 · App. 12/945,043 · Granted Sep 13, 2016

Multifunctional graphene-silicone elastomer nanocomposite, method of making the same, and uses thereof

Inventors: Shuyang Pan (Southgate, MI); Ilhan A. Aksay (Princeton, NJ); Robert K. Prud'Homme (Lawrenceville, NJ)
Assignee: The Trustees of Princeton University
C08G77/16B82Y30/00C08G77/18C08G77/20C08L83/04
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Quick Facts
Patent No.
US 9,441,076
App. No.
12/945,043
Granted
Sep 13, 2016
Kind
B2
Abstract

A nanocomposite composition having a silicone elastomer matrix having therein a filler loading of greater than 0.05 wt %, based on total nanocomposite weight, wherein the filler is functional graphene sheets (FGS) having a surface area of from 300 m 2 /g to 2630 m 2 /g; and a method for producing the nanocomposite and uses thereof.

Claims (36)

1. A method for production of a nanocomposite composition comprising a silicone elastomer matrix and functionalized graphene sheets having a surface area of from 300 m 2 /g to 2630 m 2 /g, comprising:

dispersing functional graphene sheets (FGS) in a polar solvent to form an FGS suspension;

combining the FGS suspension with a vinyl terminated polysiloxane;

removing the polar solvent;

combining the resulting mixture with a crosslinker and a hydrosilylation catalyst; and

curing the resulting mixture to provide the nanocomposite;

wherein the functional graphene sheets have a loading of greater than 0.05 wt %, based on total nanocomposite weight; and

wherein the functional graphene sheets are present within the nanocomposite in a continuous three-dimensional connected network in a manner wherein individual functional graphene sheets have nanometer scale separation at contact points between individual functional graphene sheets.

2. The method of claim 1 , wherein the curing is performed at elevated temperature for a period of time from 1 to 48 hours.

3. The method of claim 2 , wherein the curing temperature is about 100° C.

4. The method of claim 2 , wherein the curing is performed for a period of time from 5 to 30 hours.

5. The method of claim 4 , wherein the curing is performed for a period of time from 20 to 25 hours.

6. The method of claim 5 , wherein the curing is performed for a period of time of approximately 24 hours.

7. The method of claim 3 , wherein the curing is performed for a period of time of approximately 24 hours.

8. The method of claim 1 , wherein the functional graphene sheets have a loading of from 0.05 to 5 wt %, based on total nanocomposite weight.

9. The method of claim 1 , wherein the functional graphene sheets have a loading of from 0.1 to 5 wt %, based on total nanocomposite weight.

10. The method of claim 1 , wherein the functional graphene sheets have a loading of from 0.5 to 3 wt %, based on total nanocomposite weight.

11. The method of claim 1 , wherein the functional graphene sheets have a loading of from 1 to 3 wt %, based on total nanocomposite weight.

12. The method of claim 1 , wherein the silane cross-linker is a member selected from the group consisting of tetrakis(dialkylsiloxy)silanes and poly(hydromethyl siloxane) crosslinkers.

13. The method of claim 1 , wherein the silane cross-linker is a tetrakis(dimethylsiloxy)silane.

14. The method of claim 1 , wherein the vinyl-terminated polysiloxane has a viscosity of from 100 to 300,000 mPas.

15. The method of claim 1 , wherein the hydrosilylation catalyst is a member selected from the group consisting of chloroplatinic acid, elementary platinum, solid platinum supported on a carrier; platinum-vinylsiloxane complexes; platinum-phosphine complexes; platinum-phosphite complexes; Pt (acac) 2 , wherein (acac) represents acetylacetonate group; platinum-hydrocarbon conjugates; platinum alcoholates; RhCl(PPh 3 ) 3 ; RhCl 3 ; Rh/Al 2 O 3 ; RuCl 3 ; IrCl 3 ; FeCl 3 ; AlCl 3 ; PdCl 2 .2H 2 O; NiCl 2 ; and TiCl 4 .

16. The method of claim 1 , wherein the catalyst is a platinum-vinylsiloxane complex and/or a platinum-cyclovinylmethylsiloxane complex.

17. The method of claim 1 , wherein the vinyl-terminated polysiloxane is poly(dimethylsiloxane).

18. A article formed from a nanocomposite produced by the method of claim 1 .

19. The article of claim 18 , wherein the article is formed by casting.

20. The article of claim 18 , wherein the article is formed by molding.

21. The article of claim 18 , wherein the article is a member selected from the group consisting of coatings, adhesives, sealants, flexible electrodes, actuators, pressure sensors, printed circuits, and electromagnetic interference shielding materials.

22. A method for production of a nanocomposite composition comprising a silicone elastomer matrix and functionalized graphene sheets having a surface area of from 300 m 2 /g to 2630 m 2 /g, comprising:

dispersing functional graphene sheets (FGS) in a polar solvent to form an FGS suspension;

combining the FGS suspension with a vinyl terminated polysiloxane having a viscosity of from 100 to 300,000 mPas;

removing the polar solvent;

combinimg the resulting mixture with a crosslinker and a hydrosilylation catalyst, wherein the silane cross-linker is a member selected from the group consisting of tetrakis(dialkylsiloxy)silanes and poly(hydromethyl siloxane) crosslinkers, and wherein the hydrosilylation catalyst is a member selected from the group consisting of chloroplatinic acid, elementary platinum, solid platinum supported on a carrier; platinum-vinylsiloxane complexes; platinum-phosphine complexes; platinum-phosphite complexes; Pt (acac), wherein (acac) represents acetylacetonate group; platinum-hydrocarbon conjugates; platinum alcoholates; RhCl(PPh 3 ) 3 ; RhCl 3 ; Rh/Al 2 O 3 ; RuCl 3 ; IrCl 3 ; FeCl 3 ; AlCl 3 ; PdCl 2 .2H 2 O; NiCl 2 ; and TiCl 4 ; and

curing the resulting mixture to provide the nanocomposite, wherein the curing is performed at elevated temperature for a period of time from 1 to 48 hours;

wherein the functional graphene sheets have a loading of greater than 0.05 wt %, based on total nanocomposite weight; and

wherein the functional graphene sheets are present within the nanocomposite in a continuous three-dimensional connected network in a manner wherein individual functional graphene sheets have nanometer scale separation at contact points between individual functional graphene sheets.

Assignments (3)
LICENSE Recorded May 11, 2018
From: PRINCETON UNIVERSITY
To: UNITED STATES OF AMERICA AS REPRESENTED BY THE ADMINISTRATOR OF THE NATIONAL AERONAUTICS AND SPACE ADMINISTRATION
Reel/Frame 046136/0188 →
CONFIRMATORY LICENSE Recorded Sep 2, 2016
From: PRINCETON UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 039910/0055 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 1, 2011
From: PAN, SHUYANG; AKSAY, ILHAN A; PRUD'HOMME, ROBERT K
To: THE TRUSTEES OF PRINCETON UNIVERSITY
Reel/Frame 026059/0165 →
Continuity (2)
Provisional Application 61260538 · Nov 12, 2009
Related Publication 20110178224A1 · Jul 21, 2011