IP Library Granted Patent US 7,666,915
Granted Patent B2
US 7,666,915 · App. 11/860,373 · Granted Feb 23, 2010

Highly dispersible carbon nanospheres in a polar solvent and methods for making same

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Quick Facts
Patent No.
US 7,666,915
App. No.
11/860,373
Granted
Feb 23, 2010
Kind
B2
Abstract

The particle sizes of agglomerates of carbon nanospheres are reduced by dispersing the carbon nanospheres in a polar solvent. The carbon nanospheres are multi-walled, hollow, graphitic structures with an average diameter in a range from about 10 nm to about 200 nm, more preferably about 20 nm to about 100 nm. Spectral data shows that prior to being dispersed, the carbon nanospheres are agglomerated into clusters that range in size from 500 nm to 5 microns. The clusters of nanospheres are reduced in size by dispersing the carbon nanospheres in the polar solvent (e.g., water) using a surface modifying agent (e.g., glucose) and ultrasonication. The combination of polar solvent, surface modifying agent, and ultrasonication breaks up and disperses agglomerates of carbon nanospheres.

Claims (34)

1. A method for manufacturing a carbon nanomaterial dispersion, comprising,

(i) providing a carbon nanomaterial comprising a plurality of multi-walled, graphitic carbon nanospheres that have been separated from amorphous carbon, wherein the plurality of carbon nanospheres are at least partially agglomerated into a plurality of clusters of carbon nanospheres;

(ii) forming a solution comprised of a polar solvent and an organic surface modifying agent, wherein the surface modifying agent is selected from the group consisting of glucose, glycolic acid, glycine, ascorbic acid, sodium dodecyl benzene sulfonate, and combinations thereof;

(iii) mixing the carbon nanomaterial with the solution; and

(iv) ultrasonicating the solution containing the polar solvent, organic surface modifying agent, and carbon nanomaterial to at least partially disrupt the clusters of carbon nanospheres to yield carbon nanospheres suspended in the solution.

2. A method as in claim 1 , wherein the carbon nanomaterial in step (i) has an average particle size greater than about 500 nm as measured using dynamic light scattering.

3. A method as in claim 1 , wherein the carbon nanomaterial in step (iv) has an average particle size less than about 500 nm as measured using dynamic light scattering.

4. A method as in claim 1 , wherein the carbon nanomaterial in step (iv) has an average particle size less than about 300 nm as measured using dynamic light scattering.

5. A method as in claim 1 , wherein the carbon nanomaterial in step (iv) has an average particle size less than about 200 nm as measured using dynamic light scattering.

6. A method as in claim 1 , wherein the polar solvent comprises water, an alcohol, THF, or a combination thereof.

7. A method as in claim 1 , wherein the surface modifying agent is selected from the group consisting of a surfactant, an organic acid, a carbohydrate, an amino acid, and combinations thereof.

8. A method as in claim 1 , wherein the surface modifying agent is biocompatible.

9. A method as in claim 1 , wherein the surface of the carbon nanomaterial has at least about 2 wt % oxygen as measured using X-ray photoelectron spectroscopy (XPS).

10. A method as in claim 1 , wherein the carbon nanospheres are ultrasonicated for at least about 30 minutes.

11. A method as in claim 1 , wherein the carbon nanospheres are manufactured by:

forming a precursor mixture comprising a carbon precursor and a plurality of templating nanoparticles and polymerizing the carbon precursor, the templating nanoparticles comprising a catalytic metal;

carbonizing the precursor mixture to form an intermediate carbon material comprising a plurality of carbon nanostructures, amorphous carbon, and optionally remaining catalytic metal; and

purifying the intermediate carbon material by removing at least a portion of the amorphous carbon and optionally a portion of any remaining catalytic metal, thereby yielding the carbon nanomaterial comprising a plurality of carbon nanostructures provided in step (i).

12. A method as in claim 11 , in which the templating nanoparticles are prepared by,

(a) reacting a plurality of precursor catalyst atoms with a plurality of organic dispersing agent molecules to form complexed catalyst atoms; and

(b) allowing or causing the complexed catalyst atoms to form the templating nanoparticles.

13. A method for manufacturing a carbon nanomaterial dispersion, comprising:

(i) providing an agglomerated carbon nanomaterial comprising a plurality of multi-walled, graphitic carbon nanospheres that have been separated from amorphous carbon, the carbon nanospheres having an average diameter in a range from about 10 nm to about 200 nm and having an irregular surface;

(ii) forming a solution comprised of a polar solvent and an organic surface modifying agent, wherein the surface modifying agent is selected from the group consisting of glucose, glycolic acid, glycine, ascorbic acid, sodium dodecyl benzene sulfonate, and combinations thereof;

(iii) mixing the carbon nanomaterial with the solution; and

(iv) sonicating the solution containing the polar solvent, organic surface modifying agent, and carbon nanomaterial to cause at least a portion of the surface modifying agent molecules to bond to the carbon nanospheres and suspend the carbon nanospheres in the solution.

14. A method as in claim 13 , wherein the carbon nanomaterial provided in step (i) has an average particle size in a range from about 500 nm to about 5 microns as measured using dynamic light scattering and wherein the carbon nanomaterial in step (iv) has an average particle size less than about 300 nm as measured using dynamic light scattering.

15. A method as in claim 13 , wherein the carbon nanomaterial provided in step (i) has an average particle size in a range from about 500 nm to about 5 microns as measured using dynamic light scattering and wherein the carbon nanomaterial in step (iv) has an average particle size less than about 200 nm as measured using dynamic light scattering.

16. A method as in claim 13 , wherein the polar solvent comprises water.

17. A method as in claim 13 , wherein the surface modifying agent comprises one or more functional groups selected from the group consisting of carboxyl, amine, sulfonate, and hydroxyl.

18. A method as in claim 13 , the method yielding a carbon nanomaterial dispersion comprising:

the polar solvent; and

the carbon nanospheres suspended in the polar solvent, wherein the carbon nanospheres have an asapect ratio less than about 3:1 and a plurality of surface modifying agent molecules bonded to the surface thereof.

19. A method as in claim 1 , wherein the polar solvent comprises water.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 22, 2015
From: HEADWATERS TECHNOLOGY INNOVATION, LLC
To: HEADWATERS TECHNOLOGY INNOVATION GROUP, INC.
Reel/Frame 035492/0219 →
PATENT RELEASE (REEL:23699/FRAME:0452) Recorded Mar 26, 2015
From: WILMINGTON TRUST, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
To: HEADWATERS INCORPORATED, AS GRANTOR; HEADWATERS RESOURCES, INC., A UTAH CORPORATION; HEADWATERS TECHNOLOGY INNOVATION GROUP, INC., A UTAH CORPORATION; HEADWATERS HEAVY OIL, LLC, A UTAH CORPORATION; TAPCO INTERNATIONAL CORPORATION, A MICHIGAN CORPORATION
Reel/Frame 035306/0558 →
SECURITY AGREEMENT Recorded Nov 20, 2009
From: HEADWATERS INCORPORATED, A DELAWARE CORPORATION; HEADWATERS CTL, LLC, A UTAH LIMITED LIABILITY COMPANY, USA; HEADWATERS HEAVY OIL, LLC, A UTAH LIMITED LIABILITY COMPANY, USA; HEADWATERS RESOURCES, INC., A UTAH CORPORATION, USA; HEADWATERS TECHNOLOGY INNOVATION GROUP, INC., A UTAH CORPORATION, USA; TAPCO INTERNATIONAL CORPORATION, A MICHIGAN CORPORATION, USA
To: WILMINGTON TRUST FSB, AS COLLATERAL AGENT
Reel/Frame 023699/0452 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 27, 2007
From: ZHANG, CHENG; ZHOU, BING
To: HEADWATERS TECHNOLOGY INNOVATION LLC
Reel/Frame 019889/0070 →