IP Library Granted Patent US 7,960,440
Granted Patent B2
US 7,960,440 · App. 11/869,545 · Granted Jun 14, 2011

Highly dispersible carbon nanospheres in an organic solvent and methods for making same

Assignee: Headwaters Technology Innovation LLC
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Quick Facts
Patent No.
US 7,960,440
App. No.
11/869,545
Granted
Jun 14, 2011
Kind
B2
Abstract

The particle sizes of agglomerates of carbon nanospheres are reduced by dispersing the carbon nanospheres in an organic 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 an organic solvent containing at least one heteroatom (e.g., NMP) using ultrasonication. The combination of organic solvent 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 having an aspect ratio of less than about 3:1 and optionally an irregular surface with surface defects, wherein the plurality of carbon nanospheres are at least partially agglomerated into a plurality of clusters of carbon nanospheres 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 a carbon nanomaterial comprising a plurality of carbon nanostructures;

(ii) providing an organic solvent comprised of a plurality of organic molecules that each include at least one heteroatom; and

(iii) mixing the carbon nanomaterial with the solvent to form a mixture and ultrasonicating the mixture to at least partially disrupt the agglomeration of the carbon nanospheres to yield carbon nanospheres suspended in the organic solvent.

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 (iii) has an average particle size of less than about 500 nm as measured using dynamic light scattering.

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

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

6. A method as in claim 1 , wherein the organic solvent comprises at least one of methylpyrrolidone (NMP), pyridine, 1-(3 aminopropyl)imidazoles, 1-diethoxy methyl imidazoles, 1-2(hydroxyethyl)imidazoles, 4(1H-imidazole-1-yl)aniline, 4(imidazole 1-yl)phenol, barbituric acid, 1-methyl 2-pyrrolidinone hydrazone hydrochloride, quinoxaline, 1-ethyl-4-piperidone, 1-ethylpiperazine, or ethyl 2-picolinate.

7. A method as in claim 1 , wherein the at least one heteroatom is an oxygen atom, a nitrogen atom, or both.

8. A method as in claim 1 , wherein the organic solvent comprises a heterocyclic compound.

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 surface of the carbon nanomaterial has at least about 4 wt % oxygen as measured using X-ray photoelectron spectroscopy.

11. A method as in claim 1 , wherein the surface of the carbon nanomaterial has at least about 8 wt % oxygen as measured using X-ray photoelectron spectroscopy.

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

13. A method as in claim 1 , 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.

14. A method for manufacturing a carbon nanomaterial dispersion, comprising;

(i) providing an agglomerated carbon nanomaterial comprising a plurality of multi-walled, graphitic carbon nanospheres, the carbon nanospheres having an aspect ratio of less than about 3:1, an average diameter in a range from about 10 nm to about 200 nm, and an irregular surface;

(ii) providing an organic solvent comprised of a heterocyclic compound; and

(iii) mixing the carbon nanomaterial with the organic solvent to form a mixture and ultrasonicating the mixture to cause at least a portion of the organic molecules to bond to the carbon nanospheres and suspend the carbon nanospheres in the organic solvent.

15. A method as in claim 14 , 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 (iii) has an average particle size less than about 300 nm as measured using dynamic light scattering.

16. A method as in claim 14 , 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 (iii) has an average particle size less than about 200 nm as measured using dynamic light scattering.

17. A method as in claim 14 , wherein the organic solvent comprises at least one of methylpyrrolidone (NMP), pyridine, 1-(3 aminopropyl)imidazoles, 1-diethoxy methyl imidazoles, 1-2(hydroxyethyl)imidazoles, 4(1H-imidazole-1-yl)aniline, 4(imidazole 1-yl)phenol, barbituric acid, 1-methyl 2-pyrrolidinone hydrazone hydrochloride, quinoxaline, 1-ethyl-4-piperidone, 1-ethylpiperazine, or ethyl 2-picolinate.

18. A method as in claim 14 , wherein the heterocyclic compound includes at least one heteroatom selected from an oxygen atom, a nitrogen atom, or both.

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

(i) providing a carbon nanomaterial comprising a plurality of multi-walled, graphitic carbon nanospheres having an aspect ratio of less than about 3:1, wherein the plurality of carbon nanospheres are at least partially agglomerated into a plurality of clusters of carbon nanospheres;

(ii) providing an organic solvent comprised of a heterocyclic compound; and

(iii) mixing the carbon nanomaterial with the solvent to form a mixture and ultrasonicating the mixture to at least partially disrupt the agglomeration of the carbon nanospheres to yield carbon nanospheres suspended in the organic solvent.

20. A method as in claim 19 , wherein the organic solvent comprises at least one of methylpyrrolidone (NMP), pyridine, 1-(3 aminopropyl)imidazoles, 1-diethoxy methyl imidazoles, 1-2 (hydroxyethyl)imidazoles, 4(1H-imidazole-1-yl)aniline, 4(imidazole 1-yl)phenol, barbituric acid, 1-methyl 2-pyrrolidinone hydrazone hydrochloride, quinoxaline, 1-ethyl-4-piperidone, 1-ethylpiperazine, or ethyl 2-picolinate.

Assignments (6)
RELEASE OF SECURITY INTEREST Recorded May 8, 2017
From: DEUTSCHE BANK AG NEW YORK BRANCH
To: HEADWATERS TECHNOLOGY INNOVATION GROUP, INC.; HEADWATERS HEAVY OIL, LLC
Reel/Frame 042422/0740 →
SECURITY AGREEMENT Recorded Sep 17, 2015
From: HEADWATERS TECHNOLOGY INNOVATION GROUP, INC.
To: DEUTSCHE BANK AG NEW YORK BRANCH, AS ADMINISTRATIVE AGENT
Reel/Frame 036628/0277 →
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 Oct 10, 2007
From: ZHANG, CHENG; ZHOU, BING
To: HEADWATERS TECHNOLOGY INNOVATION LLC
Reel/Frame 019941/0905 →
Continuity (1)
Related Publication 20090093554A1 · Apr 9, 2009