Daniel T Colbert

US Patent:

6645455, Nov 11, 2003

Filed:

Mar 16, 2001

Appl. No.:

09/810201

Inventors:

John L. Margrave - Bellaire TX
Edward T. Mickelson - Pearland TX
Robert Hauge - Houston TX
Peter Boul - Houston TX
Chad Huffman - Houston TX
Jie Liu - Chapel Hill NC
Richard E. Smalley - Houston TX
Ken Smith - Spring TX
Daniel T. Colbert - Houston TX

Assignee:

William Marsh Rice University - Houston TX

International Classification:

D01F 912

US Classification:

4234471, 423445 R, 423445 B, 423460

Abstract:

This invention is directed to making chemical derivatives of carbon nanotubes and to uses for the derivatized nanotubes, including making arrays as a basis for synthesis of carbon fibers. In one embodiment, this invention also provides a method for preparing single wall carbon nanotubes having substituents attached to the side wall of the nanotube by reacting single wall carbon nanotubes with fluorine gas and recovering fluorine derivatized carbon nanotubes, then reacting fluorine derivatized carbon nanotubes with a nucleophile. Some of the fluorine substituents are replaced by nucleophilic substitution. If desired, the remaining fluorine can be completely or partially eliminated to produce single wall carbon nanotubes having substituents attached to the side wall of the nanotube. The substituents will, of course, be dependent on the nucleophile, and preferred nucleophiles include alkyl lithium species such as methyl lithium. Alternatively, fluorine may be fully or partially removed from fluorine derivatized carbon nanotubes by reacting the fluorine derivatized carbon nanotubes with various amounts of hydrazine, substituted hydrazine or alkyl amine.

US Patent:

6683783, Jan 27, 2004

Filed:

Dec 22, 1999

Appl. No.:

09/380545

Inventors:

Richard E. Smalley - Houston TX
Daniel T. Colbert - Houston TX
Hongjie Dai - Sunnyvale CA
Jie Liu - Houston TX
Andrew G. Rinzler - Newberry FL
Jason H. Hafner - Somerville MA
Ken Smith - Spring TX
Ting Guo - La Jolla CA
Pavel Nikolaev - Houston TX
Andreas Thess - Kusterdingen, DE

Assignee:

William Marsh Rice University - Houston TX

International Classification:

D01F 912

US Classification:

361502, 423445 B, 4234472

Abstract:

A method for purifying a mixture comprising single-wall carbon nanotubes and amorphous carbon contaminate is disclosed. The method includes the steps of heating the mixture under oxidizing conditions sufficient to remove the amorphous carbon, followed by recovering a product comprising at least about 80% by weight of single-wall carbon nanotubes. A method for producing tubular carbon molecules of about 5 to 500 nm in length is also disclosed. The method includes the steps of cutting single-wall nanotube containing-material to form a mixture of tubular carbon molecules having lengths in the range of 5-500 nm and isolating a fraction of the molecules having substantially equal lengths. The nanotubes may be used, singularly or in multiples, in power transmission cables, in solar cells, in batteries, as antennas, as molecular electronics, as probes and manipulators, and in composites.

US Patent:

6692717, Feb 17, 2004

Filed:

Mar 16, 2001

Appl. No.:

09/787582

Inventors:

Richard E. Smalley - Houston TX
Jason H. Hafner - Somerville MA
Daniel T. Colbert - Houston TX
Ken Smith - Spring TX

Assignee:

William Marsh Rice University - Houston TX

International Classification:

D01F 912

US Classification:

423445B, 4234471, 4234473, 423445 R

Abstract:

Single-walled carbon nanotubes have been synthesized by the catalytic decomposition of both carbon monoxide and ethylene over a supported metal catalyst known to produce larger multi-walled nanotubes. Under certain conditions, there is no termination of nanotube growth, and production appears to be limited only by the diffusion of reactant gas through the product nanotube mat that covers the catalyst The present invention concerns a catalyst-substrate system which promotes the growth of nanotubes that are predominantly single-walled tubes in a specific size range, rather than the large irregular-sized multi-walled carbon fibrils that are known to grow from supported catalysts. With development of the supported catalyst system to provide an effective means for production of single-wall nanotubes, and further development of the catalyst geometry to overcome the diffusion limitation, the present invention will allow bulk catalytic production of predominantly single-wall carbon nanotubes from metal catalysts located on a catalyst supporting surface.

US Patent:

6749827, Jun 15, 2004

Filed:

Dec 28, 2001

Appl. No.:

10/032732

Inventors:

Richard E. Smalley - Houston TX
Daniel T. Colbert - Houston TX
Hongjie Dai - Sunnyvale CA
Jie Liu - Houston TX
Andrew G. Rinzler - Houston TX
Jason H. Hafner - Houston TX
Kenneth A. Smith - Houston TX
Ting Guo - La Jolla CA
Pavel Nikolaev - Houston TX
Andreas Thess - Martinsried, DE

Assignee:

William Marsh Rice University - Houston TX

International Classification:

D01F 912

US Classification:

4234473

Abstract:

This invention relates generally to a method for growing carbon fiber from single-wall carbon nanotube (SWNT) molecular arrays. In one embodiment, the present invention involves a macroscopic molecular array of at least about 10 tubular carbon molecules in generally parallel orientation and having substantially similar lengths in the range of from about 50 to about 500 nanometers. The hemispheric fullerene cap is removed from the upper ends of the tubular carbon molecules in the array. The upper ends of the tubular carbon molecules in the array are then contacted with a catalytic metal. A gaseous source of carbon is supplied to the end of the array while localized energy is applied to the end of the array in order to heat the end to a temperature in the range of about 500Â C. to about 1300Â C. The growing carbon fiber is continuously recovered.

US Patent:

6756025, Jun 29, 2004

Filed:

Dec 21, 2001

Appl. No.:

10/027568

Inventors:

Daniel T. Colbert - Houston TX
Hongjie Dai - Sunnyvale CA
Jason H. Hafner - Houston TX
Andrew G. Rinzler - Houston TX
Richard E. Smalley - Houston TX

Assignee:

William Marsh Rice University - Houston TX

International Classification:

D01F 9127

US Classification:

4234473, 423445 B

Abstract:

This invention relates generally to a method for growing single-wall carbon nanotube (SWNT) from seed molecules. The supported or unsupported SWNT seed materials can be combined with a suitable growth catalyst by opening SWNT molecule ends and depositing a metal atom cluster. In one embodiment, a suspension of seed particles containing attached catalysts is injected into an evaporation zone to provide an entrained reactive nanoparticle. A carbonaceous feedstock gas is then introduced into the nanoparticle stream under conditions to grow single-wall carbon nanotubes. Recovery of the product produced can be done by filtration, centrifugation and the like.

US Patent:

6756026, Jun 29, 2004

Filed:

Dec 21, 2001

Appl. No.:

10/027750

Inventors:

Daniel T. Colbert - Houston TX
Hongjie Dai - Sunnyvale CA
Jason H. Hafner - Houston TX
Andrew G. Rinzler - Houston TX
Richard E. Smalley - Houston TX
Kenneth A. Smith - Katy TX
Jie Liu - Chapel Hill NC
Ting Guo - Davis CA
Pavel Nikolaev - Houston TX
Andreas Thess - Kusterdingen, DE

Assignee:

William Marsh Rice University - Houston TX

International Classification:

D01F 912

US Classification:

4234473, 4234471, 4234472, 423445 R

Abstract:

This invention relates generally to a method for growing carbon fiber from single-wall carbon nanotube (SWNT) molecular arrays. The carbon fiber which comprises an aggregation of substantially parallel carbon nanotubes may be produced by growth (elongation) of a suitable seed molecular array. The first step is to open the growth end of the SWNTs in the molecular array. Next, a transition metal catalyst is added to the open-ended seed array. In the next step, the SWNT molecular array with catalyst deposited on the open tube ends is subjected to tube growth (extension) conditions. The carbon supply necessary to grow the SWNT molecular array into a continuous fiber is supplied to the SWNT molecular array tip heated to a temperature sufficient to cause growth to any desired length. The continuous carbon fiber can also be grown from more than one separately prepared molecular arrays or templates.

US Patent:

6761870, Jul 13, 2004

Filed:

Jul 1, 2002

Appl. No.:

09/830642

Inventors:

Richard E. Smalley - Houston TX
Ken A. Smith - Houston TX
Daniel T. Colbert - Houston TX
Pavel Nikolaev - Houston TX
Michael J. Bronikowski - Pasadena CA
Robert K. Bradley - Houston TX
Frank Rohmund - Huttlingen, DE

Assignee:

William Marsh Rice University - Houston TX

International Classification:

D01F 912

US Classification:

4234473, 4234471, 423445 R

Abstract:

The present invention discloses the process of supplying high pressure (e. g. , 30 atmospheres) CO that has been preheated (e. g. , to about 1000Â C. ) and a catalyst precursor gas (e. g. , Fe(CO) ) in CO that is kept below the catalyst precursor decomposition temperature to a mixing zone. In this mixing zone, the catalyst precursor is rapidly heated to a temperature that results in (1) precursor decomposition, (2) formation of active catalyst metal atom clusters of the appropriate size, and (3) favorable growth of SWNTs on the catalyst clusters. Preferably a catalyst cluster nucleation agency is employed to enable rapid reaction of the catalyst precursor gas to form many small, active catalyst particles instead of a few large, inactive ones. Such nucleation agencies can include auxiliary metal precursors that cluster more rapidly than the primary catalyst, or through provision of additional energy inputs (e. g. , from a pulsed or CW laser) directed precisely at the region where cluster formation is desired.

US Patent:

6790425, Sep 14, 2004

Filed:

Jul 24, 2001

Appl. No.:

09/890030

Inventors:

Richard E. Smalley - Houston TX
Daniel T. Colbert - Houston TX
Ken A. Smith - Katy TX
Deron A. Walters - Orlando FL
Michael J. Casavant - Houston TX
Chad B. Huffman - Houston TX
Boris I. Yakobson - Houston TX
Robert H. Hague - Houston TX
Rajesh Kumar Saini - Houston TX
Wan-Ting Chiang - Sugarland TX

Assignee:

Wiliam Marsh Rice University - Houston TX

International Classification:

D01F 912

US Classification:

4234471, 423445 R, 4234472

Abstract:

The present invention is directed to the creation of macroscopic materials and objects comprising aligned nanotube segments. The invention entails aligning single-wall carbon nanotube (SWNT) segments that are suspended in a fluid medium and then removing the aligned segments from suspension in a way that macroscopic, ordered assemblies of SWNT are formed. The invention is further directed to controlling the natural proclivity of nanotube segments to self assemble into ordered structures by modifying the environment of the nanotubes and the history of that environment prior to and during the process. The materials and objects are âmacroscopicâ in that they are large enough to be seen without the aid of a microscope or of the dimensions of such objects. These macroscopic, ordered SWNT materials and objects have the remarkable physical, electrical, and chemical properties that SWNT exhibit on the microscopic scale because they are comprised nanotubes, each of which is aligned in the same direction and in contact with its nearest neighbors. An ordered assembly of closest SWNT also serves as a template for growth of more and larger ordered assemblies.