Browsing by Author "Smith, Kenneth A."
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Item Array of fullerene nanotubes(2009-12-15) Smalley, Richard E.; Colbert, Daniel T.; Dai, Hongjie; Liu, Jie; Rinzler, Andrew G.; Hafner, Jason H.; Smith, Kenneth A.; Guo, Ting; Nikolaev, Pavel; Thess, Andreas; Rice University; United States Patent and Trademark OfficeThis invention relates generally to forming an array of fullerene nanotubes. In one embodiment, a macroscopic molecular array is provided comprising at least about 106 fullerene nanotubes in generally parallel orientation and having substantially similar lengths in the range of from about 5 to about 500 nanometers.Item Array of single-wall carbon nanotubes(2006-07-04) Smalley, Richard E.; Colbert, Daniel T.; Dai, Hongjie; Liu, Jie; Rinzler, Andrew G.; Hafner, Jason H.; Smith, Kenneth A.; Guo, Ting; Nikolaev, Pavel; Thess, Andreas; Rice University; United States Patent and Trademark OfficeThis invention relates generally to forming an array of single-wall carbon nanotubes (SWNT). In one embodiment, a macroscopic molecular array is provided comprising at least about 106 single-wall carbon nanotubes in generally parallel orientation and having substantially similar lengths in the range of from about 5 to about 500 nanometers.Item Carbon fibers formed from single-wall carbon nanotubes(2004-01-27) Smalley, Richard E.; Colbert, Daniel T.; Dai, Hongjie; Liu, Jie; Rinzler, Andrew G.; Hafner, Jason H.; Smith, Kenneth A.; Guo, Ting; Nikolaev, Pavel; Thess, Andreas; Rice University; United States Patent and Trademark OfficeA 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.Item Catalytic growth of single- and double-wall carbon nanotubes from metal particles(2006-10-24) Smalley, Richard E.; Hafner, Jason H.; Colbert, Daniel T.; Smith, Kenneth A.; Rice University; United States Patent and Trademark OfficeSingle-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.Item Catalytic growth of single-and double-wall carbon nanotubes from metal particles(2007-04-10) Smalley, Richard E.; Hafner, Jason H.; Colbert, Daniel T.; Smith, Kenneth A.; Rice University; United States Patent and Trademark OfficeThe present invention concerns a method for growing carbon nanotubes using a catalyst system that preferentially promotes the growth of single- and double-wall carbon nanotubes, rather than larger multi-walled carbon nanotubes. Ropes of the carbon nanotubes are formed that comprise single-wall and/or double-wall carbon nanotubes.Item Catalytic growth of single-wall carbon nanotubes from metal particles(2004-02-17) Smalley, Richard E.; Hafner, Jason H.; Colbert, Daniel T.; Smith, Kenneth A.; Rice University; United States Patent and Trademark OfficeSingle-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.Item Chemical derivatization of single-wall carbon nanotubes to facilitate solvation thereof- and use of derivatized nanotubes(2004-12-28) Margrave, John L.; Mickelson, Edward T.; Hauge, Robert H.; Boul, Peter; Huffman, Chad; Liu, Jie; Smalley, Richard E.; Smith, Kenneth A.; Colbert, Daniel T.; Rice University; United States Patent and Trademark OfficeThis 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. The present invention also provides seed materials for growth of single wall carbon nanotubes comprising a plurality of single wall carbon nanotubes or short tubular molecules having a catalyst precursor moiety covalently bound or physisorbed on the outer surface of the sidewall to provide the optimum metal cluster size under conditions that result in migration of the metal moiety to the tube end.Item Chemical derivatization of single-wall carbon nanotubes to facilitate solvation thereof; and use of derivatized nanotubes to form catalyst-containing seed materials for use in making carbon fibers(2003-11-11) Margrave, John L.; Mickelson, Edward T.; Hauge, Robert H.; Boul, Peter; Huffman, Chad; Liu, Jie; Smalley, Richard E.; Smith, Kenneth A.; Colbert, Daniel T.; Rice University; United States Patent and Trademark OfficeThis 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. The present invention also provides seed materials for growth of single wall carbon nanotubes comprising a plurality of single wall carbon nanotubes or short tubular molecules having a catalyst precursor moiety covalently bound or physisorbed on the outer surface of the sidewall to provide the optimum metal cluster size under conditions that result in migration of the metal moiety to the tube end.Item Chemically modifying single wall carbon nanotubes to facilitate dispersal in solvents(2005-04-05) Margrave, John L.; Mickelson, Edward T.; Hauge, Robert H.; Boul, Peter; Huffman, Chad; Liu, Jie; Smalley, Richard E.; Smith, Kenneth A.; Colbert, Daniel T.; Rice University; United States Patent and Trademark OfficeThis 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. The present invention also provides seed materials for growth of single wall carbon nanotubes comprising a plurality of single wall carbon nanotubes or short tubular molecules having a catalyst precursor moiety covalently bound or physisorbed on the outer surface of the sidewall to provide the optimum metal cluster size under conditions that result in migration of the metal moiety to the tube end.Item Continuous fiber of fullerene nanotubes(2010-02-02) Smalley, Richard E.; Colbert, Daniel T.; Dai, Hongjie; Liu, Jie; Rinzler, Andrew G.; Hafner, Jason H.; Smith, Kenneth A.; Guo, Ting; Nikolaev, Pavel; Thess, Andreas; Rice University; United States Patent and Trademark OfficeThis invention relates generally to carbon fiber produced from fullerene nanotube arrays. In one embodiment, the present invention involves a macroscopic carbon fiber comprising at least 106 fullerene nanotubes in generally parallel orientation.Item Continuous fiber of single-wall carbon nanotubes(2005-12-27) Smalley, Richard E.; Colbert, Daniel T.; Dai, Hongjie; Liu, Jie; Rinzler, Andrew G.; Hafner, Jason H.; Smith, Kenneth A.; Guo, Ting; Nikolaev, Pavel; Thess, Andreas; Rice University; United States Patent and Trademark OfficeThis invention relates generally to carbon fiber produced from single-wall carbon nanotube (SWNT) molecular arrays. In one embodiment, the present invention involves a macroscopic carbon fiber comprising at least 106 signal-wall carbon nanotubes in generally parallel orientation.Item Dispersions and solutions of fluorinated single-wall carbon nanotubes(2004-12-07) Margrave, John L.; Mickelson, Edward T.; Hauge, Robert H.; Boul, Peter; Huffman, Chad; Liu, Jie; Smalley, Richard E.; Smith, Kenneth A.; Colbert, Daniel T.; Rice University; United States Patent and Trademark OfficeThis 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. The present invention also provides seed materials for growth of single wall carbon nanotubes comprising a plurality of single wall carbon nanotubes or short tubular molecules having a catalyst precursor moiety covalently bound or physisorbed on the outer surface of the sidewall to provide the optimum metal cluster size under conditions that result in migration of the metal moiety to the tube end.Item Fullerene nanotube compositions(2008-06-24) Smalley, Richard E.; Colbert, Daniel T.; Dai, Hongjie; Liu, Jie; Rinzler, Andrew G.; Hafner, Jason H.; Smith, Kenneth A.; Guo, Ting; Nikolaev, Pavel; Thess, Andreas; Rice University; United States Patent and Trademark OfficeThis invention relates generally to a fullerene nanotube composition. The fullerene nanotubes may be in the form of a felt, such as a bucky paper. Optionally, the fullerene nanotubes may be derivatized with one or more functional groups. Devices employing the fullerene nanotubes of this invention are also disclosed.Item Functionalized single-wall carbon nanotubes(2009-05-05) Margrave, John L.; Mickelson, Edward T.; Hauge, Robert H.; Boul, Peter; Huffman, Chad; Liu, Jie; Smalley, Richard E.; Smith, Kenneth A.; Colbert, Daniel T.; Rice University; United States Patent and Trademark OfficeThis 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. The present invention also provides seed materials for growth of single wall carbon nanotubes comprising a plurality of single wall carbon nanotubes or short tubular molecules having a catalyst precursor moiety covalently bound or physisorbed on the outer surface of the sidewall to provide the optimum metal cluster size under conditions that result in migration of the metal moiety to the tube end.Item Gas-phase nucleation and growth of single-wall carbon nanotubes from high pressure CO(2004-07-13) Smalley, Richard E.; Smith, Kenneth A.; Colbert, Daniel T.; Nikolaev, Pavel; Bronikowski, Michael J.; Bradley, Robert K.; Rohmund, Frank; Rice University; United States Patent and Trademark OfficeThe present invention discloses the process of supplying high pressure (e.g., 30 atmospheres) CO that has been preheated (e.g., to about 1000° C.) and a catalyst precursor gas (e.g., Fe(CO)5) 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. Under these conditions SWNTs nucleate and grow according to the Boudouard reaction. The SWNTs thus formed may be recovered directly or passed through a growth and annealing zone maintained at an elevated temperature (e.g., 1000° C.) in which tubes may continue to grow and coalesce into ropes.Item Gas-phase process for purifying single-wall carbon nanotubes and compositions thereof(2006-08-15) Smalley, Richard E.; Hauge, Robert H.; Chiang, Wan-Ting; Yang, Yuemei; Smith, Kenneth A.; Kittrell, Carter W.; Gu, Zhenning; Rice University; United States Patent and Trademark OfficeThe present invention relates to an all gas-phase process for the purification of single-wall carbon nanotubes and the purified single-wall carbon nanotube material. Known methods of single-wall carbon nanotube production result in a single-wall carbon nanotube product that contains single-wall carbon nanotubes in addition to impurities including residual metal catalyst particles and amounts of small amorphous carbon sheets that surround the catalyst particles and appear on the sides of the single-wall carbon nanotubes and “ropes” of single-wall carbon nanotubes. The purification process removes the extraneous carbon as well as metal-containing residual catalyst particles. The process comprises oxidation of the single-wall carbon nanotube material, reduction and reaction of a halogen-containing gas with the metal-containing species. The oxidation step may be done dry or in the presence of water vapor. The present invention provides a scalable means for producing high-purity single-wall carbon nanotube material.Item Macroscopic ordered assembly of carbon nanotubes(2004-09-14) Smalley, Richard E.; Colbert, Daniel T.; Smith, Kenneth A.; Walters, Deron A.; Casavant, Michael J.; Huffman, Chad; Yakobson, Boris I.; Hauge, Robert H.; Saini, Rajesh Kumar; Chiang, Wan-Ting; Rice University; United States Patent and Trademark OfficeThe 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 “macroscopic” 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. An ordered assembly further serves as a foundation for post processing treatments that modify the assembly internally to specifically enhance selected material properties such as shear strength, tensile strength, compressive strength, toughness, electrical conductivity, and thermal conductivity.Item Macroscopically manipulable nanoscale devices made from nanotube assemblies(2006-05-23) Colbert, Daniel T.; Dai, Hongjie; Hafner, Jason H.; Rinzler, Andrew G.; Smalley, Richard E.; Liu, Jie; Smith, Kenneth A.; Guo, Ting; Nikolaev, Pavel; Thess, Andreas; Rice University; United States Patent and Trademark OfficeMacroscopically manipulable nanoscale devices made from nanotube assemblies are disclosed. The article of manufacture comprises a macroscopic mounting element capable of being manipulated or observed in a macroscale environment, and a nanoscale nanotube assembly attached to the mounting element. The article permits macroscale information to be provided to or obtained from a nanoscale environment. A method for making a macroscopically manipulable nanoscale devices comprises the steps of (1) providing a nanotube-containing material; (2) preparing a nanotube assembly device having at least one carbon nanotube for attachment; and (3) attaching said nanotube assembly to a surface of a mounting element.Item Macroscopically manipulable nanoscale devices made from nanotube assemblies(2011-06-14) Colbert, Daniel T.; Dai, Hongjie; Hafner, Jason H.; Rinzler, Andrew G.; Smalley, Richard E.; Liu, Jie; Smith, Kenneth A.; Guo, Ting; Nikolaev, Pavel; Thess, Andreas; Rice University; United States Patent and Trademark OfficeThis invention relates generally to cutting single-wall carbon nanotubes (SWNT). In one embodiment, the present invention provides for preparations of homogeneous populations of short carbon nanotube molecules by cutting and annealing (reclosing) the nanotube pieces followed by fractionation. The cutting and annealing processes may be carried out on a purified nanotube bucky paper, on felts prior to purification of nanotubes or on any material that contains single-wall nanotubes. In one embodiment, oxidative etching with concentrated nitric acid is employed to cut SWNTs into shorter lengths. The annealed nanotubes may be disbursed in an aqueous detergent solution or an organic solvent for the fractionation. Closed tubes can also be derivatized to facilitate fractionation, for example, by adding solubilizing moieties to the end caps.Item Membrane comprising an array of single-wall carbon nanotubes(2007-04-17) Smalley, Richard E.; Colbert, Daniel T.; Dai, Hongjie; Liu, Jie; Rinzler, Andrew G.; Hafner, Jason H.; Smith, Kenneth A.; Guo, Ting; Nikolaev, Pavel; Thess, Andreas; Rice University; United States Patent and Trademark OfficeThis invention relates generally to membranes comprising an array of single-wall carbon nanotubes (SWNT) wherein the membrane is nanoporous. In one embodiment, the membrane comprises a substantially two-dimensional array of a homogeneous population of single-walled nanotubes aggregated in substantially parallel orientation to form a monolayer extending in directions substantially perpendicular to the orientation of the individual nanotubes. Using single-wall carbon nanotubes of the same type and structure provides a homogeneous array. By using different single-wall carbon nanotubes, either a random or ordered heterogeneous structure can be produced by employing successive reactions after removal of previously masked areas of a substrate. Other embodiments of the invention include batteries comprising a membrane comprising an array of single-wall carbon nanotubes or carbon fibers that are aggregates of single-wall carbon nanotubes, and wherein the plurality of single-wall carbon nanotubes are in a generally parallel orientation.
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