Abstract: This invention relates generally to a method for producing single-wall carbon nanotube (SWNT) catalyst supports and compositions thereof. In one embodiment, SWNTs or SWNT structures can be employed as the support material. A transition metal catalyst is added to the SWNT. In a preferred embodiment, the catalyst metal cluster is deposited on the open nanotube end by a docking process that insures optimum location for the subsequent growth reaction. The metal atoms may be subjected to reductive conditions.

Abstract: The 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.

Abstract: The present invention relates to new compositions of matter and articles of manufacture comprising SWNTs as nanometer scale conducting rods dispersed in an electrically-insulating matrix. These compositions of matter have novel and useful electrical, mechanical, and chemical properties including applications in antennas, electromagnetic and electro-optic devices, and high-toughness materials. Other compositions of matter and articles of manufacture are disclosed including polymer-coated and polymer wrapped single-wall nanotubes (SWNTs), small ropes of polymer-coated and polymer-wrapped SWNTs and materials comprising same. This composition provides one embodiment of the SWNT conducting-rod composite mentioned above, and also enables creation of high-concentration suspensions of SWNTs and compatibilization of SWNTs with polymeric matrices in composite materials.

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 “macroscopic” in that they are large enough to be seen without the aid of a microscope or of the dimensions of such objects.

Abstract: The 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.

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.

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.

Abstract: The present invention relates to a 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 employs steps including a gas-phase oxidation of the amorphous carbon and subsequent liquid-phase reaction of a halogen-containing acid with the metal-containing species. Optionally, the single-wall carbon nanotube material may be annealed dry or in the presence of moisture.

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 106 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 500° C. to about 1300° C. The growing carbon fiber is continuously recovered.

Abstract: The invention relates to a process for sorting and separating a mixture of (n, m) type single-wall carbon nanotubes according to (n, m) type. A mixture of (n, m) type single-wall carbon nanotubes is suspended such that the single-wall carbon nanotubes are individually dispersed. The nanotube suspension can be done in a surfactant-water solution and the surfactant surrounding the nanotubes keeps the nanotube isolated and from aggregating with other nanotubes. The nanotube suspension is acidified to protonate a fraction of the nanotubes. An electric field is applied and the protonated nanotubes migrate in the electric fields at different rates dependent on their (n, m) type. Fractions of nanotubes are collected at different fractionation times. The process of protonation, applying an electric field, and fractionation is repeated at increasingly higher pH to separated the (n, m) nanotube mixture into individual (n, m) nanotube fractions.

Abstract: The invention relates to macroscopic amounts of (n, m) type single-wall carbon nanotubes and sensing and monitoring devices comprising specific nanotube types. Selected (n, m)-type fractions of single-wall carbon nanotubes are separated from a suspension of mixed single-wall carbon nanotubes are individually dispersed and isolated. The nanotubes are isolated and precluded from reassociating with other nanotubes by encasing the nanotube with a non-perturbing molecular species, such as surfactant molecules or polymers that can wrap around the nanotube. In contrast to metallic single-wall carbon nanotubes, semiconducting single-wall carbon nanotubes have been found to fluoresce in the near-IR region of the electromagnetic spectrum. The nanotubes are very sensitive to environmental perturbations and the nanotube's fluorescence profile will be affected by these perturbations.

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.

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.

Abstract: A method for cutting single-wall carbon nanotubes involves partially fluorinating single-wall carbon nanotubes and pyrolyzing the partially fluorinated nanotubes in an inert atmosphere or vacuum up to about 1000° C. The nanotubes are optionally purified before cutting. The partial fluorination involves fluorinating the nanotubes to a carbon-fluorine stoichiometry of CFx, where x is up to about 0.3. The invention also relates to the derivatization of fluorinated and cut single-wall carbon nanotubes. The single-wall carbon nanotubes can be cut to any length depending on the fluorination and pyrolysis conditions. Short nanotubes are useful in various applications, such as field emitters for flat panel displays and as “seeds” for further nanotube growth.

Abstract: Buckyrock is a three-dimensional, solid block material comprising an entangled network of single-wall carbon nanotubes (SWNT), wherein the block comprises greater than 75 wt % SWNT. SWNT buckyrock is mechanically strong, tough and impact resistant. The single-wall carbon nanotubes in buckyrock form are present in a random network of individual single-wall carbon nanotubes, SWNT “ropes” and combinations thereof. The random network of the SWNT or SWNT ropes can be held in place by non-covalent “cross-links” between the nanotubes at nanotube contact points. In one embodiment, SWNT buckyrock is made by forming a SWNT-water slurry, slowly removing water from the slurry which results in a SWNT-water paste, and allowing the paste to dry very slowly, such that the SWNT network of the SWNT-water paste is preserved during solvent evaporation.

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.

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.

Abstract: The present invention involves fibers of highly aligned single-wall carbon nanotubes and a process for making the same. The present invention provides a method for effectively dispersing single-wall carbon nanotubes. The process for dispersing the single-wall carbon nanotubes comprises mixing single-wall carbon nanotubes with 100% sulfuric acid or a superacid, heating and stirring under an inert, oxygen-free environment. The single-wall carbon nanotube/acid mixture is wet spun into a coagulant to form the single-wall carbon nanotube fibers. The fibers are recovered, washed and dried. The single-wall carbon nanotubes were highly aligned in the fibers, as determined by Raman spectroscopy analysis.

Abstract: A continuous gas-phase method for producing single-wall carbon nanotubes at high catalyst productivity and high yield is disclosed. The method involves the use of a novel in-situ formed catalyst to initiate and grow single-wall carbon nanotubes using a carbon-containing feedstock in a high temperature and pressure process. The catalyst comprises in-situ-generated transition metal particles in contact with in-situ-generated refractory particles. The population of nucleating sites for single-wall carbon nanotubes is enhanced due to the ease of formation of a population of refractory particles. These, in turn, improve the nucleation and stability of the transition metal particles that grow on them. The larger number of transition metal particles translate into a larger number of sites for single-wall carbon nanotube production. The higher catalyst yields provide a means for obtaining higher purity single-wall carbon nanotubes.

Abstract: The present invention involves alewives of highly aligned single-wall carbon nanotubes (SWNT), process for making the same and compositions thereof. The present invention provides a method for effectively making carbon alewives, which are discrete, acicular-shaped aggregates of aligned single-wall carbon nanotubes and resemble the Atlantic fish of the same name. Single-wall carbon nanotube alewives can be conveniently dispersed in materials such as polymers, ceramics, metals, metal oxides and liquids. The process for preparing the alewives comprises mixing single-wall carbon nanotubes with 100% sulfuric acid or a superacid, heating and stirring, and slowly introducing water into the single-wall carbon nanotube/acid mixture to form the alewives. The alewives can be recovered, washed and dried. The properties of the single-wall carbon nanotubes are retained in the alewives.