William Marsh Rice University

Other

Richard E Smalley

Daniel T Colbert

Andrew Gabriel Rinzler

Jason H Hafner

Jie Liu

Pavel Nikolaev

Andreas Thess

Ting Guo

Hongjie Dai

Ken A Smith

Robert H Hauge

Kenneth A Smith

Chad Huffman

Peter James Boul

John L Margrave

Edward T Mickelson

W Carter Kittrell

Ramesh Sivarajan

James Mitchell Tour

Rajesh Kumar Saini

Michael S Strano

Zhenning Gu

Christopher A Dyke

Irene Morin Marek, Legal Representative

Wan-Ting Chiang

Howard K Schmidt

Monica Usrey

Matteo Pasquali

Paul Walter Barone

Kirk Jeremy Ziegler

Robert Kelley Bradley

Boris I Yakobson

Peter Willis

Virginia Angelica Davis

Lars Martin Ericson

Michael O'Connell

Michael J Bronikowski

Frank Rohmund

Andrew Ross Barron

Michael P Stewart

Haiqing Peng

Elizabeth Whitsitt

Satish Kumar

Wen-Fang Hwang

Ramon Colorado, Jr

Mary Lou Margrave, Legal Representative

Yuhuang Wang

Yuemei Yang

Myung Jong Kim

Sergei M Bachilo

Ya-Qiong Xu

Kenneth L Smith

R Bruce Weisman

W Edward Billups

Sreekumar Thaliyil Veedu

Valerie C Moore

Robin E Anderson

Robert E Haufler

Honglie Dai

Irene Marie Marek, Legal Representative

Daniel J Schmidt

Pavel V Avramov

Wilber Carter Kittrell

Robert H Hague

Douglas C Ogrin

Deron A Walters

Urs Rauwald

Michael J Casavant

Chad B Huffman

Robert H Rice Univers Mailstop Chem Ms60 Hauge

Xiao Chuan Qin

Boris I Rice Univ Mech Eng & Mat Sci Yakobson

The present invention is directed towards methods (processes) of providing large quantities of carbon nanotubes (CNTs) of defined diameter and chirality (i.e., precise populations). In such processes, CNT seeds of a pre-selected diameter and chirality are grown to many (e.g., hundreds) times their original length. This is optionally followed by cycling some of the newly grown material back as seed material for regrowth. Thus, the present invention provides for the large-scale production of precise populations of CNTs, the precise composition of such populations capable of being optimized for a particular application (e.g., hydrogen storage). The present invention is also directed to complexes of CNTs and transition metal catalyst precurors, such complexes typically being formed en route to forming CNT seeds.

Amplification of carbon nanotubes via seeded-growth methods

According to some embodiments, the present invention provides a method for attaining short carbon nanotubes utilizing electron beam irradiation, for example, of a carbon nanotube sample. The sample may be pretreated, for example by oxonation. The pretreatment may introduce defects to the sidewalls of the nanotubes. The method is shown to produces nanotubes with a distribution of lengths, with the majority of lengths shorter than 100 tun. Further, the median length of the nanotubes is between about 20 nm and about 100 nm.

Bulk cutting of carbon nanotubes using electron beam irradiation

This 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.

Macroscopically manipulable nanoscale devices made from nanotube assemblies

The formation of arrays of fullerene nanotubes is described. A microscopic molecular array of fullerene nanotubes is formed by assembling subarrays of up to 10fullerene nanotubes into a composite array.

Method for forming composites of sub-arrays of fullerene nanotubes

The present invention is directed toward methods of selectively functionalizing carbon nanotubes of a specific type or range of types, based on their electronic properties, using diazonium chemistry. The present invention is also directed toward methods of separating carbon nanotubes into populations of specific types or range(s) of types via selective functionalization and electrophoresis, and also to the novel compositions generated by such separations.

Methods for selective functionalization and separation of carbon nanotubes

This invention is directed to chemical derivatives of carbon nanotubes wherein the carbon nanotubes have a diameter up to 3 nm. In one embodiment, this invention also provides a method for preparing 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 carbon nanotubes having substituents attached to the side wall of the nanotube. The substituents are dependent on the nucleophile, and preferred nucleophiles include alkyl lithium species such as methyl lithium.

Sidewall derivatized carbon nanotubes

The present invention is directed to fibers of epitaxially grown single-wall carbon nanotubes (SWNTs) and methods of making same. Such methods generally comprise the steps of: (a) providing a spun SWNT fiber; (b) cutting the fiber substantially perpendicular to the fiber axis to yield a cut fiber; (c) etching the cut fiber at its end with a plasma to yield an etched cut fiber; (d) depositing metal catalyst on the etched cut fiber end to form a continuous SWNT fiber precursor; and (e) introducing feedstock gases under SWNT growth conditions to grow the continuous SWNT fiber precursor into a continuous SWNT fiber.

Fibers comprised of epitaxially grown single-wall carbon nanotubes, and a method for added catalyst and continuous growth at the tip

The present invention relates to processes for the purification of single-wall carbon nanotubes (SWNTs). 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 side of the single-wall carbon nanotubes. The present purification processes remove the extraneous carbon as well as metal-containing residual catalyst particles.

Multi-step purification of single-wall carbon nanotubes

This 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 10fullerene nanotubes in generally parallel orientation.

Continuous fiber of fullerene nanotubes

This invention relates generally to forming an array of fullerene nanotubes. In one embodiment, a macroscopic molecular array is provided comprising at least about 10fullerene nanotubes in generally parallel orientation and having substantially similar lengths in the range of from about 5 to about 500 nanometers.

Array of fullerene nanotubes

The present invention is generally directed to new liquid-liquid extraction methods for the length-based separation of carbon nanotubes (CNTs) and other 1-dimensional nanostructures. In some embodiments, such methods are directed to separating SWNTs on the basis of their length, wherein such methods comprise the steps of: (a) functionalizing SWNTs to form functionalized SWNTs with ionizable functional moieties; (b) dissolving said functionalized SWNTs in a polar solvent to form a polar phase; (c) dissolving a substoichiometric (relative to the amount of ionizable functional moieties present on the SWNTs) amount of a phase transfer agent in a non-polar solvent to form a non-polar phase; (d) combining the polar and non-polar phases to form a bi-phase mixture; (e) adding a cationic donor species to the bi-phase mixture; and (f) agitating the bi-phase mixture to effect the preferential transport of short SWNTs into the non-polar phase such that the non-polar phase is enriched in short SWNTs and the polar phase is enriched in longer SWNTs. In other embodiments, analogous methods are used for the length-based separation of any type of CNT, and more generally, for any type of 1-dimensional nanostructure.

Length-based liquid-liquid extraction of carbon nanotubes using a phase transfer catalyst

Selective functionalization of carbon nanotubes

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. 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.

Functionalized single-wall carbon nanotubes

This invention relates generally to forming a patterned array of fullerene nanotubes. In one embodiment, a nanoscale array of microwells is provided on a substrate; a metal catalyst is deposited in each microwells; and a stream of hydrocarbon or CO feedstock gas is directed at the substrate under conditions that effect growth of fullerene nanotubes from each microwell.

Method for forming a patterned array of fullerene nanotubes

This invention relates generally to cutting fullerene nanotubes. In one embodiment, the present invention provides for preparation of homogeneous populations of short fullerene nanotubes 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 fullerene nanotubes. In one embodiment, oxidative etching with concentrated nitric acid is employed to cut fullerene nanotubes 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.

Method for cutting fullerene nanotubes

Growing community of inventors

Houston, TX, United States of America

Richard E Smalley