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1.发明申请Fibers comprised of epitaxially grown single-wall carbon nanotubes, and a method for added catalyst and continuous growth at the tip 失效由外延生长的单壁碳纳米管组成的纤维，以及在尖端处添加催化剂和连续生长的方法公开(公告)号：US20070009421A1
公开(公告)日：2007-01-11
申请号：US11291449
申请日：2005-12-01
申请人： W. Kittrell , Yuhuang Wang , Myung Kim , Robert Hauge , Richard Smalley , Irene Marek
发明人： W. Kittrell , Yuhuang Wang , Myung Kim , Robert Hauge , Richard Smalley , Irene Marek
IPC分类号： D01F9/12
CPC分类号： D01F9/127 , B82Y30/00 , Y10S977/843 , Y10S977/848
摘要： 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.
摘要翻译： 本发明涉及外延生长的单壁碳纳米管（SWNT）的纤维及其制造方法。 这样的方法通常包括以下步骤：（a）提供纺丝的SWNT纤维; （b）切割基本垂直于纤维轴线的纤维以产生切割的纤维; （c）用等离子体在其端部蚀刻切割的纤维，得到蚀刻的切割纤维; （d）将金属催化剂沉积在蚀刻的切割的纤维端上以形成连续的SWNT纤维前体; 和（e）在SWNT生长条件下引入原料气体以将连续的SWNT纤维前体生长成连续的SWNT纤维。
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2.发明申请公开(公告)号：US20070065975A1
公开(公告)日：2007-03-22
申请号：US11319707
申请日：2005-12-28
申请人： Richard Smalley , Irene Marek , Yuhuang Wang , Robert Hauge , Hongwei Shan
发明人： Richard Smalley , Irene Marek , Yuhuang Wang , Robert Hauge , Hongwei Shan
IPC分类号： H01L51/40
CPC分类号： B82Y30/00 , B82Y10/00 , B82Y40/00 , C01B32/17 , C01B2202/02 , C01B2202/04 , C01B2202/06 , C01B2202/36 , H01L51/0025 , H01L51/0048 , Y10S977/845
摘要： The present invention is directed to methods of purifying carbon nanotubes (CNTs). In general, such methods comprise the following steps: (a) preparing an aqueous slurry of impure CNT material; (b) establishing a source of Fe2+ ions in the slurry to provide a catalytic slurry; (c) adding hydrogen peroxide to the catalytic slurry to provide an oxidative slurry, wherein the Fe2+ ions catalyze the production of hydroxyl radicals; and (d) utilizing the hydroxyl radicals in the oxidative slurry to purify the CNT material and provide purified CNTs.
摘要翻译： 本发明涉及净化碳纳米管（CNTs）的方法。 通常，这些方法包括以下步骤：（a）制备不纯的CNT材料的含水浆料; （b）在浆料中建立Fe 2+ 2+离子源以提供催化浆液; （c）向催化浆料中加入过氧化氢以提供氧化浆料，其中Fe 2+ 2+催化羟基自由基的产生; 和（d）利用氧化浆液中的羟基自由基来纯化CNT材料并提供纯化的CNT。
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3.发明申请公开(公告)号：US20060201880A1
公开(公告)日：2006-09-14
申请号：US11289000
申请日：2005-11-29
申请人： Kirk Ziegler , Daniel Schmidt , Robert Hauge , Richard Smalley , Irene Marek
发明人： Kirk Ziegler , Daniel Schmidt , Robert Hauge , Richard Smalley , Irene Marek
IPC分类号： B01D15/00
CPC分类号： B82Y30/00 , B82Y10/00 , B82Y40/00 , C01B32/172 , C01B32/174 , C01B2202/02 , C01B2202/28 , Y10S977/75 , Y10S977/845 , Y10S977/847
摘要： 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.
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公开(公告)号：US20060159612A1
公开(公告)日：2006-07-20
申请号：US11285232
申请日：2005-11-22
申请人： Kirk Ziegler , Jonah Shaver , Robert Hauge , Richard Smalley , Irene Marek
发明人： Kirk Ziegler , Jonah Shaver , Robert Hauge , Richard Smalley , Irene Marek
CPC分类号： B82Y30/00 , B82Y40/00 , C01B32/174 , C01B2202/02 , D01F11/122 , Y10S977/847
摘要： The present invention is generally directed to methods of ozonating CNTs in fluorinated solvents (fluoro-solvents), wherein such methods provide a less dangerous alternative to existing ozonolysis methods. In some embodiments, such methods comprise the steps of: (a) dispersing carbon nanotubes in a fluoro-solvent to form a dispersion; and (b) reacting ozone with the carbon nanotubes in the dispersion to functionalize the sidewalls of the carbon nanotubes and yield functionalized carbon nanotubes with oxygen-containing functional moieties. In some such embodiments, the fluoro-solvent is a fluorocarbon solvent, such as a perfluorinated polyether.
摘要翻译： 本发明一般涉及在氟化溶剂（氟溶剂）中臭氧化碳纳米管的方法，其中这些方法对现有的臭氧分解方法提供了较不危险的替代方法。 在一些实施方案中，这些方法包括以下步骤：（a）将碳纳米管分散在氟溶剂中以形成分散体; 和（b）使臭氧与分散体中的碳纳米管反应，使碳纳米管的侧壁官能化，并产生具有含氧官能团的官能化碳纳米管。 在一些这样的实施方案中，氟 - 溶剂是氟烃溶剂，例如全氟化聚醚。
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公开(公告)号：US20060231399A1
公开(公告)日：2006-10-19
申请号：US11410658
申请日：2006-06-19
申请人： Richard Smalley , Robert Hauge , W. Kittrell , Ramesh Sivarajan , Michael Strano , Sergei Bachilo , R. Weisman
发明人： Richard Smalley , Robert Hauge , W. Kittrell , Ramesh Sivarajan , Michael Strano , Sergei Bachilo , R. Weisman
IPC分类号： C07K1/26
CPC分类号： G01N21/6428 , B82Y15/00 , B82Y30/00 , B82Y40/00 , C01B32/172 , C01B2202/02 , C01B2202/22 , G01N21/6489 , G01N21/65 , G01N33/574 , G01N33/588 , G01N2021/6417 , G01N2021/7786
摘要： 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. The separation enables new electronic devices requiring selected (n, m) nanotube types.
摘要翻译： 本发明涉及一种根据（n，m）型分选（n，m）型单壁碳纳米管的混合物的方法。 （n，m）型单壁碳纳米管的混合物被悬浮，使得单壁碳纳米管分散分散。 纳米管悬浮液可以在表面活性剂 - 水溶液中进行，并且包围纳米管的表面活性剂保持纳米管分离并与其他纳米管聚集。 将纳米管悬浮液酸化以质子化纳米管的一部分。 施加电场，并且质子化的纳米管在电场中以取决于它们的（n，m）类型的不同速率迁移。 在不同的分馏时间收集纳米管的级分。 在越来越高的pH下重复质子化，施加电场和分级的过程，以将（n，m）纳米管混合物分离成单个（n，m）纳米管部分。 该分离使需要所选（n，m）纳米管类型的新电子器件成为可能。
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6.发明申请Copolymerization of polybenzazoles and other aromatic polymers with carbon nanotubes 失效聚苯并唑和其他芳族聚合物与碳纳米管的共聚合公开(公告)号：US20050171281A1
公开(公告)日：2005-08-04
申请号：US10972560
申请日：2004-10-25
申请人： Wen-Fang Hwang , Richard Smalley , Robert Hauge
发明人： Wen-Fang Hwang , Richard Smalley , Robert Hauge
CPC分类号： C08J5/18 , B82Y30/00 , C08G73/18 , C08G73/22 , C08J2379/06 , D01F6/74 , D01F6/94 , Y10S977/75 , Y10S977/753 , Y10S977/783
摘要： The present invention is generally directed to the block copolymerization of rigid rod polymers with carbon nanotubes (CNTs), the CNTs generally being shortened, to form nanotube block copolymers. The present invention is also directed to fibers and other shaped articles made from the nanotube block copolymers of the present invention.
摘要翻译： 本发明一般涉及刚性棒状聚合物与碳纳米管（CNTs）的嵌段共聚合，CNT通常被缩短以形成纳米管嵌段共聚物。 本发明还涉及由本发明的纳米管嵌段共聚物制成的纤维和其它成型制品。
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公开(公告)号：US20070098621A1
公开(公告)日：2007-05-03
申请号：US11408520
申请日：2006-06-13
申请人： John Margrave , Edward Mickelson , Robert Hauge , Peter Boul , Chad Huffman , Jie Liu , Richard Smalley
发明人： John Margrave , Edward Mickelson , Robert Hauge , Peter Boul , Chad Huffman , Jie Liu , Richard Smalley
IPC分类号： D01F9/12
CPC分类号： B01J21/18 , B01J23/74 , B01J23/755 , B01J35/006 , B01J35/06 , B82Y30/00 , B82Y40/00 , C01B32/174 , C01B2202/02 , C01B2202/06 , D01F11/121 , Y10S977/74 , Y10S977/748 , Y10S977/75 , Y10S977/843 , Y10S977/848
摘要： 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.
摘要翻译： 本发明涉及制备碳纳米管的化学衍生物和衍生纳米管的用途，包括制备阵列作为碳纤维合成的基础。 在一个实施方案中，本发明还提供了通过使单壁碳纳米管与氟气反应并回收氟衍生的碳纳米管，制备具有连接到纳米管侧壁上的取代基的单壁碳纳米管的方法，然后使氟衍生的碳纳米管与 亲核试剂 一些氟取代基被亲核取代取代。 如果需要，可以完全或部分地除去剩余的氟以产生具有连接到纳米管的侧壁上的取代基的单壁碳纳米管。 取代基当然取决于亲核试剂，优选的亲核试剂包括烷基锂物质如甲基锂。 或者，可以通过使氟衍生的碳纳米管与各种量的肼，取代的肼或烷基胺反应，从氟衍生的碳纳米管中完全或部分地除去氟。 本发明还提供用于生长单壁碳纳米管的种子材料，其包含多个单壁碳纳米管或具有在侧壁的外表面上共价结合或物理吸附的催化剂前体部分的短管状分子，以提供最佳金属簇尺寸 导致金属部分迁移到管端的条件。
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公开(公告)号：US08591854B2
公开(公告)日：2013-11-26
申请号：US12672605
申请日：2008-08-08
CPC分类号： B82Y40/00 , B82Y30/00 , C01B32/15 , C01B32/152
摘要： We have discovered that size dependent solubility of large fullerenes in strong acids is dependent on acid strength. This provides a scalable method for separating large fullerenes by size. According to some embodiments, a method for processing a fullerene starting material comprises large fullerenes comprises mixing the starting material with a first concentrated sulfuric acid solution so as to obtain a first dispersion comprising a first portion of the large fullerenes solubilized in the first concentrated sulfuric acid solution.
摘要翻译： 我们已经发现大富勒烯在强酸中的尺寸依赖性溶解度取决于酸强度。 这提供了一种用于按大小分离大富勒烯的可扩展方法。 根据一些实施方案，用于处理富勒烯起始材料的方法包括大的富勒烯，包括将起始材料与第一浓硫酸溶液混合，以获得第一分散体，其包含溶解在第一浓硫酸中的第一部分富勒烯 解。
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公开(公告)号：US20110318248A1
公开(公告)日：2011-12-29
申请号：US12672605
申请日：2008-08-08
CPC分类号： B82Y40/00 , B82Y30/00 , C01B32/15 , C01B32/152
摘要： We have discovered that size dependent solubility of large fullerenes in strong acids is dependent on acid strength. This provides a scalable method for separating large fullerenes by size. According to some embodiments, a method for processing a fullerene starting material comprises large fullerenes comprises mixing the starting material with a first concentrated sulfuric acid solution so as to obtain a first dispersion comprising a first portion of the large fullerenes solubilized in the first concentrated sulfuric acid solution.
摘要翻译： 我们已经发现大富勒烯在强酸中的尺寸依赖性溶解度取决于酸强度。 这提供了一种用于按大小分离大富勒烯的可扩展方法。 根据一些实施方案，用于处理富勒烯起始材料的方法包括大的富勒烯，包括将起始材料与第一浓硫酸溶液混合，以获得第一分散体，其包含溶解在第一浓硫酸中的第一部分富勒烯 解。
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10.发明授权Chemical derivatization of single-wall carbon nanotubes to facilitate solvation thereof, and use of derivatized nanotubes 失效单壁碳纳米管的化学衍生化以促进其溶剂化，以及衍生的纳米管的使用公开(公告)号：US06835366B1
公开(公告)日：2004-12-28
申请号：US09787473
申请日：2001-03-16
申请人： John L. Margrave , Edward T. Mickelson , Robert Hauge , Peter Boul , Chad Huffman , Jie Liu , Richard E. Smalley , Ken Smith , Daniel T. Colbert
发明人： John L. Margrave , Edward T. Mickelson , Robert Hauge , Peter Boul , Chad Huffman , Jie Liu , Richard E. Smalley , Ken Smith , Daniel T. Colbert
IPC分类号： D01F912
CPC分类号： B01J21/18 , B01J23/74 , B01J23/755 , B01J35/006 , B01J35/06 , B82Y30/00 , B82Y40/00 , C01B32/174 , C01B2202/02 , C01B2202/06 , D01F11/121 , Y10S977/74 , Y10S977/748 , Y10S977/75 , Y10S977/843 , Y10S977/848
摘要： 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.
摘要翻译： 本发明涉及制备碳纳米管的化学衍生物和衍生纳米管的用途，包括制备阵列作为碳纤维合成的基础。 在一个实施方案中，本发明还提供了通过使单壁碳纳米管与氟气反应并回收氟衍生的碳纳米管，制备具有连接到纳米管侧壁上的取代基的单壁碳纳米管的方法，然后使氟衍生的碳纳米管与 亲核试剂 一些氟取代基被亲核取代取代。 如果需要，可以完全或部分地除去剩余的氟以产生具有连接到纳米管的侧壁上的取代基的单壁碳纳米管。 取代基当然取决于亲核试剂，优选的亲核试剂包括烷基锂物质如甲基锂。 或者，可以通过使氟衍生的碳纳米管与各种量的肼，取代的肼或烷基胺反应，从氟衍生的碳纳米管中完全或部分地除去氟。 本发明还提供用于生长单壁碳纳米管的种子材料，其包含多个单壁碳纳米管或具有在侧壁的外表面上共价结合或物理吸附的催化剂前体部分的短管状分子，以提供最佳金属簇尺寸 导致金属部分迁移到管端的条件。
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