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1. 发明申请

US20050160798A1 METHOD AND APPARATUS FOR DETERMINING THE LENGTH OF SINGLE-WALLED CARBON NANOTUBES 失效
标题翻译：用于确定单壁碳纳米管长度的方法和装置
公开(公告)号：US20050160798A1
公开(公告)日：2005-07-28
申请号：US10836551
申请日：2004-04-30
申请人： Matteo Pasquali , Virginia Davis , Ingrid Stepanek-Basset , A. Nicholas Parra-Vasquez , Robert Hauge
发明人： Matteo Pasquali , Virginia Davis , Ingrid Stepanek-Basset , A. Nicholas Parra-Vasquez , Robert Hauge
IPC分类号： C01B31/02 , G01B13/02 , G01N11/00 , G01N33/00
CPC分类号： B82Y30/00 , B82Y15/00 , B82Y40/00 , C01B32/15 , C01B2202/02 , C01B2202/34 , G01N11/00 , Y10S977/88
摘要： The present invention is directed to at least one method and at least one apparatus for determining the length of single-wall carbon nanotubes (SWNTs). The method generally comprises the steps of: dispersing a sample of SWNTs into a suitable dispersing medium to form a solvent-suspension of solvent-suspended SWNTs; determining the mean SWNT diameter of the solvent-suspended SWNTs; introducing the solvent-suspended SWNTs into a viscosity-measuring device; obtaining a specific viscosity for the SWNT solvent-suspension; and determining the length of the SWNTs based upon the specific viscosity by solving, for example, the Kirkwood-Auer equation corrected by Batchelor's formula for the drag on a slender cylinder for “L,” to determine the length of the SWNTs. The apparatus generally comprises: a SWNT sample introduction mechanism; a dispersal chamber; a SWNT radius-determination chamber; and a viscosity determining chamber, wherein the SWNT sample introduction mechanism, the dispersal chamber, the SWNT radius-determination chamber, and the viscosity determination chamber are each operatively connected to at least one of the others.
摘要翻译：本发明涉及用于确定单壁碳纳米管（SWNT）的长度的至少一种方法和至少一种装置。该方法通常包括以下步骤：将SWNT样品分散到合适的分散介质中以形成溶剂悬浮的SWNT的溶剂 - 悬浮液; 确定溶剂悬浮的SWNT的平均SWNT直径; 将溶剂悬浮的SWNT引入粘度测量装置中; 获得SWNT溶剂 - 悬浮液的比粘度; 以及通过解决例如通过Batchelor公式修正的Kirkwood-Auer方程式来确定SWNTs的长度，以便通过在“L”的细长圆筒上拖动来确定SWNT的长度。该装置通常包括：SWNT样品引入机构; 分散室; SWNT半径测定室; 和粘度确定室，其中SWNT样品引入机构，分散室，SWNT半径确定室和粘度确定室各自可操作地连接到至少其中之一。

2. 发明授权

US08591854B2 Methods for solubilizing and separating large fullerenes 失效
标题翻译：溶解和分离大富勒烯的方法
公开(公告)号：US08591854B2
公开(公告)日：2013-11-26
申请号：US12672605
申请日：2008-08-08
申请人： Pradeep K. Rai , A. Nicholas Parra-Vasquez , Haiqing Peng , Robert Hauge , Matteo Pasquali
发明人： Pradeep K. Rai , A. Nicholas Parra-Vasquez , Haiqing Peng , Robert Hauge , Matteo Pasquali
IPC分类号： C01B31/00 , B82Y40/00 , B82Y30/00
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。

3. 发明申请

US20110318248A1 Methods for Solubilizing and Separating Large Fullerenes 失效
标题翻译：溶解和分离大富勒烯的方法
公开(公告)号：US20110318248A1
公开(公告)日：2011-12-29
申请号：US12672605
申请日：2008-08-08
申请人： Pradeep K. Rai , A. Nicholas Parra-Vasquez , Haiqing Peng , Robert Hauge , Matteo Pasquali
发明人： Pradeep K. Rai , A. Nicholas Parra-Vasquez , Haiqing Peng , Robert Hauge , Matteo Pasquali
IPC分类号： C01B31/00 , B82Y40/00 , B82Y30/00
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。

4. 发明申请

US20110262772A1 Method for Producing Aligned Near Full Density Pure Carbon Nanotube Sheets, Ribbons, and Films From Aligned Arrays of as Grown Carbon Nanotube Carpets/Forests and Direct Transfer to Metal and Polymer Surfaces 审中-公开
标题翻译：用于生成对称的近全密度纯碳纳米管片，丝带和从作为生长碳纳米管地毯/森林的对齐阵列的膜和直接转移到金属和聚合物表面的方法
公开(公告)号：US20110262772A1
公开(公告)日：2011-10-27
申请号：US12671644
申请日：2008-07-31
申请人： Robert Hauge , Cary Pint , Ya-Qiong Xu , Matteo Pasquali
发明人： Robert Hauge , Cary Pint , Ya-Qiong Xu , Matteo Pasquali
IPC分类号： B32B19/00 , C03C25/44 , B29C67/24 , B32B37/18 , B82Y40/00
CPC分类号： D01F9/12 , B29C43/22 , B29K2105/162 , B82Y30/00 , B82Y40/00 , C01B32/162 , C01B2202/02 , C01B2202/04 , C01B2202/06 , C01B2202/08 , C08J5/005
摘要： Methods for preparing carbon nanotube layers are disclosed herein. Carbon nanotube layers may be films, ribbons, and sheets. The methods comprise preparing an aligned carbon nanotube array and compressing the array with a roller to create a carbon nanotube layer. Another method disclosed herein comprises preparing a carbon nanotube layer from an aligned carbon nanotube array grown on a grouping of lines of metallic catalyst. A composite material comprising at least one carbon nanotube layer and prepared by the process comprising a) compressing an aligned single-wall carbon nanotube array with a roller, and b) transferring the carbon nanotube layer to a polymer is also disclosed.
摘要翻译：本文公开了制备碳纳米管层的方法。碳纳米管层可以是膜，带和片。所述方法包括制备对准的碳纳米管阵列并用辊压缩阵列以产生碳纳米管层。本文公开的另一种方法包括从在一组金属催化剂上生长的排列的碳纳米管阵列制备碳纳米管层。一种复合材料，其包含至少一个碳纳米管层，并通过包括以下步骤制备的方法制备：a）用辊压缩对齐的单壁碳纳米管阵列，和b）将碳纳米管层转移到聚合物上。

5. 发明授权

US06835366B1 Chemical derivatization of single-wall carbon nanotubes to facilitate solvation thereof, and use of derivatized nanotubes 失效
标题翻译：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。

6. 发明申请

US20070196262A1 Reductive functionalization of carbon nanotubes 有权
标题翻译：碳纳米管的还原官能化
公开(公告)号：US20070196262A1
公开(公告)日：2007-08-23
申请号：US10592463
申请日：2005-03-11
申请人： Edward Billups , Anil Sadana , Feng Liang , Robert Hauge
发明人： Edward Billups , Anil Sadana , Feng Liang , Robert Hauge
IPC分类号： C01B31/02
CPC分类号： B82Y40/00 , B82Y30/00 , C01B32/05 , C01B32/152 , C01B32/174 , C01B2202/02 , C01B2202/36 , C01P2002/82 , C01P2002/88 , C01P2004/03 , C01P2004/04 , C01P2004/13
摘要： The present invention is directed to novel processes for the functionalization (derivatization) of carbon nanotubes and, as an extension, to fullerenes and other carbon surfaces. Generally, such processes involve reductive pathways. In some embodiments, carbon nanotubes are reacted with alkali metal and organic halides in anhydrous liquid ammonia. In other embodiments, polymers are grown from carbon nanotube sidewalls by reacting carbon nanotubes with alkali metal and monomer species in anhydrous liquid ammonia.
摘要翻译：本发明涉及用于碳纳米管的功能化（衍生化）和作为对富勒烯和其它碳表面的延伸的新方法。通常，这些方法涉及还原途径。在一些实施方案中，碳纳米管与碱金属和有机卤化物在无水液态氨中反应。在其它实施方案中，通过使碳纳米管与碱金属和单体物质在无水液态氨中反应，从碳纳米管侧壁生长聚合物。

7. 发明申请

US20050169830A1 Macroscopic ordered assembly of carbon nanotubes 审中-公开
标题翻译：宏观有序的碳纳米管组装
公开(公告)号：US20050169830A1
公开(公告)日：2005-08-04
申请号：US10759356
申请日：2004-01-16
申请人： Smalley Richard , Daniel Colbert , Kenneth Smith , Deron Walters , Michael Casavant , Chad Huffman , Boris Yakobson , Robert Hauge , Rajesh Saini , Wan-Ting Chiang , Xiao Qin
发明人： Smalley Richard , Daniel Colbert , Kenneth Smith , Deron Walters , Michael Casavant , Chad Huffman , Boris Yakobson , Robert Hauge , Rajesh Saini , Wan-Ting Chiang , Xiao Qin
IPC分类号： C01B31/02 , H01J1/304 , H01J9/02 , D01F9/12 , H05F3/00
CPC分类号： B82Y40/00 , B82Y10/00 , B82Y30/00 , C01B32/168 , C01B2202/02 , C01B2202/08 , H01J2201/30469 , Y10S977/75 , Y10S977/845 , Y10S977/847 , Y10T156/10
摘要： 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. 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 of 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.
摘要翻译：本发明涉及包括对准的纳米管段的宏观材料和物体的产生。本发明需要将悬浮在流体介质中的单壁碳纳米管（SWNT）段对准，然后以形成SWNT的宏观有序组件的方式从悬浮液中除去对准的段。本发明进一步涉及通过在过程之前和过程中修改纳米管的环境和该环境的历史来控制纳米管段的自然倾向自我组装成有序结构。材料和物体是“宏观的”，因为它们足够大以便在没有显微镜或这些物体的尺寸的情况下被看到。这些宏观有序的SWNT材料和物体具有显着的物理，电学和化学性质，SWNT在微观尺度上显示，因为它们由纳米管组成，其中每个纳米管沿相同方向排列并与其最近的邻近物接触。最近的SWNT的有序组件也可以作为增加更多和更大订单组件的模板。订购的组件还用作后处理处理的基础，其在内部改变组件以特异性地增强选定的材料性能，例如剪切强度，抗拉强度，抗压强度，韧性，导电性和导热性。

8. 发明授权

US06645455B2 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 有权
公开(公告)号：US06645455B2
公开(公告)日：2003-11-11
申请号：US09810201
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 , B01J35/06 , B82Y30/00 , B82Y40/00 , C01B32/162 , C01B32/174 , C01B2202/02 , C01B2202/06 , C01B2202/08 , D01F11/121 , Y10S977/745 , Y10S977/75 , Y10S977/835 , Y10S977/843 , Y10S977/848 , Y10T428/139 , Y10T428/2918
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.

9. 发明授权

US08709373B2 Strongly bound carbon nanotube arrays directly grown on substrates and methods for production thereof 有权
标题翻译：直接生长在基材上的强烈结合的碳纳米管阵列及其生产方法
公开(公告)号：US08709373B2
公开(公告)日：2014-04-29
申请号：US13139418
申请日：2009-12-11
申请人： Robert Hauge , Cary Pint , Noe Alvarez , W. Carter Kittrell
发明人： Robert Hauge , Cary Pint , Noe Alvarez , W. Carter Kittrell
IPC分类号： D01F9/12
CPC分类号： B82Y30/00 , B82Y40/00 , C01B32/15 , C01B32/162 , C01B2202/08 , H01J9/025 , H01J2201/30469
摘要： The present disclosure describes carbon nanotube arrays having carbon nanotubes grown directly on a substrate and methods for making such carbon nanotube arrays. In various embodiments, the carbon nanotubes may be covalently bonded to the substrate by nanotube carbon-substrate covalent bonds. The present carbon nanotube arrays may be grown on substrates that are not typically conducive to carbon nanotube growth by conventional carbon nanotube growth methods. For example, the carbon nanotube arrays of the present disclosure may be grown on carbon substrates including carbon foil, carbon fibers and diamond. Methods for growing carbon nanotubes include a) providing a substrate, b) depositing a catalyst layer on the substrate, c) depositing an insulating layer on the catalyst layer, and d) growing carbon nanotubes on the substrate. Various uses for the carbon nanotube arrays are contemplated herein including, for example, electronic device and polymer composite applications.
摘要翻译：本公开描述了具有直接在基底上生长的碳纳米管的碳纳米管阵列和制备这种碳纳米管阵列的方法。在各种实施方案中，碳纳米管可以通过纳米管碳 - 基质共价键共价结合到基底上。可以通过常规的碳纳米管生长方法将本发明的碳纳米管阵列生长在通常不利于碳纳米管生长的基底上。例如，本公开的碳纳米管阵列可以在包括碳箔，碳纤维和金刚石的碳基板上生长。用于生长碳纳米管的方法包括a）提供基底，b）在基底上沉积催化剂层，c）在催化剂层上沉积绝缘层，以及d）在基底上生长碳纳米管。本文考虑了碳纳米管阵列的各种用途，包括例如电子器件和聚合物复合材料应用。

10. 发明申请

US20070065975A1 Purification of carbon nanotubes based on the chemistry of fenton's reagent 有权
标题翻译：基于芬顿试剂的化学成分对碳纳米管进行纯化
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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