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    MULTI-STEP PURIFICATION OF SINGLE-WALL CARBON NANOTUBES
    3.
    发明申请
    MULTI-STEP PURIFICATION OF SINGLE-WALL CARBON NANOTUBES 有权
    单壁碳纳米管的多步纯化

    公开(公告)号：US20100008843A1

    公开(公告)日：2010-01-14

    申请号：US11291638

    申请日：2005-11-30

    申请人： Robert H. Hauge ,  Ya-Qiong Xu ,  Haiqing Peng ,  Richard E. Smalley ,  Irene Morin Marek

    发明人： Robert H. Hauge ,  Ya-Qiong Xu ,  Haiqing Peng ,  Richard E. Smalley ,  Irene Morin Marek

    IPC分类号： D01F9/12 ,  B82B3/00

    CPC分类号： B82Y30/00 ,  B82Y40/00 ,  C01B32/17 ,  C01B2202/02 ,  C01B2202/36 ,  Y10S977/845

    摘要： 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.

    摘要翻译： 本发明涉及单壁碳纳米管（SWNT）的纯化方法。 单壁碳纳米管生产的已知方法导致单壁碳纳米管产物，除了包含残留金属催化剂颗粒的杂质和围绕催化剂颗粒的小的无定形碳片的含量之外，还包含单壁碳纳米管，并出现在 侧壁的单壁碳纳米管。 本纯化方法除去了外来的碳以及含金属的残留催化剂颗粒。

    Length-based liquid-liquid extraction of carbon nanotubes using a phase transfer catalyst
    4.
    发明授权
    Length-based liquid-liquid extraction of carbon nanotubes using a phase transfer catalyst 失效
    使用相转移催化剂的基于长度的液 - 液萃取碳纳米管

    公开(公告)号：US07578941B2

    公开(公告)日：2009-08-25

    申请号：US11289000

    申请日：2005-11-29

    申请人： Kirk J. Ziegler ,  Daniel J. Schmidt ,  Robert H. Hauge ,  Richard E. Smalley ,  Irene Morin Marek, legal representative

    发明人： Kirk J. Ziegler ,  Daniel J. Schmidt ,  Robert H. Hauge ,  Richard E. Smalley

    IPC分类号： B01D11/02

    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.

    摘要翻译： 本发明一般涉及用于碳纳米管（CNT）和其它一维纳米结构的基于长度的分离的新的液 - 液萃取方法。 在一些实施方案中，这样的方法涉及基于其长度分离SWNT，其中此类方法包括以下步骤：（a）使SWNT官能化形成具有可离子化功能部分的官能化SWNT; （b）将所述官能化的单壁碳纳米管溶解在极性溶剂中以形成极性相; （c）在非极性溶剂中将相转移剂的亚化学计量（相对于存在于SWNT上的可离子化官能团的量）量溶解以形成非极性相; （d）组合极性和非极性相以形成双相混合物; （e）向双相混合物中加入阳离子供体物质; 和（f）搅拌双相混合物以实现短的单壁碳纳米管优先转运到非极性相中，使得非极性相富集在短的单壁碳纳米管中，极性相富集较长的单壁碳纳米管。 在其它实施方案中，类似的方法用于任何类型的CNT的长度分离，更通常地，对于任何类型的一维纳米结构。

    Method for cutting single-wall carbon nanotubes through fluorination
    8.
    发明授权
    Method for cutting single-wall carbon nanotubes through fluorination 失效
    通过氟化法切割单壁碳纳米管的方法

    公开(公告)号：US07029646B2

    公开(公告)日：2006-04-18

    申请号：US10408886

    申请日：2003-04-08

    申请人： John L. Margrave ,  Zhenning Gu ,  Robert H. Hauge ,  Richard E. Smalley

    发明人： John L. Margrave ,  Zhenning Gu ,  Robert H. Hauge ,  Richard E. Smalley

    IPC分类号： D01F9/12

    CPC分类号： B82Y30/00 ,  B82Y40/00 ,  C01B32/174 ,  C01B32/176 ,  C01B2202/02

    摘要： 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.

    摘要翻译： 用于切割单壁碳纳米管的方法涉及部分氟化单壁碳纳米管并在惰性气氛或真空中高达约1000℃热解部分氟化的纳米管。在切割之前，任选地提纯纳米管。 部分氟化涉及将纳米管氟化为CF x的碳氟化学计量，其中x为约0.3。 本发明还涉及氟化和切割的单壁碳纳米管的衍生化。 根据氟化和热解条件，可以将单壁碳纳米管切割成任何长度。 短纳米管在各种应用中是有用的，例如用于平板显示器的场发射器和用于进一步的纳米管生长的“种子”。

    Process utilizing pre-formed cluster catalysts for making single-wall carbon nanotubes
    9.
    发明授权
    Process utilizing pre-formed cluster catalysts for making single-wall carbon nanotubes 有权
    使用预先形成的簇催化剂制备单壁碳纳米管的方法

    公开(公告)号：US06913789B2

    公开(公告)日：2005-07-05

    申请号：US10059570

    申请日：2002-01-29

    申请人： Richard E. Smalley ,  Robert H. Hauge ,  Peter Athol Willis ,  W. Carter Kittrell

    发明人： Richard E. Smalley ,  Robert H. Hauge ,  Peter Athol Willis ,  W. Carter Kittrell

    IPC分类号： B01J3/00 ,  B01J19/26 ,  C01B31/02 ,  D01F9/127 ,  C23C16/26

    CPC分类号： B82Y30/00 ,  B01J3/008 ,  B01J19/26 ,  B01J2219/00085 ,  B01J2219/00094 ,  B01J2219/00108 ,  B01J2219/00121 ,  B82Y40/00 ,  C01B32/162 ,  C01B2202/02 ,  D01F9/127 ,  Y02P20/544 ,  Y10S977/843

    摘要： A gas-phase method for producing high yields of single-wall carbon nanotubes with high purity and homogeneity is disclosed. The method involves using preformed metal catalyst clusters to initiate and grow single-wall carbon nanotubes. In one embodiment, multi-metallic catalyst precursors are used to facilitate the metal catalyst cluster formation. The catalyst clusters are grown to the desired size before mixing with a carbon-containing feedstock at a temperature and pressure sufficient to initiate and form single-wall carbon nanotubes. The method also involves using small fullerenes and preformed sections of single-wall carbon nanotubes, either derivatized or underivatized, as seed molecules for expediting the growth and increasing the yield of single-wall carbon nanotubes. The multi-metallic catalyst precursors and the seed molecules may be introduced into the reactor by means of a supercritical fluid. In addition the seed molecules may be introduced into the reactor via an aerosol or smoke.

    摘要翻译： 公开了一种用于产生高纯度和均匀性的高产率单壁碳纳米管的气相方法。 该方法涉及使用预制金属催化剂簇来引发和生长单壁碳纳米管。 在一个实施方案中，多金属催化剂前体用于促进金属催化剂簇形成。 在与含碳原料混合之前，在足以引发和形成单壁碳纳米管的温度和压力下将催化剂簇生长至所需尺寸。 该方法还涉及使用衍生化或未衍生化的单壁碳纳米管的小富勒烯和预制部分作为种子分子，用于加速生长并提高单壁碳纳米管的产率。 可以通过超临界流体将多金属催化剂前体和种子分子引入反应器。 此外，可以通过气溶胶或烟雾将种子分子引入反应器。

    Process for purifying single-wall carbon nanotubes and compositions thereof
    10.
    发明授权
    Process for purifying single-wall carbon nanotubes and compositions thereof 有权
    单壁碳纳米管纯化方法及其组合物

    公开(公告)号：US06752977B2

    公开(公告)日：2004-06-22

    申请号：US10068907

    申请日：2002-02-08

    申请人： Richard E. Smalley ,  Robert H. Hauge ,  Wan-Ting Chiang

    发明人： Richard E. Smalley ,  Robert H. Hauge ,  Wan-Ting Chiang

    IPC分类号： D01F912

    CPC分类号： B82Y30/00 ,  B82Y40/00 ,  C01B32/17 ,  C01B2202/02 ,  D01F9/1278 ,  D01F11/121 ,  Y10S977/75 ,  Y10S977/845

    摘要： 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. The present invention provides a scalable means for producing high-purity single-wall carbon nanotube material.

    摘要翻译： 本发明涉及纯化单壁碳纳米管和纯化的单壁碳纳米管材料的方法。 单壁碳纳米管生产的已知方法导致单壁碳纳米管产物，除了包含残留金属催化剂颗粒的杂质和围绕催化剂颗粒的小的无定形碳片的含量之外，还包含单壁碳纳米管，并出现在 单壁碳纳米管的侧面和单壁碳纳米管的“绳索”。 净化过程除去外来碳以及含金属的残留催化剂颗粒。 该方法采用包括无定形碳的气相氧化和随后的含卤素酸与含金属物质的液相反应的步骤。 任选地，单壁碳纳米管材料可以是干燥的或在水分存在下退火的。 本发明提供了用于生产高纯度单壁碳纳米管材料的可伸缩手段。