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    • 1. 发明授权
    • Halogen-assisted chemical vapor deposition of diamond
    • 金属辅助化学气相沉积金刚石
    • US5071677A
    • 1991-12-10
    • US528804
    • 1990-05-24
    • Donald E. PattersonRobert H. HaugeC. Judith ChuJohn L. Margrave
    • Donald E. PattersonRobert H. HaugeC. Judith ChuJohn L. Margrave
    • C23C16/26C23C16/27
    • C23C16/27C23C16/277Y10S427/103
    • The present invention is directed to a method for depositing diamond films and particles on a variety of substrates by flowing a gas or gas mixture capable of supplying (1) carbon, (2) hydrogen and (3) a halogen through a reactor over the substrate material. The reactant gases may be pre-mixed with an inert gas in order to keep the overall gas mixture composition low in volume percent of carbon and rich in hydrogen. Pre-treatment of the reactant gases to a high energy state is not required as it is in most prior art processes for chemical vapor deposition of diamond. Since pre-treatment is not required, the process may be applied to substrates of virtually any desired size, shape or configuration.The reactant gas mixture preferably is passed through a reactor, a first portion of which is heated to a temperature of from about 400.degree. C. to about 920.degree. C. and more preferably from about 800.degree. C. to about 920.degree. C. The substrate on which the diamond is to be grown is placed in the reactor in a zone that is maintained at a lower temperature of from about 250.degree. C. to about 750.degree. C., which is the preferred diamond growth temperature range. The process preferably is practiced at ambient pressures, although lower or higher pressures may be used. Significant amounts of pure diamond films and particles have been obtained in as little as eight hours. The purity of the diamond films and particles has been verified by Raman spectroscopy and powder x-ray diffraction techniques.
    • 本发明涉及通过使能够(1)碳,(2)氢和(3)卤素的气体或气体混合物通过反应器流过衬底的方式将金刚石膜和颗粒沉积在各种衬底上的方法 材料。 反应物气体可以与惰性气体预混合,以便使总体气体混合物组合物的碳体积百分比低并富含氢气。 不需要将反应物气体预处理至高能量状态,如在金刚石的化学气相沉积的大多数现有技术方法中。 由于不需要预处理,所以该方法可以应用于几乎任何所需尺寸,形状或构型的基底。 反应气体混合物优选通过反应器,其第一部分被加热到约400℃至约920℃,更优选约800℃至约920℃的温度。 将金刚石生长在其上的底物置于反应器中,该区域保持在约250℃至约750℃的较低温度,这是优选的金刚石生长温度范围。 该方法优选在环境压力下实施,尽管可以使用更低或更高的压力。 在短短8小时内就已经获得了大量的纯金刚石膜和颗粒。 通过拉曼光谱和粉末X射线衍射技术验证了金刚石膜和颗粒的纯度。
    • 9. 发明授权
    • Chemical derivatization of single-wall carbon nanotubes to facilitate solvation thereof, and use of derivatized nanotubes
    • 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
    • US06835366B1
    • 2004-12-28
    • US09787473
    • 2001-03-16
    • John L. MargraveEdward T. MickelsonRobert HaugePeter BoulChad HuffmanJie LiuRichard E. SmalleyKen SmithDaniel T. Colbert
    • John L. MargraveEdward T. MickelsonRobert HaugePeter BoulChad HuffmanJie LiuRichard E. SmalleyKen SmithDaniel T. Colbert
    • D01F912
    • B01J21/18B01J23/74B01J23/755B01J35/006B01J35/06B82Y30/00B82Y40/00C01B32/174C01B2202/02C01B2202/06D01F11/121Y10S977/74Y10S977/748Y10S977/75Y10S977/843Y10S977/848
    • 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.
    • 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。