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    • 1. 发明授权
    • Single-wall carbon nanotubes from high pressure CO
    • 单壁碳纳米管由高压CO
    • US07204970B2
    • 2007-04-17
    • US10730630
    • 2003-12-08
    • Richard E. SmalleyKen A. SmithDaniel T. ColbertPavel NikolaevMichael J. BronikowskiRobert K. BradleyFrank Rohmund
    • Richard E. SmalleyKen A. SmithDaniel T. ColbertPavel NikolaevMichael J. BronikowskiRobert K. BradleyFrank Rohmund
    • C01B11/02
    • B01J4/002B01J3/04B01J3/042B01J19/121B01J19/26B01J2219/0875B82Y30/00B82Y40/00C01B32/162C01B2202/02C01B2202/36D01F9/1278Y10S977/75Y10S977/751Y10S977/843Y10S977/845Y10S977/951Y10T428/30
    • The present invention discloses the process of supplying high pressure (e.g., 30 atmospheres) CO that has been preheated (e.g., to about 1000° C.) and a catalyst precursor gas (e.g., Fe(CO)5) in CO that is kept below the catalyst precursor decomposition temperature to a mixing zone. In this mixing zone, the catalyst precursor is rapidly heated to a temperature that results in (1) precursor decomposition, (2) formation of active catalyst metal atom clusters of the appropriate size, and (3) favorable growth of SWNTs on the catalyst clusters. Preferably a catalyst cluster nucleation agency is employed to enable rapid reaction of the catalyst precursor gas to form many small, active catalyst particles instead of a few large, inactive ones. Such nucleation agencies can include auxiliary metal precursors that cluster more rapidly than the primary catalyst, or through provision of additional energy inputs (e.g., from a pulsed or CW laser) directed precisely at the region where cluster formation is desired. Under these conditions SWNTs nucleate and grow according to the Boudouard reaction. The SWNTs thus formed may be recovered directly or passed through a growth and annealing zone maintained at an elevated temperature (e.g., 1000° C.) in which tubes may continue to grow and coalesce into ropes.
    • 本发明公开了提供已被预热(例如,约1000℃)的高压(例如30个大气压)的CO和催化剂前体气体(例如Fe(CO)5) >)在CO中,其保持低于催化剂前体分解温度至混合区。 在该混合区中,将催化剂前体快速加热到导致(1)前体分解的温度,(2)形成适当尺寸的活性催化剂金属原子簇,和(3)在催化剂簇上的SWNT的有利生长 。 优选使用催化剂簇成核剂来使催化剂前体气体快速反应以形成许多小的活性催化剂颗粒,而不是几个大的非活性催化剂颗粒。 这样的成核机构可以包括比主要催化剂更快地聚集的辅助金属前体,或者通过提供精确地指向需要簇形成的区域的额外的能量输入(例如来自脉冲或CW激光)。 在这些条件下,SWNT根据Boudouard反应成核并生长。 如此形成的SWNT可以直接回收或通过保持在高温(例如1000℃)的生长和退火区域,其中管可以继续生长并聚结成绳索。