CN1349478A - 多层碳纳米管薄膜 - Google Patents
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Abstract
本发明涉及一种制备无基质的排列好的纳米管薄膜的方法,该法包括:(a)在适合纳米管形成的催化剂存在下,通过含碳材料的热解在石英玻璃基质上合成一层排列好的碳纳米管;以及(b)在纳米管/基质界面刻蚀石英玻璃基质,以便从基质上剥离所述的排列好的纳米管层。本发明的另一方法提供一种制备多层碳纳米管薄膜的方法,该法包括将无基质的碳纳米管薄膜沉积在另一纳米管薄膜上。在本发明的另一方面,提供一种制备“异质结构的”多层碳纳米管薄膜的方法,该薄膜含有一层或多层碳纳米管层和其他材料例如金属、半导体和聚合物的层。
Description
本发明涉及多层碳纳米管材料,每一层中的纳米管有可控的厚度、直径和堆积密度,以及涉及其制备方法。本发明还涉及包含一层或多层碳纳米管的异质结构的多层碳纳米管材料,以及涉及其制备方法。本发明还涉及由这样的材料制造的在许多领域中实际应用的设备结构,包括电子场发射体、人造激励器、化学传感器、气体贮存、分子过滤膜、贮能材料、分子晶体管和其他光电设备。
碳纳米管的直径通常为约数十埃,其长度高达数微米。这些细长的纳米管由按同心方式排列的碳六角体组成,管的两端通常被含有七角体的类fullerene结构物覆盖。它们可起半导体和金属的作用,它与直径和管壁中石墨环排列的螺旋性有关;不同的碳纳米管可连接在一起,生成具有有兴趣的电学、磁学、非线性光学、热学和机械学性质的分子细丝。这些独特的性质使碳纳米管在材料科学和纳米技术中有各种各样潜在的应用。的确,已提出碳纳米管在平面显示器中用作电子场发射体,用作单分子晶体管、扫描探针显微镜头、气体贮存和电化学能贮存、催化剂和蛋白质/DNA载体、分子过滤膜和吸能材料等新材料(例如参见M.Dresselhaus等,物理世界,一月号,33,1998;P.M.Ajayan和T.W.Ebbesen,Rep.Prog.Phys.(物理进展报告),60,1027,1997;R.Dagani,化学与工程新闻,1月11日,31,1999)。
对于上述大多数应用来说,十分希望制备排列好的碳纳米管,以致单个纳米管的性质可以很容易评价,以及它们可以有效地结合到设备中。用大多数通用的技术合成的碳纳米管(例如电弧放电和催化热解)常常存在随意缠结的状态(例如参见:T.W.Ebbesen和P.M.Ajayan,自然,358,220,1992;M.Endo等,物理化学固体杂志,54,1841,1994;V.Ivanov等,化学物理通讯,223,329,1994)。但是,最近已用合成操作法(例如参见:M.Endo等,物理化学固体杂志,54,1841,1994;V.Ivanov等,化学物理通讯,223,329,1994;H.Takikawa等,日本应用物理杂志,37,L187,1998)或用诱发合成的排列法(例如参见:W.Z.Li,科学,274,1071,1996;Che,G,自然,393,346,1998;Z.G.Ren等,科学,282,1105,1998;C.N.Rao等,化学学会杂志,化学通讯,1525,1998)来制备排列好的碳纳米管。
由排列好的碳纳米管产生的多层结构物具有很重要的意义,因为多层半导体材料和设备的应用对于许多应用来说是十分希望的。例子包括分子束外延用于制备由砷化镓和砷化铝交替层组成的超点阵结构物作为异质结构的半导体材料(M.A.Herman和H.Sitter,“束外延;基础和现状”,Springer-Verlag,柏林,1989)、Langmuir-Blodgett和化学蒸汽沉积技术用于有机场发射晶体管的制作(M.F.Rubner和T.A.Skotheim,“共轭聚合物”,J.L.Bredas和R.Silbey(编辑),Kluwer科学出版社,多德雷赫特,1991;G.Horowitz,材料进展,10,365,1998)和层与层吸附和溶液喷淋法用于制备用作有机光发射二极管的多层薄膜(S.A.Jenekhe和K.J.Wynne,“光聚合物和光电聚合物”,美国化学学会讨论会系列,672,美国化学学会,华盛顿,1995;L.Dai,J.Macromole.Sci.,Rev.Macromole.Chem.Phys.1999,39(2),273-387)。多层材料和/或设备的整个性质不仅与每一层中的组成材料的固有特性,而且也与具体层的叠排顺序、界面和表面结构物有密切关系,因此与设计和控制它们的行为的新加的额外参数有密切关系。现已发现,大面积上垂直排列的碳纳米管的多层结构物可用顺序合成法或用转移无基质纳米管薄膜法来制备。
根据第一个方面,本发明提供一种制备无基质的排列好的纳米管薄膜的方法,该法包括:(a)在适合纳米管生成的催化剂存在下,通过含碳材料的热解在石英玻璃基质上合成一层排列好的碳纳米管;以及(b)在纳米管/基质界面处刻蚀石英玻璃基质,以便从基质上剥离所述的排列好的纳米管层。
通过刻蚀石英玻璃基质分离排列好的纳米管层能生成沉积在另外的基质例如电极上和/或在多层材料中作为一层的纳米管薄膜,在转移的薄膜中很大程度保持了排列好的纳米管的完整性。
含碳的材料可为任何一种含碳的和在适合的催化剂存在下热解时能形成碳纳米管的化合物或物质。适合的含碳材料的例子包括烷烃、烯烃、炔烃或芳烃及其衍生物,例如甲烷、乙炔、苯、过渡金属酞菁(例如Fe(II)酞菁)以及其他有机金属化合物(例如铁茂和镍二环戊二烯)。
催化剂可为任何一种适合在热解条件下催化含碳材料转化成排列好的碳纳米管的化合物、元素或物质。催化剂可为过渡金属,例如Fe、Co、Al、Ni、Mn、Pd、Cr或它们任何适合氧化态的合金。
催化剂可结合到基质中或可包含在含碳的材料中,包含过渡金属催化剂的含碳材料的例子是Fe(II)酞菁、Ni(II)酞菁、镍二环戊二烯和铁茂。当催化剂和含碳材料包含在相同材料中时,可能需要提供另外的催化剂源或另外的含碳材料源。例如,当铁茂用作催化剂和碳源时,需要提供另外的碳源(例如乙烯),以便获得所需的纳米管生长。
所用的热解条件取决于所用的含碳材料的类型和催化剂类型,以及所需的纳米管的长度和密度。在这方面,为了得到有不同特性的纳米管,改变热解的条件,例如温度、时间、压力或通过热解反应器的速率是可能的。
例如,在较高的温度下进行热解可能生成与在较低温度下制备的有不同基端结构物的纳米管。热解通常在800-1100℃下进行。类似的是,降低通过流动型热解反应器的流速可导致纳米管有更小的堆积密度,反之亦然。熟悉本专业的技术人员能够选择和控制热解条件,以制得有所需特性的纳米管。
石英玻璃基质可用以下方法刻蚀:使涂覆过的石英玻璃基质经受能从基质上剥离碳纳米管薄膜的任何条件,或者将石英玻璃基质溶解。例如,可将涂覆过的基质浸泡在氢氟酸水溶液中或与氢氟酸水溶液接触。
在本发明的另一方面,提供了一种制备多层碳纳米管薄膜的方法,该法包括:(a)在适合纳米管形成的催化剂存在下,通过含碳材料的热解,在适合的基质上合成一层排列好的碳纳米管,得到纳米管涂覆的基质;(b)在适合纳米管形成的催化剂存在下,通过含碳材料的热解,在所述的纳米管涂覆的基质上合成另一层排列好的碳纳米管。
根据这一方面,基质可为任何一种能经受住所用的热解条件并能支持排列好的碳纳米管生长的基质。适合基质的例子包括石英玻璃、中孔氧化硅、纳米孔氧化铝、陶瓷板、玻璃、石墨和云母。优选的基质是石英玻璃。
可重复本发明这一方面的第二步,以提供三层或更多层的碳纳米管层。
步骤(b)使用的热解条件可与步骤(a)使用的条件相同或不同。类似的是,与合成任何另外层有关的热解条件都可与步骤(a)和(b)中使用的条件相同或不同。热解条件的改变可能得到不同结构物的层,导致不同的特性,例如导电性,对于每一纳米管层,能制造类二极管的电子设备或制造在每一表面上有不同材料的非对称层状复合材料。
按照上述方法,通过选择石英玻璃作为基质以及将薄膜从基质上剥离,还可制备无基质的排列好的多层碳纳米管薄膜。
本发明的另一方面,提供这样一种制备多层碳纳米管薄膜的方法,该法包括将无基质的碳纳米管薄膜沉积到另一碳纳米管薄膜上。
这一方面代表形成多层碳纳米管薄膜的供选择的方法。根据本发明的这一方面,可为单层或多层的碳纳米管薄膜从在上面形成它的石英玻璃基质上剥离,然后作为另一层沉积在另外的碳纳米管薄膜上,后者本身可为单层的或多层的,它可能附着到基质上或没有基质。为了增加层的数目,这一过程可重复使用。
本发明的另一方面,提供一种制备无基质的异质结构的多层碳纳米管薄膜的方法,该法包括:(a)在适合形成纳米管的催化剂存在下,通过含碳材料的热解在金属、金属氧化物或半导体涂覆的石英玻璃基质上合成一层排列好的碳纳米管;以及(b)在石英/金属表面刻蚀所述的基质,以便从石英玻璃上剥离所述的异质结构的多层薄膜。
这里使用的术语“异质结构的”指含有一个或多个碳纳米管层以及其他材料例如金属、半导体、聚合物等层的多层结构。
用来涂覆石英玻璃基质的金属可为任何一种能在所用的热解条件下支持碳纳米管生长的适合金属。适合金属的例子包括Au、Pt、Cu、Cr、Ni、Fe、Co和Pd。适合金属氧化物的例子包括铟锡氧化物(ITO)、Al2O3、TiO2和MgO。半导体材料的例子包括砷化镓、砷化铝、硫化铝和硫化镓。
在从石英玻璃基质上刻蚀异质结构的薄膜以前,有可能将一层或多层外加的层加到薄膜上。这些外加的层可为在适合催化剂存在下通过含碳材料进一步热解加入的碳纳米管层或可通过无基质的单层或多层排列好的碳纳米管薄膜的沉积加入。外加的层也可包括其他材料(例如金属、金属氧化物、半导体材料或聚合物)通过任何一种适合的方法沉积到碳纳米管层上的层。适合的聚合物的例子包括共轭(导电)聚合物、热敏/压敏聚合物、生物活性聚合物和工程树脂。
另一方面,本发明提供一种制备异质结构的多层碳纳米管薄膜的方法,该法包括将无基质的排列好的碳纳米管薄膜插入到多层结构中。
在这一方面,多层结构可能包含金属、金属氧化物、半导体材料或聚合物层。
在本发明的另一方面,提供这样一种制备异质结构的多层碳纳米管薄膜的方法,该法包括:(a)在适合纳米管形成的催化剂存在下,通过含碳材料的热解在石英玻璃基质上合成一层排列好的碳纳米管;得到纳米管涂覆的基质;(b)将一层耐热解的材料涂覆到所述的纳米管涂覆的基质上,得到异质结构的多层基质;(c)在适合纳米管形成的催化剂存在下,通过含碳材料的热解在所述的异质结构的多层基质上合成另一层排列好的碳纳米管。
正如象以前讨论的本发明方面一样,可包含外加的碳纳米管或其他材料层,以及薄膜可从石英玻璃基质上刻蚀,得到无基质的薄膜。
根据本发明任一方法制备的多层薄膜、以及用这些多层薄膜涂覆或包含这些多层薄膜的设备和材料表示本发明另外一些方面。
正如从上述清楚的,本发明能制备各种各样多层薄膜和结构物。也可能用适合的掩蔽技术和刻蚀技术得到有图案的层。本发明的方法和制成的薄膜结构物可能用于以下应用场合:1)电子发射器;2)场-发射晶体管;3)光电池的电极和光发射二极管;4)光电元件;5)铋激励器;6)化学传感器和生物传感器;7)气体贮存;8)分子过滤膜;9)吸能材料。
从以下几个实施例的详细描述可更加全面地理解本发明,其中涉及一些附图。应当理解,所述的实施例仅仅为了说明目的,并不打算构成本发明的限制。
参考附图:
图1为适合于制备本发明排列好的碳纳米管的热解流动反应器图。
图2a为本发明制备的排列好的碳纳米管的扫描电子显微镜图。
图2b为单个碳纳米管的高分辨率透射电子显微镜图。
图3为通过无基质的碳纳米管薄膜的沉积制备的双层碳纳米管结构物的扫描电子显微镜图。
图4a为用第一纳米管层作为第二层生长的基质制备的双层碳纳米管结构物的扫描电子显微镜图。
图4b与图4a相似,不同的是在第二层的合成过程中使用降低的流速。
实施例1 排列好的碳纳米管的制备
排列好的碳纳米管在Ar/H2、800-1100℃下,用适合的基质在石英玻璃管和装有独立的温度控制器的双热解炉组成的流动反应器(图1)中,通过Fe(II)酞菁的热解来制备。图2a表示碳纳米管的典型扫描电子显微镜图(SEM,XL-30FEGSEM,Philips,5KV)表明刚合成的纳米管相对于基质表面几乎正交排列。排列好的纳米管紧密地堆积,有大约25微米的十分均匀的管长。但是,排列好的纳米管的长度可通过改变实验条件(例如热解时间、流速)以可控的方式在宽的范围内(几微米到几十微米)变化。在单个纳米管的高分辨率透射电子显微镜图(图2)(HR-TEM,CM30,Philips,300KV)中说明很好石墨化的结构,约40同心碳壁和约40纳米外径。
实施例2 排列好的碳纳米管的无基质薄膜的制备
实施例1中制备的碳纳米管作为黑色层出现在基质(例如石英玻璃板)上,它可作为粉末从基质上刮掉。更重要的是,黑色沉积物很容易通过简单地将纳米管沉积的石英板浸泡在氢氟酸水溶液(10-40%重量)中作为无基质的漂浮的薄膜从石英玻璃上分离出来。这一技术能将纳米管薄膜转移到各种其他特别有意义的基质上(例如电化学的电极),在转移的薄膜中很大程度保持了排列好的纳米管的完整性。
实施例3 通过重复转移自由悬浮的薄膜制备多层纳米管薄膜
排列好的纳米管的无基质薄膜可以很容易转移到各种基质上,包括那些可能在高温下通过Langmuir-Blodgett技术不适合纳米管生长的基质(例如聚合物膜)。通过无基质的纳米管薄膜彼此反复沉积,可制得排列好的碳纳米管的多层薄膜(如图3中所示的双层结构)。应当指出,通过交替沉积无基质的纳米管薄膜和外来材料可制成任何两连续层之间夹杂有外来组分的异质结构的多层薄膜。
实施例4 通过在热解过程中的就地生长法来制备多层纳米管薄膜
图4a表示通过使用第一纳米管层作为基质或第二层纳米管在分开的实验中生长的方法制备的双层碳纳米管薄膜的典型扫描电子显微镜图。图4b表示通过在第一纳米管层形成时降低单体流速生成的双层纳米管薄膜的相应SEM图,表明第二纳米管层有较小的堆积密度。所以,正如可看见的,每一层中的排列好的纳米管的长度和堆积密度可通过选择不同的合成途径和/或改变实验条件(例如热解时间、流速)来改变。而且,与图4a有关的合成法能通过在任何两个连续层之间引入外来材料(例如Au、Pt、Cu和ITO)来制得异质结构的多层纳米管薄膜。
除非需要另加说明,整个说明书和随后的权利要求书中,“comprise”一词及其变化形式例如“comprises”和“comprising”应理解包括所述的整数或步骤或一组整数或步骤,但不排除任何其他的整数或步骤或一组整数或步骤。
熟悉本专业的技术人员应理解,在这里描述的本发明可以作出不同于这些具体描述的变通方案和改变。应当理解,本发明包括所有这样的变通方案和改变。本发明还单个包括或总体包括说明书涉及的和包含的所有步骤、特点、组合物和化合物以及所述步骤或特点的任何两个或多个的任何组合和所有组合。
Claims (24)
1.一种制备无基质的排列好的纳米管薄膜的方法,该法包括:
(a)在适合纳米管形成的催化剂存在下,通过含碳材料的热解在石英玻璃基质上合成一层排列好的碳纳米管;以及
(b)在纳米管/基质界面刻蚀石英玻璃基质,以便从基质上剥离所述的排列好的纳米管层。
2.根据权利要求1的方法,其中含碳的材料选自烷烃、烯烃、炔烃、芳烃及其过渡金属衍生物。
3.根据权利要求1的方法,其中催化剂包括过渡金属。
4.根据权利要求3的方法,其中催化剂选自Fe、Co、Al、Ni、Mn、Pd、Cr及其任何适合氧化态的合金。
5.根据权利要求1的方法,其中将催化剂结合到基质中。
6.根据权利要求1的方法,其中至少一部分催化剂包含在含碳的材料中。
7.根据权利要求6的方法,其中含有催化剂的含碳材料选自Fe(II)酞菁、Ni(II)酞菁、铁茂和镍二环戊二烯。
8.根据权利要求6的方法,其中在热解步骤中提供外加催化剂源或外加含碳材料源。
9.根据权利要求1的方法,其中热解在800-1100℃下进行。
10.根据权利要求1的方法,其中步骤(a)在流动型热解反应器中进行。
11.根据权利要求10的方法,其中在基质中合成的排列好的碳分子有这样的堆积密度,它可通过调节通过反应器的含碳材料的流速来控制。
12.根据权利要求1的方法,其中通过用氢氟酸水溶液浸泡涂覆过的基质或涂覆过的基质与氢氟酸水溶液接触来从基质上刻蚀排列好的分子层。
13.一种制备多层碳纳米管薄膜的方法,该法包括:
(a)在适合纳米管形成的催化剂存在下,通过含碳材料的热解在适合的基质上合成一层排列好的碳纳米管,得到纳米管涂覆的基质;
(b)在适合纳米管形成的催化剂存在下,通过含碳材料的热解在所述的纳米管涂覆的基质上合成另一层排列好的碳纳米管。
14.根据权利要求13的方法,其中基质选自石英玻璃、中孔氧化硅、纳米孔氧化铝、陶瓷板、玻璃、石墨和云母。
15.根据权利要求14的方法,其中基质为石英玻璃。
16.根据权利要求13的方法,其中步骤(b)被重复,得到3层或3层以上的碳纳米管。
17.根据权利要求13的方法,其中使用不同于在步骤(a)中使用的那些条件合成另外的层。
18.一种制备无基质的异质结构的多层碳纳米管薄膜,该法包括:
(a)在适合纳米管形成的催化剂存在下,通过含碳材料的热解在金属、金属氧化物或半导体涂覆的石英玻璃基质上合成一层排列好的碳纳米管;以及
(b)在石英/金属表面刻蚀所述的基质,使所述的异质结构的多层薄膜从石英玻璃剥离。
19.根据权利要求18的方法,其中石英玻璃基质用选自Au、Pt、Cu、Cr、Ni、Fe、Co和Pd的金属、选自铟锡氧化物(ITO)、Al2O3、TiO2和MgO的金属氧化物或选自砷化镓、砷化铝、硫化铝和硫化镓的半导体材料涂覆。
20.一种制备异质结构的多层碳纳米管薄膜的方法,该法包括将无基质的排列好的碳纳米管薄膜插入到多层结构中。
21.一种制备异质结构的碳纳米管薄膜的方法,该法包括:
(a)在适合纳米管形成的催化剂存在下,通过含碳材料的热解在石英玻璃基质上合成一层排列好的碳纳米管,得到纳米管涂覆的基质;
(b)将一层耐热解的材料涂覆到所述的纳米管涂覆的基质上,得到异质结构的多层基质;
(c)在适合纳米管形成的催化剂存在下,通过含碳材料的热解在所述的异质结构的多层基质上合成另一层排列好的碳纳米管。
22.一种根据权利要求1的方法制备的无基质的排列好的碳纳米管薄膜。
23.一种根据权利要求13的方法制备的多层碳纳米管。
24.一种根据权利要求18、20或21中任一项的方法制备的无基质的异质结构的碳纳米管。
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- 2000-04-14 KR KR1020017012977A patent/KR20020024580A/ko not_active Application Discontinuation
- 2000-04-14 EP EP00915051A patent/EP1183210B1/en not_active Expired - Lifetime
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ATE458698T1 (de) | 2010-03-15 |
TW483870B (en) | 2002-04-21 |
AUPP976499A0 (en) | 1999-05-06 |
ZA200108303B (en) | 2003-03-26 |
JP2002542136A (ja) | 2002-12-10 |
EP1183210A4 (en) | 2004-06-09 |
IL145896A0 (en) | 2002-07-25 |
EP1183210B1 (en) | 2010-02-24 |
US6808746B1 (en) | 2004-10-26 |
CA2370022A1 (en) | 2000-10-26 |
DE60043887D1 (de) | 2010-04-08 |
EP1183210A1 (en) | 2002-03-06 |
WO2000063115A1 (en) | 2000-10-26 |
KR20020024580A (ko) | 2002-03-30 |
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