CN1483668A - 一种碳纳米管阵列生长方法 - Google Patents

一种碳纳米管阵列生长方法 Download PDF

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CN1483668A
CN1483668A CNA02134776XA CN02134776A CN1483668A CN 1483668 A CN1483668 A CN 1483668A CN A02134776X A CNA02134776X A CN A02134776XA CN 02134776 A CN02134776 A CN 02134776A CN 1483668 A CN1483668 A CN 1483668A
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姜开利
范守善
李群庆
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Hongfujin Precision Industry Shenzhen Co Ltd
Beijing Funate Innovation Technology Co Ltd
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Abstract

一种碳纳米管阵列生长方法，包括以下步骤：提供一平滑基底，将催化剂沉积于该基底表面，将沉积有催化剂的基底在气体保护下加热至一特定温度后通入碳源气与保护气体的混合气体，控制该混合气体的流速及流量比，使催化剂温度与环境温度温差在50℃以上，且使碳源气的分压低于20％，反应5－30分钟使碳纳米管阵列从基底长出。该碳纳米管阵列中的碳纳米管呈束状。

Description

一种碳纳米管阵列生长方法
【技术领域】
本发明涉及一种碳纳米管生长方法，尤指一种碳纳米管阵列生长方法。
【背景技术】
碳纳米管是一种由碳原子组成的直径为纳米量级的碳管，在碳纳米管石墨层中央部份都是六元环，而在末端或转折部份则有五元环或七元环。碳纳米管是在1991年由Iijiima在电弧放电的产物中首次发现的，发表在1991年出版的Nature 354，56。碳纳米管的特殊结构决定了其具有优良的综合力学性能，如高弹性模量、高杨氏模量和低密度，以及优异的电学性能、热学性能和吸附性能。随着碳纳米管的长度、直径和螺旋方式的变化，碳纳米管可呈现出金属性或半导体性质。由于碳纳米管的优异特性，因此可望其在纳米电子学、材料科学、生物学、化学等领域中发挥重要作用。
目前制备碳纳米管的方法主要有电弧放电法、脉冲激光蒸发法及化学气相沉积法几种。电弧放电及脉冲激光蒸发法形成碳纳米管有以下几个缺点：(1)碳纳米管产量较低；(2)碳纳米管是和其他碳纳米颗粒混杂在一起，因此造成碳纳米管的纯度很低，还需要复杂的净化工艺，增加制造成本；(3)碳纳米管的生长方向无法控制，所形成的碳纳米管是无序混乱的，难于工业上应用。而形成有序碳纳米管阵列的方法目前主要是化学气相沉积法。化学气相沉积主要是运用纳米尺度的过渡金属或其氧化物作为催化剂，在相对低的温度下热解含碳的源气体来制备碳纳米管阵列。
范守善等人在文献Science 283，512-514(1999)，Self-orientedregular arrays of carbon nanotubes and their field emission properties中所描述的制备方法是：首先提供一多孔硅基底，其孔径大约为3纳米，然后通过掩模板用电子束蒸发法在基底上形成一层具有规则图案的催化剂层-铁层，然后将沉积有铁的基底在空气中300℃退火，然后将基底放在石英反应舟里送入石英管反应炉的中央反应室中，在氩气的保护下，将反应炉加热到700℃后，以流量1000sccm通入乙烯气，反应15-60分钟，然后将反应炉冷却到室温，有序碳纳米管阵列即沉积在基底上有铁的区域，并垂直于基底。但是因为碳纳米管生长过程中，无定型碳会同时沉积在碳纳米管的外表面，使碳纳米管之间的范德华力降低，故依该法生长出的碳纳米管阵列中的碳纳米管之间范德华力较弱。图1即为将依该法生长出的碳纳米管阵列放入二氯乙烷中超声作用10分钟后的透射电子显微镜(TEM，transmission electron microscope)照片，由图1可看到，超声作用后，碳纳米管阵列中碳纳米管已基本分散在二氯乙烷中。
【发明内容】
本发明的目的在于提供一种碳纳米管阵列生长方法，其生长出碳纳米管阵列中的碳纳米管表面干净平滑，通过范德华力结合成稳定的束状，即为束状碳纳米管阵列。
本发明的目的是这样实现的：提供一平滑基底，将催化剂沉积于该基底上，将沉积有催化剂的基底在气体保护下加热至一特定温度后通入碳源气与保护气体的混合气体，控制该混合气体的流速，使催化剂温度与环境温度的温差在50℃以上，控制该混合气体的流量比，使碳源气的分压低于20％，反应5-30分钟使碳纳米管阵列从基底长出。该生长出的碳纳米管阵列为束状碳纳米管阵列。
与现有技术相比较，本发明通过控制混合气体的流速使催化剂与环境产生温差，使碳纳米管生长速度提高；通过控制混合气体流量比使碳源气的分压较低，使无定性碳的沉积速度减慢，从而使生长出的碳纳米管具有干净光滑的表面，碳纳米管之间的范德华力增加，又因采用平滑基底，生长出的碳纳米管更密集易于通过范德华力聚集呈束状，形成束状碳纳米管阵列。
【附图说明】
图1是现有技术生长出的碳纳米管阵列在二氯乙烷中超声作用10分钟后的TEM照片。
图2是以本发明碳纳米管阵列生长方法生长出的碳纳米管阵列的扫描电子显微镜(SEM，scanning electron microscope)照片，其中***的SEM照片为放大的碳纳米管阵列。
图3是以本发明碳纳米管阵列生长方法生长出的碳纳米管阵列中一束碳纳米管的TEM照片。
图4是以本发明碳纳米管阵列生长方法生长出的碳纳米管阵列在二氯乙烷中超声作用10分钟后的TEM照片。
【具体实施方式】
首先提供一平滑基底，可选用P型或N型或本征硅晶片或表面有一层氧化硅的硅晶片为基底，本发明中选用P型硅晶片或表面有一层氧化硅的硅晶片作为基底，其直径为5.08厘米，厚350微米，将该基底抛光获得平滑基底。将金属催化剂利用电子束蒸发沉积、热沉积或溅射法等方法形成于基底上，其厚度为几纳米到几百纳米，其中金属催化剂可为铁(Fe)、钴(Co)、镍(Ni)或其合金之一，本发明选用铁为催化剂，沉积厚度为5纳米。
将沉积有催化剂的基底在空气中，在300-400℃热处理约10小时，使催化剂氧化成颗粒，然后再将其用氢气或氨气还原形成纳米级颗粒，再将处理后的基底切割成矩形基底。
将其中一片矩形基底装入一反应舟中，一般为石英反应舟，将舟装入管状石英炉中央的反应室里，在气体保护下加热至一预定温度，其中，该保护气体为惰性气体或氮气，本发明选用氩气，该预定温度因催化剂不同而不同，当选用催化剂为铁，则一般加热到500-700℃，优选为650℃。
通入碳源气与保护气体的混合气体，其中碳源气为碳氢化合物，可为乙炔、乙烯等，本发明选用乙炔；该保护气体为惰性气体或氮气，本发明选用氩气。通过控制碳源气的流速来控制催化剂的局部温度TC，环境温度TL直接通过控制炉子来调节，使催化剂的温度TC与反应炉中环境温度TL形成一温差ΔT至少在50℃以上，控制碳源气与保护气体的流量比，使碳源气的分压至少在20％以下，优选为分压在10％以下，反应5-30分钟使碳纳米管阵列从基底长出，如图2所示。因为碳纳米管生长速度和催化剂温度与环境温度的温差成正比，温差越大，碳纳米管生长越快；而无定性碳的沉积速度与碳源气分压成正比，碳源气分压越低，无定型碳的沉积速度越慢。故，本发明通过控制催化剂的温度TC与环境温度TL的温差ΔT至少在50℃以上，使碳纳米管的生长速度提高；通过调节碳源气与混合气体的流量比，使碳源气的分压至少在20％以下，使无定型碳的沉积速度减慢。采用此工艺条件后生长出的碳纳米管具干净光滑的表面，且碳纳米管之间范德华力较大，又因基底为平滑基底，生长出的碳纳米管较在多孔基底上生长出的碳纳米管更紧密，故碳纳米管易于因范德华力聚集形成束状，如图3所示。
故采用本发明的方法制备的碳纳米管阵列为束状碳纳米管阵列，且该束状结构很稳定，将以本发明的方法生长出的碳纳米管阵列在二氯乙烷中超声作用10分钟，拍得TEM照片，如图4所示，该阵列中的碳纳米管没有分散在二氯乙烷中，仍然成束状结构。

Claims (9)

1.一种碳纳米管阵列生长方法，其特征在于包括以下步骤：
(1)提供一平滑基底；
(2)将催化剂沉积于该基底表面；
(3)通入碳源气与保护气体的混合气体反应，使碳源气的分压低于20％，并且使催化剂的温度与环境温度的温差为50℃以上，使碳纳米管从基底上长出。
2.如权利要求1所述的碳纳米管阵列生长方法，其特征在于步骤(1)中的平滑基底为硅晶片或具氧化硅层的硅晶片。
3.如权利要求1所述的碳纳米管阵列生长方法，其特征在于催化剂与环境温度的温差是通过控制混合气体的流速实现的。
4.如权利要求1所述的碳纳米管阵列生长方法，其特征在于碳源气的分压通过控制碳源气与保护气体的流量比实现的。
5.如权利要求4所述的碳纳米管阵列生长方法，其特征在于该碳源气分压为10％。
6.如权利要求1所述的碳纳米管阵列生长方法，其特征在于步骤(2)中所用催化剂为铁、钴、镍或其合金之一。
7.如权利要求1所述的碳纳米管阵列生长方法，其特征在于在通入碳源气与保护气体的混合气体反应前还包括将沉积有催化剂的基底在空气中于300-400℃热处理10小时。
8.如权利要求7所述的碳纳米管阵列生长方法，其特征在于热处理后，通入混合气体反应之前还包括将基底在气体保护下，预加热到650℃。
9.如权利要求5所述的碳纳米管阵列生长方法，其特征在于步骤(3)中，通入的碳源气为乙炔，保护气体为氩气。
CNB02134776XA 2002-09-17 2002-09-17 一种碳纳米管阵列生长方法 Expired - Lifetime CN1248959C (zh)

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US10/334,547 US7754182B2 (en) 2002-09-17 2002-12-31 Carbon nanotube array and method for forming same
JP2003076542A JP3850380B2 (ja) 2002-09-17 2003-03-19 炭素ナノチューブのマトリックスの成長方法

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CN107597118B (zh) * 2017-09-01 2020-07-17 哈尔滨万鑫石墨谷科技有限公司 一种制备束丛状碳纳米管用催化剂、其制备方法及束丛状碳纳米管
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