CN1312318C - 制备无机纳米管的方法 - Google Patents

制备无机纳米管的方法 Download PDF

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CN1312318C
CN1312318C CNB031072585A CN03107258A CN1312318C CN 1312318 C CN1312318 C CN 1312318C CN B031072585 A CNB031072585 A CN B031072585A CN 03107258 A CN03107258 A CN 03107258A CN 1312318 C CN1312318 C CN 1312318C
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闵约赛
裵恩珠
崔原凤
曹永真
李正贤
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Samsung Electronics Co Ltd
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Abstract

本发明提供一种利用碳纳米管(CNT)作为模板制备无机纳米管的方法。该方法包括制备其上形成CNT或CNT阵列的模板；利用原子层沉积法(ALD)通过在模板上沉积无机材料，于CNT上形成无机薄膜；及除去CNT，得到无机纳米管或无机纳米管阵列。

Description

制备无机纳米管的方法
技术领域
本发明涉及制备无机纳米管或无机纳米管阵列的方法，更具体地，本发明涉及以碳纳米管为模板的制备无机纳米管的方法。
背景技术
最近，随着集成与紧凑的光电设备的发展，有关纳米结构的材料及其制备方法正在积极地研发[Nature，1999，402，273；Angew.Chem.，Int.Ed.1999，38，2175]。具体地，自发现碳纳米管(CNT)之后，已经多次尝试采用CNT作为超精细的电子器件材料，方法是采用CNT的有序阵列和图案制备所述的器件[Nature，1991，354，56；Adv.Mater.2002，14，277；Appl.Phy.Lett.2001，79，3696；and Nature，2002，416，495]。另外，已经进行了各种尝试，希望将纳米管的结构和性能应用于下列的领域中：
高灵敏度的微量天平：Science 283，1513(1999)；
气体检测器：Science 287，622(2000)；
氢能贮存装置：Nature 386，512(1999)；
场发射显示器(FED)：Appl.Phys.Lett.72，2912(1998)；Science 283，512(1999)；
纳米镊子：Science 286，2148(1999)；
单电子晶体管(SET)：Science 293，76(2001)；
激励器：Science 284，1340(1999)；
存储器：Science 289，94(2000)；
催化剂：USP 6210800 B1；Nature 375，564(1995)；
UV吸收剂：USP 6027775；及
药物递送剂，油吸收剂，复合材料。
因此，已经广泛地研究采用不同材料制备纳米棒、线、管及颗粒的方法。然而，很少有人知道在系统阵列中采用适于制造纳米级器件的气相沉积法制造无机纳米管的方法。
已经研究过采用CNT制造第二纳米结构材料。例如，在高于其熔点的温度下熔化V2O5粉末并利用毛细管现象涂布CNT的方法[Science 375，564(1995)]；采用化学镀形成金属薄膜的方法[JJAP 36，L501(1997)]；利用CNT与B2O3之间的取代反应制造硼氮化物(BN)纳米管的方法[Appl.Phys.Lett.73，3085(1998)]；通过H2WO4与H2S之间的高温反应，用WS2涂布多壁纳米管(MWNT)的方法[Chem.Mater.14，2209，(2002)]；利用纳米管与金属氧化物(MO)之间的受限反应制造金属碳化物纳米棒的方法[Science 277，1287(1997)]；采用阳极多孔氧化铝和聚甲基丙烯酸甲酯(PMMA)制造TiO2纳米管阵列的方法[Langmuir 12，1441(1996)]；以及通过沉积SiO2制备纳米管的方法，该方法利用垂直排列的纳米纤维作模板，通过蚀刻暴露纳米纤维，并蚀刻掉所暴露出来的纳米纤维[Abstract of 46th International Conference onElectron，Ion and Photon Beam Technology and Nanofabrication，Anaheim，CA，269，(2002)]。这些方法采用了非常有限的反应，其被限制为采用特定的材料或蚀刻工艺，所以将这些方法应用于纳米结构材料的制造是不合适的。
发明内容
本发明提供一种制造各种类型的无机纳米管的方法。
一方面，本发明提供一种制造无机纳米管的方法。该方法包括制备其上形成碳纳米管(CNT)或CNT阵列的模板；利用原子层沉积法(ALD)通过在模板上沉积无机材料，于CNT上形成无机薄膜；及除去CNT，得到无机纳米管或无机纳米管阵列。
优选模板的制备包括在基材上形成多孔材料层；及由多孔材料层中的微孔生长CNT。
优选多孔材料层是由多孔氧化铝制成的。
优选多孔材料层的形成包括在基材上形成铝薄膜；及氧化所述铝薄膜，形成多孔氧化铝层。
优选CNT的除去包括在提供氧或臭氧的同时灰化和氧化无机薄膜。优选无机材料为钌，而且该钌是在低于300℃的温度下沉积的。作为选择，CNT的除去可以包括采用等离子体的蚀刻，以便在除去CNT时不氧化无机材料。
附图说明
通过参照附图详细地描述其优选实施方案，本发明的上述及其它特征和优点将会变得更加显而易见，在附图中：
图1利用原子层沉积(ALD)形成钌(Ru)薄膜时的沉积温度-生长速度曲线图；
图2A是形成于多孔氧化铝上的碳纳米管(CNT)阵列的纵向结构的扫描电子显微镜(SEM)照片；
图2B是形成于多孔氧化铝上的CNT阵列的平面结构的动力显微镜(DFM)照片；
图3A是根据本发明实施方案形成于CNT阵列上的Ru薄膜的纵向结构的SEM照片；
图3B是根据本发明实施方案形成于CNT阵列上的Ru薄膜的平面结构的DFM照片；
图3C是根据本发明实施方案形成于CNT阵列上的Ru薄膜的高分辨率发射电子显微镜(TEM)照片；
图3D是根据本发明实施方案形成于CNT阵列上的Ru薄膜的强反差图像；
图4A是根据本发明实施方案制备的RuOx纳米管的纵向结构的SEM照片；
图4B是根据本发明实施方案制备的RuOx纳米管的平面结构的DFM照片；
图4C是根据本发明实施方案制备的RuOx纳米管的高分辨率TEM照片；及
图4D是根据本发明实施方案制备的RuOx纳米管的强反差图像。
具体实施方式
为了制备无机纳米管或无机纳米管阵列，在本发明中采用碳纳米管(CNT)或CNT阵列作为模板。换言之，通过原子层沉积(ALD)，用无机纳米管的无机薄膜涂布CNT或CNT阵列。采用ALD形成无机薄膜的沉积行为在CNT的内外壁上是不同的。具体地，形成于CNT内壁的无机薄膜具有稀疏的微结构。因此，当在活泼的氧化气氛如氧、臭氧或等离子体气氛中处理无机薄膜时，CNT燃烧掉并形成新的第二无机纳米管或无机纳米管阵列。
根据本发明，通过除去CNT，涂有无机材料的CNT可以随第二无机纳米管一起制造，其在应用中用作模板。
本发明采用ALD制备无机纳米管，因而将简要地描述ALD。与同时提供前体和反应气体的化学气相沉积不同，在ALD中，前体和反应气体是利用吹扫工艺通过分时器单独提供的[Nanotechnology 10，19(1999)]。换言之，通过一系列步骤，例如前体提供步骤，吹扫步骤，反应气体提供步骤，以及吹扫步骤，前体通过化学作用吸附在基材表面的单原子层因与反应气体发生反应而分解，从而形成具有原子层厚度的薄膜。因此，生长速度自我限制的，所以可以通过控制处理循环的次数精确地控制薄膜的厚度。另外，沉积只有在化学吸附的化学物质与反应气体反应时才完成，所以生长速度取决于前体在所沉积之表面的化学吸附速度。采用ALD的最重要的特征和优点在于沉积可以在足以使前体不发生热分解的低温下进行。因此，当沉积在具有很大纵横比的立方基材上进行时，该立方基材可以完全被沉积层所覆盖。具体地，在不进行前体热分解的ALD条件下，生长速度不受温度的影响。然而，ALD要求前体或反应气体具有足够高的反应性，以便在表面上引发吸附物质与反应气体之间的反应。
同时，CNT通过碳原子之间的共价键得以形成，所以CNT在高于400℃的温度因为氧而燃烧掉[Nature 375，564(1995)]。因此，为了在CNT上形成薄膜，沉积需要在低温下进行，使得氧化反应受到抑制，或者采用氧化强度较弱的反应物如水。
钌(Ru)的ALD生长速度试验
图1示出了每个沉积循环Ru薄膜的ALD生长速度，该Ru薄膜用于制备本发明的纳米管。在本文中，基材是包含SiO2的Si基材。
为了在Si基材上形成Ru薄膜，利用Ar载气以150sccm的速度提供作为前体的0.1MRu(od)3(od＝辛烷-2，4-二酮酸)/乙酸正丁酯溶液2秒钟，并以100sccm的速度提供作为反应气体的氧2秒钟。在提供前体之后与提供反应气体之前，提供3秒钟的吹扫气体。因此，将每个沉积循环的总时间控制为10秒钟。ALD在275～450℃的范围内以25℃的间隔进行。结果，在低于350℃的温度下得到纯的Ru薄膜，但是在400℃以上的温度下所得到的主要是RuOx。在350～400℃，RuOx具有随温度增加而逐步增加的趋势。参照图1，由于在低于375℃时很少发生热分解导致的沉积，所以生长速度非常慢，即低于每沉积循环0.1nm。
CNT模板的制备
利用溅射法在Si晶片上形成厚度为500nm的Al薄膜，然后令其在0.3M的草酸溶液中在16℃和40V的直流电压下进行阳极氧化，从而形成多孔的氧化铝。随后，用0.1M的磷酸处理多孔氧化铝，以便扩大微孔的直径。其后，用10％的乙炔和N2平衡气体，于700℃和管式炉中于Si晶片上生长CNT 30分钟。用50W的Ar离子磨从所生长的CNT中除去石墨，从而得到CNT阵列，如图2A和2B所示。图2A是扫描电子显微镜(SEM)照片，示出了实际制备的CNT阵列的纵向结构；图2B是动力显微镜(DFM)照片，示出了CNT阵列的平面结构。
CNT模板上的无机ALD
采用ALD，在CNT模板的表面上形成本发明实施方案的无机纳米管即Ru纳米管。ALD的条件与Ru的ALD生长速度试验中所使用的相同。Ru的沉积是在低温例如在300℃下进行的，以便抑制CNT的分解，进而得到厚度为6nm或更小的Ru薄膜。
图3A是SEM照片，示出了采用ALD的Ru薄膜的纵向结构；图3B是DFM照片，示出了Ru薄膜的平面结构。与示出纯粹CNT之平面结构的图2B相比，图3B示出了披覆了Ru薄膜的CNT的平面结构，CNT的内径因为Ru薄膜而降低。图3C是Ru薄膜的高分辨率发射电子显微镜(TEM)照片。从图3C可以推断，CNT上的Ru薄膜具有结晶的微结构，而CNT模板具有很多缺陷的无定形结构。图3D的强反差图像表明，形成于CNT2的内壁3上的Ru薄膜的微结构比形成于CNT2的外壁1上的更稀疏。
无机纳米管的制备
Ru薄膜形成于CNT阵列上之后，在1托的压力和500℃的温度下进行1小时的灰化，通过氧的冲洗速度为100sccm，以便除去Ru薄膜下面的CNT并氧化Ru薄膜，进而形成RuOx管阵列，即无机纳米管阵列。
图4A示出了利用灰化法除去CNT所暴露出来的氧化铝微孔。图4B示出了采用灰化法除去CNT(见图3B)之后管的轻微扩张。CNT还可以利用等离子体而非伴随氧化反应的灰化法除去。
图4C和4D示出了利用灰化法除去CNT同时氧化形成于CNT上的Ru薄膜而制得的RuOx纳米管。
下表示出了每种元素的特征X-射线计数，作为发射电子显微术-能量色散光谱(TEM-EDS)的结果。Ru/CNT结构上的位置为外壁1上的位置1，如图3D所示；CNT2上的位置2如图3D所示；内壁3上的位置3如图3D所示。RuOx纳米管结构上的位置为氧化铝基材上的位置4，如图4D所示；Ru纳米管上的位置5如图4D所示。如果比较Ru/CNT结构中位置1、2和3处的C/Ru比，则可以推断，外壁1具有比内壁3更精细的结构。在RuOx结构中，碳很少出现，因为它已经被灰化。另外，由于Ru已经被氧化成RuOx，所以Al的特征X-射线计数在位置5处的比在位置4处的小。不过，位置4与5之间的氧计数没有变化，因为从RuOx中引入了氧。
表：各元素的特征X-射线峰的TEM-EDS分析结果
  Ru/CNT   RuOx
  元素   位置1   位置2   位置3   位置4   位置5
  C，Kα(0.282keV)   32   117   64   12   22
  O，Kα(0.523keV)   -   14   18   59   59
  Al，Lα(1.487keV)   -   -   -   116   31
  Ru，Kα(2.588keV)   110   33   116   8   99
为了通过上述方法制备无机纳米管，下面的条件必须得到满足。首先，必须固定前体、反应气体和沉积温度的条件，使得无机薄膜的ALD可以在不分解CNT的情况下进行。其次，在ALD过程中，必须提供允许内外壁沉积行为不同的CNT灰化的通道。然而，根据纳米管的应用目的，也可以采用无机薄膜披覆的CNT，而不通过灰化除去CNT。
本发明提供一种制备无机薄膜披覆的CNT的方法，通过ALD用无机薄膜披覆CNT或CNT阵列，同时允许通过高温灰化除去CNT来制备第二无机纳米管。由于本发明未采用受具体材料限制的反应，所以本发明可以应用于采用ALD前体于CNT上制备无机纳米管的任何情况。另外，本发明与其它微处理技术如半导体器件的制造相容。此外，采用ALD可以于各种阵列中制造不同形状的无机纳米管，而且可以很容易地在系统阵列中制造无机纳米管，无需进行单独的蚀刻过程。

Claims (8)

1.一种制备无机纳米管的方法，包括：
制备在其上形成碳纳米管或CNT阵列的模板；
在温度为275-450℃的范围内，利用原子层沉积法通过在模板上沉积无机材料，于CNT上形成无机薄膜；及
除去CNT，得到无机纳米管或无机纳米管阵列。
2.权利要求1的方法，其中所述模板的制备包括：
在基材上形成多孔的材料层；及
由该多孔材料层中的微孔生长CNT。
3.权利要求2的方法，其中该多孔材料层是由多孔氧化铝制成的。
4.权利要求2或3的方法，其中该多孔材料层的形成包括：
在基材上形成铝薄膜；及
氧化该铝薄膜，从而形成多孔的氧化铝层。
5.权利要求1～3中任一项的方法，其中CNT的除去包括在提供氧或臭氧的同时，灰化和氧化无机薄膜。
6.权利要求1～3中任一项的方法，其中CNT的除去包括采用等离子体的蚀刻。
7.权利要求1～3中任一项的方法，其中该无机材料为钌。
8.权利要求7的方法，其中所述的钌是在低于300℃的温度下沉积的。
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