CN1883807A - 用于制造碳纳米管的催化剂的制备方法 - Google Patents
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Abstract
本发明提供一种以更高的均匀性形成催化剂颗粒的新方法，该催化剂用于生长碳纳米管；以及一种均匀性得到提高的碳纳米管的合成方法。所述形成催化剂颗粒的方法包括：将催化金属前体溶液涂布到基材上；冷冻干燥涂布到基材上的催化金属前体溶液；及还原冷冻干燥的催化金属前体为催化金属。该形成催化剂颗粒的方法，在通过冷冻干燥催化剂金属前体溶液形成催化剂颗粒时，可以使催化剂颗粒的结块和/或重结晶最小化。通过该方法形成的催化剂颗粒，具有非常均匀的颗粒尺寸，并非常均匀地分布在基材上。
Description
技术领域
本发明涉及一种用于制造碳纳米管的催化剂的制备方法，以及一种利用该催化剂制备碳纳米管的方法。
背景技术
碳纳米管具有直径为几个纳米且纵横比非常大(约为10～1000)的圆柱形结构。在碳纳米管中，碳原子一般以六边形的蜂巢形图案排列。一个碳原子与三个相邻的碳原子结合。根据其结构，碳纳米管可以是导体或半导体。作为导体，碳纳米管有高的电导率。此外，碳纳米管有优良的机械强度、太拉(万亿)级的杨氏模量和高的热导率。具有这些性能的碳纳米管可以有利地用于不同的技术领域，如FED的发射器、二次电池的阴极材料、燃料电池的催化剂载体、高强度的复合材料等。
制备碳纳米管的方法的实例包括：电弧放电、激光沉积、等离子体增强的化学气相沉积(PECVD)、化学气相沉积、气相生长、电解等。气相生长适于制备松散型碳纳米管，因为它通过直接供应反应气体和催化金属到反应器中而不利用基材，合成气相的碳纳米管。电弧放电和激光沉积制备的碳纳米管的产率较低。当利用电弧放电和激光沉积时，难于控制碳纳米管的直径和长度。而且，在电弧放电和激光沉积中，除了碳纳米管外，还产生大量的无定形碳簇，因而必须进行复杂的纯化过程。
一般使用化学气相沉积法(CVD)，如热化学气相沉积、低压化学气相沉积和PECVD，以在基材上形成碳纳米管。在PECVD中，通过用等离子体活化气体，可以在低温下合成碳纳米管。在PECVD中，相对容易控制碳纳米管的直径、长度、密度等。
对于化学气相沉积(CVD)法，催化剂颗粒预先分散在用于生长碳纳米管的基材上，以在基材上形成的密度均匀的碳纳米管。
例如，韩国专利待审公开第2001-0049398号公开了一种形成多个催化剂颗粒的方法，其通过在基材上形成催化金属膜，并用蚀刻气体蚀刻所述催化金属膜。
此外，Chemical Physics Letter，vol.377 p.49，2003公开了一种在基材上形成催化剂颗粒的方法，其通过涂布催化金属前体溶液到基材上，然后干燥并热处理所涂布的催化金属前体溶液。然而，在这种情况下，在干燥和热处理的过程中，发生催化金属的重结晶和结块，因此形成在基材上的催化剂颗粒的均匀性恶化。由于形成在基材上的催化剂颗粒的均匀性恶化，在催化颗粒的基础上生长的碳纳米管的直径和生产密度的均匀性都恶化。
通过测量催化剂颗粒的颗粒尺寸的均匀度和催化剂颗粒的生产密度的均匀度，可以评价形成在基材上的催化剂颗粒的均匀性。由迄今为止已知的方法所形成的催化剂颗粒的均匀性不够。因而，需要一种形成催化剂颗粒的新方法，以改善形成在基材上的催化剂颗粒的均匀性。
发明内容
本发明提供一种以更好的均匀性在基材上形成催化剂颗粒的新方法，所述催化剂颗粒用于在其上面生长碳纳米管。
本发明还提供一种合成均匀性得到提高的碳纳米管的方法。
根据本发明的一个方面，提供一种形成催化剂颗粒的方法，所述方法包括：涂布催化金属前体溶液到基材上；冷冻干燥涂布到基材上的所述催化金属前体溶液；及还原所述冷冻干燥的催化金属前体为催化金属。
当通过冷冻干燥所述催化金属前体溶液，形成催化金属颗粒时，所述形成催化剂颗粒的方法可以使催化金属颗粒的结块和/或重结晶最小。因此，通过本发明的方法形成的催化金属颗粒具有非常高的均匀性的颗粒尺寸，并且非常均匀地分布在基材上。
根据本发明的另一个方面，提供一种制造碳纳米管的方法，所述方法包括：通过涂布催化金属前体溶液到基材上，在基材上形成催化剂颗粒，所述催化剂颗粒用于在其上面生长碳纳米管，冷冻干燥涂布到基材上的所述催化金属前体溶液，及还原所述冷冻干燥的催化金属前体为催化金属；及通过供应碳源到催化剂颗粒，在所述催化剂颗粒上生长碳纳米管。
附图说明
通过参考附图详述其示例性的实施方式，本发明的上面和其它特点和优点将变得更显而易见，附图中：
图1为根据本发明的实施例制备的用于制造碳纳米管的催化剂颗粒的光学显微照片；
图2为根据本发明的实施例制备的碳纳米管的侧视图的电子显微镜照片；
图3为根据本发明的实施例制备的碳纳米管的俯视图的电子显微镜照片；
图4为根据对比例制备的用于制造碳纳米管的催化剂颗粒的光学显微照片；
图5为图4的局部的放大图；及
图6为根据对比例制备的碳纳米管的状态的电子显微镜照片。
具体实施方式
在下文，将详述根据本发明的实施方式的一种在基材上形成催化剂颗粒的方法，所述催化剂颗粒用于在其上面生长碳纳米管。形成催化剂颗粒的方法包括：涂布催化金属前体溶液到基材上；冷冻干燥涂布到基材上的所述催化金属前体溶液；及还原所述冷冻干燥的催化金属前体为催化金属。
所述催化金属前体溶液包括催化金属前体和溶解所述催化金属前体的溶剂。
催化金属前体可以是能够转换成金属颗粒的任何物质，所述金属颗粒用于在其上面可以生长碳纳米管。所述催化金属前体的实例包括有机金属化合物。所述有机金属化合物可以包含选自下列的至少一种金属元素：Fe、Co、Ni、Y、Mo、Cu、Pt、V和Ti。有机金属化合物的实例包括乙酸亚铁、草酸铁、乙酸钴、乙酸镍、二茂络铁或其混合物。
溶剂可以是可以溶解所述催化金属前体的任何液体物质。所述溶剂的实例包括乙醇、乙二醇、聚乙二醇、聚乙烯醇及其混合物。
不特别限制在所述催化金属前体溶液中的催化金属前体的浓度。如果在所述催化金属前体溶液中的催化金属前体的浓度太低，那么在随后的制造过程中可能不会产生碳纳米管。如果在所述催化金属前体溶液中的催化金属前体的浓度太高，那么在随后的制造过程中产生的碳纳米管的直径可能增加，或者所产生的碳纳米管或碳纳米纤维的结晶度可能降低。在所述催化金属前体溶液中的催化金属前体的浓度一般可以为约10～200mM。
基材可以由在其上面能够附着催化剂颗粒的任何物质组成，例如，具有高熔点的金属如Mo、Cr和W，硅，玻璃，塑料，石英等。
涂布所述催化金属前体溶液到基材上的方法，可以是能够均匀地涂布溶液在基材的表面上的任何方法。所述方法的实例包括浸涂，蒸发镀层，丝网印刷，旋涂等。这些方法还可以组合使用。
可以将所述催化金属前体溶液涂布到基材的全部表面上或仅在基材的一部分表面上。
冷冻干燥涂布到基材上的所述催化金属前体溶液。所述冷冻干燥过程包括：冷却涂布到基材上的催化金属前体溶液到所述催化金属前体溶液的凝固点下，及减压蒸发所述催化金属前体溶液中的溶剂。
所述催化金属前体溶液的凝固点，可以依据所述催化金属前体溶液的组成变化。即，催化金属前体溶液的凝固点可以由下列因素确定：催化金属前体的类型，溶剂的类型，催化金属前体的浓度等。经过热力学计算和试差法，本领域的技术人员可以很容易地确定催化金属前体溶液的凝固点。通过调整催化金属前体溶液的组成，也可以选择催化金属前体溶液的凝固点。
利用适合于所述催化金属前体溶液的凝固点的冷却方法，可以进行冷却涂布到基材上的催化金属前体溶液到催化剂溶液的凝固点下的过程。例如，可以使用制冷器，液氮等。当使用液氮时，通过浸渍带有涂布在其上的催化金属前体溶液的基材到液氮中，可以冷却涂布到基材上的所述催化金属前体溶液到所述催化金属前体溶液的凝固点下。
在涂布到基材上的所述催化金属前体溶液冻结后，所述对基材进行减压，以使得在冻结的催化金属前体溶液中的溶剂能蒸发。例如，将带有涂布在其上的冻结的催化金属前体溶液的基材放入到真空室中，然后降低真空室内部的压力。
降低了的压力应该足够，使得在冻结的催化金属前体溶液中的溶剂能蒸发。在下文，足以使在冻结的催化金属前体溶液中的溶剂能蒸发的降低了的压力缩写为“蒸发压力”。所述蒸发压力可以依据所使用的催化金属前体溶液的组成变化。即，由催化金属前体的类型、溶剂的类型、催化金属前体的浓度、凝固点等，可以确定蒸发压力。经过热力学计算和试差法，本领域的技术人员可以容易确定催化金属前体溶液的蒸发压力。通过调整所述催化金属前体溶液的组成、凝固点等，也可以选择所述催化金属前体溶液的蒸发压力。
经过蒸发，除去在冻结的催化金属前体溶液中的溶剂。结果，催化金属前体成分在基材上形成为颗粒形式。注意到根据该方法形成的催化金属前体颗粒具有相对高的均匀性的颗粒尺寸，并均匀地分布在基材上。
接着，形成在基材上的催化金属前体颗粒还原为催化金属颗粒。例如，将催化金属前体颗粒还原为催化金属颗粒，可以按照如下的过程进行。首先，经过在氧化气氛下热处理，将催化金属前体转换成氧化物，然后在还原气氛下，热处理或等离子体处理所述氧化物，还原为金属。可以通过各种本领域已知的方法，进行还原催化金属前体的过程，因而，这里省略其详细描述。
图1为根据本发明的实施例制备的催化金属颗粒的电子显微镜照片。参考图1，催化金属颗粒均匀地分布在基材上，其颗粒尺寸相对均匀。
现在将更详细地描述根据本发明的实施方式的一种制造碳纳米管的方法。
制造碳纳米管的方法，包括：通过涂布催化金属前体溶液到基材上，在基材上形成催化剂颗粒，所述催化剂颗粒用于在其上面生长碳纳米管，冷冻干燥涂布到基材上的所述催化金属前体溶液，及还原所述冷冻干燥的催化金属前体为催化金属；及生长碳纳米管在所述催化剂颗粒上通过供应碳源到催化剂颗粒。
按照在形成催化剂颗粒的方法中所述的同样的方式，进行在基材上形成催化剂颗粒的过程。
通过供应碳源到催化剂颗粒，在所述催化剂颗粒上面生长碳纳米管的过程，可能采用用于碳纳米管的制备的各种方法进行。
例如，在所述催化剂颗粒上生长碳纳米管的过程，包括：将带有形成在其上的催化剂颗粒的基材放入到反应室中，所述催化剂颗粒用于在其上面生长碳纳米管；供应碳前体气体到所述反应室中；及分解在反应室中的所述碳前体气体，以供应碳到催化剂颗粒。
生长碳纳米管的过程可以通过下列方法进行：低压化学气相沉积、热化学气相沉积、PECVD或其组合。
碳前体气体的实例包括含碳的化合物，如乙炔、甲烷、丙烷、乙烯、一氧化碳、二氧化碳、醇及苯。
如果反应室的内部温度太低，那么所产生的碳纳米管的结晶性可能降低。如果反应室的内部温度太高，那么可能不形成碳纳米管。考虑到这点，反应室的内部温度一般可以为约450～1100℃。
在生长碳纳米管的过程中，其它条件一般可以为适于碳纳米管的生长的那些条件，本领域的技术人员容易根据具体的应用目的选择。因而，这里省略其它条件的详述。
因为在本实施方式的制造碳纳米管的方法中，碳纳米管生长在催化剂颗粒上，所述催化剂颗粒具有均匀的颗粒尺寸，并均匀地分布在基材上，所以所得的碳纳米管的均匀性也得到高度地改善。由碳纳米管的长度和直径的均匀性评价碳纳米管的均匀性。可以分别用电子显微镜和透射电子显微镜测量碳纳米管的长度和直径。
而且，由本实施方式的方法制得的碳纳米管的垂直定向特性非常好。这可以从图2的电子显微镜照片证实。图2为在本发明的实施例中制备的碳纳米管的侧视图的照片。参考图2，根据本实施方式的方法制备的碳纳米管垂直地定向，而不相互缠在一起。
图3为本发明的实施例中制备的碳纳米管的俯视图照片。参考图3，根据本实施方式的方法制备的碳纳米管的生产密度非常均匀。
实施例
利用乙醇和乙二醇作为溶剂，制得40mM乙酸亚铁溶液。将20mL的乙醇和20mL的乙二醇加入到0.1g的乙酸亚铁粉末，从而得到具有适当的粘度的溶液。将直径为20.32cm的硅基材浸渍在所得的溶液中。立即用液氮冷却所涂布的基材，然后转移到真空室中。接着，向该室中施加低于0.1mmHg的真空，以蒸发溶剂。为了使剩余溶剂的量最小化，还在100℃下加热所述基材。
在300℃下，热处理冷冻干燥的基材10分钟，以氧化乙酸亚铁。接着，在600℃下，用氢对基材进行还原处理。
结果，所述铁颗粒均匀地形成在基材上。图1为根据本实施例形成在硅基材上的铁颗粒的电子显微镜照片。参考图1，铁颗粒均匀地分布在基材上，其颗粒尺寸相对均匀。
将带有形成在其上的铁颗粒的基材放入反应室中，进行化学气相沉积(CVD)，反应室的内部温度为600℃，然后将一氧化碳和氢气的混合气体(重量比1∶2)供应到所述反应室中20分钟，从而合成基于铁颗粒的碳纳米管。
图2为在本实施例中制备的碳纳米管的侧视图照片。从图2中显而易见，在本实施例中制备的碳纳米管垂直地定向，而不相互缠在一起。图3为在本实施例中制备的碳纳米管的俯视图照片。从图3中可以看出，在本实施例中制备的碳纳米管的生产密度非常均匀。
为了评价所形成的碳纳米管的均匀性，利用电子显微镜和透射电子显微镜，分别测量在等分为9个部分的基材的各个部分上的碳纳米管的长度和直径。结果，证实在等分为9个部分的基材上的碳纳米管具有在±5％以内的均匀度。
对比例
按照与上面的实施例相同的方式合成碳纳米管，所不同的是，涂布到基材上的乙酸亚铁溶液没有进行冷冻干燥，而是自然干燥。
图4为在对比例中制备的铁颗粒的光学显微照片。图5为图4的部分的放大图。从图4和5中可以看出，在对比例中制备的铁颗粒没有均匀性。
图6为在对比例中合成的碳纳米管簇的电子显微镜照片。参考图6，在对比例中合成的碳纳米管部分地集中在基材上，相互缠在一起，并且不垂直定向。
当通过冷冻干燥催化剂金属前体溶液，形成催化剂颗粒时，根据本发明的实施方式的形成催化剂颗粒的方法，可以使催化剂颗粒的结块和/或重结晶最小。通过本实施方式的方法形成的催化剂颗粒具有非常均匀的颗粒尺寸，并非常均匀地分布在基材上。
在根据本发明的另一个实施方式的制造碳纳米管的方法中，碳纳米管生长在催化剂颗粒上面，所述催化剂颗粒具有均匀的颗粒尺寸，并均匀地分布在基材上，因而，所合成的碳纳米管具有高度改善的均匀性。
尽管已经参考其示例性的实施方式具体地描述了本发明，本领域的普通技术人员将会理解其中可以进行各种形式和细节上的变化，而不脱离如所附的权利要求书所限定的本发明的精神和范围。
Claims (6)
1.一种用于生长碳纳米管的催化剂颗粒的制备方法，该方法包括：
涂布催化金属前体溶液到基材上；
冷冻干燥涂布到基材上的催化金属前体溶液；及
还原所述冷冻干燥的催化金属前体为催化金属。
2.根据权利要求1的方法，其中所述催化金属前体为有机金属化合物。
3.根据权利要求2的方法，其中所述催化金属前体为包含至少一种选自下列的金属元素的有机金属化合物：Fe、Co、Ni、Y、Mo、Cu、Pt、V和Ti。
4.根据权利要求1的方法，其中所述催化金属前体溶液的溶剂为：乙醇、乙二醇、聚乙二醇、聚乙烯醇或其混合物。
5.根据权利要求1的方法，其中所述催化金属前体在催化金属前体溶液中的浓度为10～200mM。
6.一种制造碳纳米管的方法，该方法包括：
将催化金属前体溶液涂布到基材上，以在基材上形成用于生长碳纳米管的催化剂颗粒，冷冻干燥涂布到基材上的催化金属前体溶液，及还原所述冷冻干燥的催化金属前体为催化金属；以及
将碳源提供给所述催化剂颗粒，以在催化剂颗粒上生长碳纳米管。
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Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3049019B2 (ja) * | 1998-09-11 | 2000-06-05 | 双葉電子工業株式会社 | 単層カーボンナノチューブの皮膜を形成する方法及びその方法により皮膜を形成された単層カーボンナノチューブ |
| US20030012722A1 (en) * | 2002-07-02 | 2003-01-16 | Jie Liu | High yiel vapor phase deposition method for large scale sing walled carbon nanotube preparation |
-
2004
- 2004-06-22 KR KR1020040046552A patent/KR20050121426A/ko not_active Application Discontinuation
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2005
- 2005-06-21 CN CNA2005100794134A patent/CN1883807A/zh active Pending
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- 2005-06-22 US US11/158,047 patent/US20070020167A1/en not_active Abandoned
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101185904B (zh) * | 2007-01-18 | 2011-01-19 | 江苏工业学院 | 一种选择性液相加氢的催化剂及其制备方法及用途 |
| CN101816956A (zh) * | 2010-04-20 | 2010-09-01 | 武汉理工大学 | 一种提高纳米金属颗粒在石墨化碳载体表面分散的方法 |
| CN101816956B (zh) * | 2010-04-20 | 2011-10-19 | 武汉理工大学 | 一种提高纳米金属颗粒在石墨化碳载体表面分散的方法 |
Also Published As
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| JP2006007213A (ja) | 2006-01-12 |
| KR20050121426A (ko) | 2005-12-27 |
| US20070020167A1 (en) | 2007-01-25 |
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