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电热法液态气相催化制备碳纳米管的研究
Electo-thermal Gaseous Catalysis in Liquid Phase Synthesis of Carbon Nanotubes
【作者】 李锐;
【导师】 杨骥;
【作者基本信息】 上海交通大学 , 环境工程, 2011, 硕士
【摘要】 碳纳米管优异的物理化学性能使其拥有广泛的应用前景,其制备工艺的研究得到了广泛的关注,传统碳纳米管制备方法工艺成熟,应用广泛,但或多或少的存在一些缺陷,如成本较高,对制备条件要求较高,实验设备复杂等,因此,探寻一些制备方法简单,成本低廉及环境友好的碳纳米管制备工艺成为碳纳米管制备的发展方向。本文尝试并开发了一种设备简单,成本低廉,操作简单,环境友好的碳纳米管制备工艺,该工艺的特征如下:构造一个基底,并在基底上构造出一种金属元素作为催化剂,使金属催化剂在基底上形成一层薄膜或细小颗粒,将载有催化剂的基底置于含有碳氢化合物的溶液中,利用直流电源将基底加热至预定温度,使基底周围的液体逐渐处于紊动状态并在基底表面有气泡产生,并使基底的表面产生一层气态薄膜,从而构造出碳纳米管生长的条件。该方法中选择硅片作为基地,Fe作为金属催化剂。利用该工艺尝试使用碳氢化合物作为碳源对碳纳米管进行制备,考察该工艺的可行性,并寻找利用该工艺制备碳纳米管的最佳参数,通过对可行性的考察和参数的研究,利用该方法的最佳参数尝试能否利用工业排放的高浓度有机废水制备碳纳米管。具体研究工作如下:1.尝试以乙醇作为碳源,利用SEM和TEM考察和验证利用本文所述的方法能否进行碳纳米管的制备。研究结果表明,反应时间1h就会有碳纳米管的生成,并且碳纳米管形貌多样,数量丰富,证明该法制备碳纳米管的可行性。2.尝试在无水乙醇中引入水作为碳源,利用本文叙述的方法制备碳纳米管,通过SEM和TEM观察表明,可以生成形状多样的碳纳米管,证明加水后该方法仍具备制备多种形态碳纳米管的能力;通过对引入水量的考察后发现,碳源溶液中引入水后,水对碳纳米管的生长具有双重作用,水量太多或太少都会影响所得碳纳米管的产率,在适量水量的参与下,碳纳米管的生长状况可以达到最佳。水量过小,催化剂容易较快失活,碳纳米管高速生长时间短,产率受限;水量过大,一方面碳源浓度不足使碳纳米管生长速度降低,另一方面水还会消耗部份已经生成的碳纳米管,也不利于碳纳米管的生长。3.尝试在碳源中酸碱度,考察对碳纳米管生长的影响,发现加入酸度后,会阻碍碳纳米管的生长,并且对碳纳米管的生长影响很大;而加入碱度以后对碳纳米管的产量影响不大,仍可使碳纳米管大量生长并可以产生多种形态的碳纳米管。4.尝试多种碳氢化合物混合物作为碳源,并考察碳纳米管的生长状况,利用乙醇与乙二醇乙醚乙酸酯配比溶液作为碳源,可以生成数量众多的碳纳米管,且生成的碳管形状多样,可以证明利用多种碳氢化合物的混合物作为碳源可以制备出碳纳米管。5.尝试利用现场废水作为碳源制备碳纳米管,考察实验的可行性,最终没有得到理想的效果,分析其主要原因可能为选择的废水含水率较高且含水率难以降低。
【Abstract】 Carbon nanotubes(CNTs) has excellent properties and wide potential application.The investigation on CNTs has become a hot topic in the world. Some low cost,easy-to-operate and environmentally friendly methods has been explored for several years.In this paper,a low cost,easy-to-operate and environmentally friendly method has been developed for synthesis of carbon nanotubes by simply electro-thermal heating a substrate in organic liquids.We used Si as the substrates covered with a thin(about 5nm) Fe film.This substrates were electrically heated to the expected temperature in organic liquid.The carbon nanotubes were grown on the substrates by using hydrocarbon such as ethanol.We studied the effect of using hydrocarbon in this methods,and inspects the feasibility of this methods,and sought the optimum parameter.Then,we tried to use the organic wates water as the carbon source to synthesize carbon nanotubes by this methods.The main researches in this paper are as follows: 1.We used ethanol as the carbon source by our methods to synthesize the carbon nanotubes. The results by SEM and TEM showed that the CNTs were grown in just one hour, and the sample consists a great deal of nanotubes.It fully proved the feasibility of the method in this paper.2.Water was introduced into the carbon nanotubes growth reaction to study the effect of water on the carbon nanotubes.The sample was characterized by SEM and TEM.The results showed that,the CNTs synthesized from the suitable amount of water was outstanding,too much or too little water both affected the CNTs yield.3. Acid-Base was introduced into the carbon source to study the effect of acid-base on the CNTs.The results by SEM and TEM showed that,with adding suitable alkalinity,CNTs yield can have a increase in the contrast of acidity.4. We used other hydrocarbon as the carbon source and studied the effect to carbon nanotubes growth reaction.The results showed that a variety of hydrocarbon had the feasibility to synthesize the CNTs.5.We tried to used the organic waste water as the carbon source to synthesize the CNTs,but we failed as the result.The main reason may be the organic waste water contains too much water.