摘要:本文对多孔壁碳纳米笼的提纯进行了研究。使用不同种类酸对其酸洗再过滤提纯,通过透射电镜、X 射线粉末衍射等测试,观察其形貌和结构变化及计算失重率得出最好的酸洗提纯方法。由于石墨层包覆了铁质内核,阻止了酸与铁质内核接触,增大了其被酸洗出去的难度,导致在使用单一酸进行酸洗时,铁质内核未被除去。在本试验中,使用混合酸是一种有效提纯方法,其增强了氧化性,比起单一酸洗,破坏了更多碳纳米笼的石墨壁,从而使绝大多数的铁质内核与酸反应,提高了碳纳米笼提纯的效率,尽管碳纳米笼结构遭到破坏。另一种有效提纯方法是利用其磁性除去浓盐酸酸洗后残余的铁质杂质,也能获得石墨壁完整的纯碳纳米笼,但是,磁性提纯的失重率较混合酸提纯的失重率高很多,提纯效率低。5434
关键字:碳纳米笼;提纯;酸洗;磁分离
An Investigation on the Purification of the Carbon Nanocages with Porous Shells
Abstract: Methods for purifying carbon nanocages (CNCs) with porous shells have been investigated. To find out the best method for purification, the changes of the CNCs’ structure and morphology were observed by transmission electron microscope and X-ray diffraction after different purifications, and their weight loss was also calculated. Because of being encapsulated by graphitic shells, the ferrous cores can’t completely touch acid solution leading to an incomplete purification by the single acid treatment. According to our results, the mixed acid treatment is an efficient method to purify the samples. The mixed acids can strongly oxidizing the graphitic shells for exposing the ferrous cores to the acid to remove them, compared with single acid treatments. Thus, this method is an efficient one, despite of violent damage of graphitic shells. The other effective purification method is removal of ferrous cores by an additional magnet after the sample is treated in HCl to get CNCs with intact graphitic shells. However, the methods is not efficient, as its weight loss is quite high.
Keywords: Carbon nanocages; Purification; Acid-treatment; Magnetic separation
目录
1 文献综述 1
1.1 研究背景 1
1.2 碳纳米材料的应用前景 3
1.3 本课题研究目的和意义 6
2 实验部分 9
2.1 实验原料 9
2.2 实验设备 9
2.3 实验装置 9
2.4.1 多孔壁碳纳米笼的制备 10
2.4.2 多孔壁纳米笼的盐酸提纯 10
2.4.3 多孔壁碳纳米笼的硝酸提纯 11
2.4.4 多孔壁碳纳米笼的王水提纯 11
2.4.5 多孔壁纳米笼的磁分离 11
2.5 样品表征 11
2.5.1 透射电镜(Transmission electron microscopy, TEM) 11
2.5.2 X射线衍射(X-ray Diffraction,XRD) 12
3 结果与讨论 13
3.1 多孔壁碳纳米笼原始样品分析 13
3.2 不同工艺对多孔壁碳纳米笼提纯的影响 14
3.2.1 浓盐酸酸洗 15
3.2.2 浓硝酸酸洗 16
3.2.3 王水酸洗 17
3.3 磁分离对多孔壁碳纳米笼提纯的影响 19
4 结论 23
致谢 24
参考文献 25
1.3 本课题研究目的和意义
碳纳米笼的提纯方法很多种,大体上与碳纳米管的提纯方法相似,分为物理方法和化学方法两种。物理方法主要以离心分离法,电泳纯化法,空间排阻色谱法为主。
离心分离法的基本原理就在于,由于碳纳米笼比超细石墨微粒、碳纳米颗粒和无定形碳等杂质的粒度大,所以离心分离时,碳纳米笼先沉积下来,而粒度较小的单壁碳纳米笼、碳纳米颗粒、超细石墨粒子却悬浮在溶液之中,将悬浮液在加压或者超声振荡的协助下通过微孔过滤膜,就可以将粒度小于微孔过滤膜孔径的杂质粒子除去。当离心速度达到 15000r/min 时,直径小于 50nm的杂质颗粒也基本能沉淀下来,而大部分的 SWNTs 仍存在于悬浮液中,这样分离出来的 SWNTs 的纯度可以达到40%~70%。离心分离法的基本原理直观、操作简单,缺点是要么回收率较低,要么产物纯度不够高。 多孔壁碳纳米笼的提纯研究:http://www.youerw.com/cailiao/lunwen_2455.html