采用液相注入的化学气相流催化反应,在乙醇为碳源和二茂铁为催化剂的反应系统中加入微量的水,在氩气流中高产率合成出具有氧化基表面、高结晶度和大内管径的多壁碳纳米管。此方法合成的碳管可高浓度分散于乙醇、苯、甲苯、二甲苯、正己烷等有机溶剂中。高分辨电镜观察碳管端部呈开口状,碳管表层部分有缺陷,但管内碳层完整、排列整齐、呈高度结晶态。光电子能谱(XPS)分析测得碳管表面有碳氧键。由此可知,在反应系统中加入微量的水一方面活化了催化剂、提高了碳管产率,另一方面产生了氧化的碳管表面。对碳管进行氧化处理获得可分散纳米碳管是实现其众多应用的关键步骤,常规采用酸处理氧化或热氧化等后续处理方法,但这些处理常常导致破坏结晶性,降低材料性能。本工作采用一步法高产率合成出具有氧功能化表面的、可分散、高结晶度的碳纳米管,这对碳管的制备及相关应用具有重要意义。
Introduction a small amount of water into the reactions system of ethanol and ferrocene in the solvent injection catalytic chemical vapor reactions yielded surface oxidized,highly crystallized and large hollow size multiple walled carbon nanotubes in argon flow.The nanotubes thus produced is dispersible in organic solvents like ethanol,benzene,toluene and xylene.High resolution transmission electronic microscopy observation revealed the existence of defects in the surface graphite layers of the nanotubes,but the inner graphite layers were well aligned and highly crystallized structures.X-ray photoelectronic spectrum(XPS) analysis detected the existence of carbon-oxygen bonds.Therefore,the water added not only activated the catalysts,increased the nanotube yield,but also oxidized the surface of the nanotubes.Oxidization processing of carbon nanotubes to dispersible materials is the key step towards their applications.This was previous done by post-processing nanotubes such as strong acid oxidizing or thermal oxidizing,which however,resulted in structural damage of the materials,hence degrading their properties.The present synthesis enables one-step yield of the surface oxidized and dispersible nanotubes which is of significance to their processing and the relevant applications.