多壁碳纳米管的纯化及其表面含氧基团的表征

Purification of Multiwalled Carbon Nanotubes and Characterization of Their Oxygen-Containing Surface Groups

用兼具酸性和氧化性的HNO3水溶液可方便地除去残留在原生态多壁碳纳米管(CNT)上的Ni-MgO催化剂组分,同时在其表面产生某些含氧官能团,使原生态多壁碳纳米管的疏水性表面变为亲水性表面.采用Boehm中和滴定法以及X射线衍射(XRD)、热脱附谱(TPD)、傅里叶变换红外(FTIR)光谱和X射线光电子能谱(XPS)等技术对HNO3处理过的多壁碳纳米管的相组成和表面含氧官能团进行测量和表征.结果表明:所生成表面含氧官能团的总量以经7.0mol·L-1硝酸378K处理24h的CNT为最高;3种主要表面含氧官能团的含量高低顺序为,羧基>内酯型羧基>酚型羟基.

We conveniently removed the Ni-MgO catalyst components from an as-grown multiwalled carbon nanotube （CNT） using an aqueous HNO3 solution with strong acidity and oxidizability as a purifying reagent. Some oxygen-containing surface groups were generated at the CNT surface, which converted the hydrophobic surface into a hydrophilic surface. The phase composition and the oxygen-containing surface groups of the CNTs treated by nitric acid were determined and characterized using Boehm′ s neutralizing titration method and X-ray powder diffraction （XRD）, temperature-programmed desorption （TPD）, Fourier transform infrared （FTIR） spectroscopy, and X-ray photoelectron spectroscopy （XPS） techniques. The results indicated that the total content of the formed oxygen-containing surface groups was the highest for the CNTs treated with 7.0 mol·L-1 aqueous HNO3 at 378 K for 24 h. The content of the three major oxygen-containing surface groups was： carboxyllactonic carboxylphenolic hydroxyl.