The purification of HiPco SWCNTs with liquid bromine at room temperature

Abstract

A new procedure to purify HiPco single-walled carbon nanotubes (SWCNTs) from iron catalyst impurity is introduced. The protocol, which uses liquid bromine at room temperature (RT) as an oxidant, improves nanotube purity from iron by a factor of approximately 10, while maintaining good nanotube integrity as demonstrated by near infrared (NIR) luminescence and absorbance measurements. When HiPco SWCNTs are dissolved in RT Br 2(l) (free of O 2 and H 2O), the metallic iron impurity is quickly oxidized to its bromide salt and easily removed by aqueous washing or by washing with dilute acid. The iron content (by ICP-AE) for the purified SWCNT material was 2.8–3.6% by weight (for three different samples) for a single purification step, but could be lowered to 1.6–1.8% with an additional purification cycle. Characterization of the resulting purified SWCNT material has been achieved by TEM imaging, XPS, ICP-AE analysis, Raman spectroscopy, electronic absorption spectroscopy, and by NIR photoluminescence measurements. Finally, the new Br 2(l) purification procedure has been compared to and contrasted with other established purification procedures for HiPco SWCNTs and found to be a highly desirable alternative.