Temperature effects on the nitric acid oxidation of industrial grade multiwalled carbon nanotubes

In this study, we report an oxidative treatment of multiwalled carbon nanotubes (MWCNTs) by using nitric acid at different temperatures (25–175 °C). The analyzed materials have diameters varying from 10 to 40 nm and majority lengths between 3 and 6 μm. The characterization results obtained by different techniques (e.g., field emission scanning electron microscopy, thermogravimetric analysis, energy-filtered transmission electron microscopy, Braunauer, Emmet and Teller method, ζ-potential and confocal Raman spectroscopy) allowed us to access the effects of temperature treatment on the relevant physico-chemical properties of the MWCNTs samples studied in view of an integrated perspective to use these samples in a bio-toxicological context. Analytical microbalance measurements were used to access the purity of samples (metallic residue) after thermogravimetric analysis. Confocal Raman spectroscopy measurements were used to evaluate the density of structural defects created on the surface of the tubes due to the oxidation process by using 2D Raman image. Finally, we have demonstrated that temperature is an important parameter in the generation of oxidation debris (a byproduct which has not been properly taken into account in the literature) in the industrial grade MWCNTs studied after nitric acid purification and functionalization.