Chemical oxidation of multiwalled carbon nanotubes

• Published in: Carbon (New York) 2008-05, Vol.46 (6), p.833-840
• Main Authors: Datsyuk, V., Kalyva, M., Papagelis, K., Parthenios, J., Tasis, D., Siokou, A., Kallitsis, I., Galiotis, C.
• Format: Article
• Language: English
• Subjects: Cross-disciplinary physics: materials science; rheology; Exact sciences and technology; Fullerenes and related materials; diamonds, graphite; Materials science; Physics; Specific materials
• ISSN: 0008-6223; 1873-3891
• DOI: 10.1016/j.carbon.2008.02.012

The effect of oxidation on the structural integrity of multiwalled carbon nanotubes through acidic (nitric acid and a mixture of sulfuric acid and hydrogen peroxide) and basic (ammonium hydroxide/hydrogen peroxide) agents has been studied. In order to purify the as-received material, a non-oxidative treatment (with hydrochloric acid) was also applied. Electron microscopy and thermogravimetric analysis clearly revealed that the nitric acid-treated material under reflux conditions suffered the highest degree of degradation, such as, nanotube shortening and additional defect generation in the graphitic network. Basic oxidative treatment led to the complete removal of amorphous carbon and metal oxide impurities but the structural integrity was found to be intact. X-ray photoelectron spectroscopy was employed to confirm the different functionalities produced for each oxidation agent, whereas titration measurements determined the relative concentration of carboxylic functions onto the graphitic surface. Moreover, a general relationship between the chemical treatment and the amount of non-graphitic carbon was established by means of Raman spectroscopy measurements. The possibility of controlling the required amount of functionality, carboxylic and hydroxyl, via these oxidation procedures is discussed.