Estimation of the number of cross-links of multi-walled carbon nanotube films formed by a dehydration condensation reaction

Preparation procedure of multi-walled carbon nanotube (MWCNT) films shows as follows. First, as-grown MWCNTs heated in the air and treated with hydrochloric acid to remove amorphous carbon and catalytic metal particles respectively. Then, the o1btained MWCNT samples were treated with nitric acid at 373K to add carboxylic acid and hydroxyl groups on their surface. Finally, MWCNT films were prepared by employing a condensation reaction utilizing 1,3-dicyclohexylcarbodiimide (DCC) to cross-link each MWCNT with chemical bonds. Morphological changes in the resultant MWCNT films were monitored using scanning electron microscopy, and showed that the MWCNTs were randomly intertwined in the films. The prepared MWCNT films were 17mm in diameter and 20μm in thickness, and the apparent density was 0.59 g/cm³. Fourier transform-infrared spectroscopy confirmed that each MWCNT modified with carboxylic acid and hydroxyl groups was cross-linked through the ester bond. It was found that the ratio of the number of ester cross-links and carbon atoms of the nanotubes per unit apparent volume (cm³) of condensed-MWCNT films was 5.23×10^-3 using TGA. The tensile strength and Vickers hardness of condensed-MWCNT films achieved an average of 15MPa and 9.2MPa, respectively, and was greater than those of free-standing MWCNT films without ester bond.