Chemical functionalization of helical carbon nanotubes: influence of sonication time and concentrations of sulfuric and nitric acids with 3:1 mixing ratio

Abstract

Carbon nanotubes (CNTs) with straight geometries have been widely studied for various engineering applications, and they are often treated or functionalized to improve their effectiveness, depending on their role and expected performance. However, helical configurations of CNTs (HCNTs) have not been sufficiently investigated, especially in their functionalized states for high-performance nanocomposite applications. The coil-shaped geometry of these HCNTs increases the mechanical entanglement of these nanotubes with a host resin system when they are used as reinforcements. This consequently has the potential to improve the mechanical, thermal, electrical, and magnetic properties of the polymeric matrix systems. A uniform dispersion of CNTs in the resin plays an important role in obtaining improved and consistent properties in the final nanocomposite part. To improve the homogeneous dispersion (individual suspension) of these nanotubes in the host resin and to enhance their interactions/bonds with the resin molecules, the surface of these nanotubes should be modified. This study investigates a sonication method for chemical functionalization of HCNTs using a mixture of sulfuric and nitric acids with 3 to 1 mixing ratio [3 : 1], and it evaluates the effects of acid concentrations and sonication time on the severity of the functionalization process. To evaluate the effectiveness of the process parameters, the functionalized HCNTs (FHCNTs) were examined using several characterization instruments and techniques such as Scanning Electron Microscopy (SEM), Fourier Transform Infrared (FTIR), X-ray Diffraction (XRD), visual dispersion test, and Raman spectroscopy. The characterization results confirmed that the changes in process parameters were mostly effective and the atomic structures of the functionalized HCNTs were successfully altered. All FHCNT samples demonstrated higher dispersion uniformity, increase in Raman ID/IG ratios, and changes in the FTIR spectra compared to the pristine HCNTs. Most of the FHCNTs had a reduction in crystallinity, which was consistent with our expectation that functionalization generates more defects on the surface structure of HCNTs, thus leading to a lower intensity of the graphitic peak. The largest reduction in crystallinity was seen for HCNTs treated with a 16 molarity acidic solution; therefore, the HCNTs that were treated with lower molarity acids could be used for further studies and explored for their effective applications in improving the mechanical, thermal, and electrical properties of polymeric nanocomposites.