Effect of surface-active substances on the macrodispersion behavior of thermal stress-modified multi-wall carbon nanotubes in cryogenic environments

In the preparation of nanocomposites, the agglomeration of multi-walled carbon nanotubes (MWCNTs) in the composite due to their low colloidal stability limits their use in industrial areas. To overcome these problems, it is important to develop simpler, economical, high-yield and non-hazardous techniques to replace existing techniques with low yields, expensive additional equipment or hazardous liquids. This study explores how surfactants affect the macrodispersion of thermal stress-modified MWCNTs in cryogenic environments, focusing on their application in polymer film preparation. Firstly, optimal conditions for modifying MWCNTs through thermal stress were identified using liquid nitrogen. Parameters assessed included the number of cycles (2, 4, and 6), duration in liquid nitrogen (10, 20, and 30 min), and subsequent waiting time at room temperature (5, 12, and 20 min). Results showed that the highest surface area was obtained with 2 cycles, 20 min in liquid nitrogen, and 5 min at room temperature. Analytical techniques such as Brunauer-Emmett-Teller (BET), X-Ray Diffraction (XRD), High Contrast Transmission Electron Microscopy (CTEM) and Raman spectroscopy were used to evaluate the functionalization process's effects on MWCNTs' internal graphitic structure and physicochemical properties. CTEM micrographs indicated that thermal stress reduced the length of MWCNTs, while Raman analysis showed improved graphite quality. The modification process, carried out with 100 % efficiency and no sample loss, increased the BET surface area from 297.551 m²/g to 397.295 m²/g. The study also investigated the impact of surfactants (polyethylene glycol sorbitan monooleate-Tween 80, sodium dodecyl sulfate-SDS, and hexadecyltrimethylammonium bromide-CTAB) on MWCNTs' macrodispersion degrees (DM%) and energy band gaps via UV–visible (UV–Vis) absorption spectroscopy. CTAB provided the highest and most stable macrodispersion, reducing the energy band gaps of MWCNTs from 5.65–5.75 eV to 3.53–3.60 eV. CTAB showed excellent colloidal stability with a zeta potential of 44.2 mV, while SDS had −49.9 mV. Polyvinyl alcohol (PVA) polymer films, created using MWCNT solutions with optimal macrodispersion, were confirmed by Scanning Electron Microscope (SEM), Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimeters (DSC), and BET surface area analyses to have successfully and homogeneously incorporated MWCNTs. In addition to the superior properties of MWCNTs modified with the functionalization technique developed within the scope of this study by increasing their specific surface area and porosity, the excellent colloidal stability provided may have various effects in many industrial areas. These advantages enable MWCNTs functionalized with the developed technique to have a wider range of applications in industrial applications and provide more efficient and sustainable solutions.