Multilayered graphene nanoplatelets (MLGs) were prepared from thermally expanded graphite flakes using an electrochemical technique. Morphological characterization of MLGs was performed using scanning electron microscopy (SEM), X-ray diffraction analysis (XRD), Raman spectroscopy (RS), and the Brunauer–Emmett–Teller (BET) method. DGEBA-epoxy-based nanocomposites filled with synthesized MLGs were studied using Static Mechanical Loading (SML), Thermal Desorption Mass Spectroscopy (TDMS), Broad-Band Dielectric Spectroscopy (BDS), and Positron Annihilation Lifetime Spectroscopy (PALS). The mass loading of the MLGs in the nanocomposites was varied between 0.0, 0.1, 0.2, 0.5, and 1% in the case of the SML study and 0.0, 1.0, 2, and 5% for the other measurements. Enhancements in the compression strength and the Young’s modulus were obtained at extremely low loadings ($C\le$ 0.01%). An essential increase in thermal stability and a decrease in destruction activation energy were observed at $C\le$ 5%. Both the dielectric permittivity (${\epsilon }_1$) and the dielectric loss factor (${\epsilon }_2$) increased with increasing $C$ over the entire frequency region tested (4 Hz–8 MHz). Increased ${\epsilon }_2$ is correlated with decreased free volume when increasing $C$. Physical mechanisms of MLG–epoxy interactions underlying the effects observed are discussed.

Viscose-derived carbon fibers (VDCFs) are lightweight and flexible textile materials with strong potential for electromagnetic interference (EMI) shielding; however, their performance is governed by surface chemistry. This study aims to tailor the functional properties of VDCFs via process-driven sulfurization. The fibers were treated with sulfur vapor at 400–800 °C under argon, followed by rapid quenching, enabling controlled sulfur incorporation (0.5–12 mmol g⁻¹). Structural and chemical analyses (XRD, SEM–EDS, ATR–FTIR, and TPD–MS) revealed temperature-dependent sulfur incorporation and evolution of sulfur-containing surface functionalities. Sulfurization at 400–500 °C favored the formation of thermally labile sulfur species, tentatively assigned to mercapto-, sulfide-, and polysulfide-type groups, whereas higher treatment temperatures promoted more thermally stable sulfur-containing functionalities associated with the carbon framework. Two desorption regimes (120–250 °C and 250–500 °C) indicate the coexistence of weakly and strongly bound sulfur species. Importantly, sulfurization preserved fibrous morphology while increasing surface roughness and defect density, enhancing interfacial activity. The treatment temperature was identified as the key factor controlling sulfur loading and distribution, with sulfur content continuing to decrease above 600 °C, albeit at a reduced rate. Electromagnetic characterization in the X-band (8–12 GHz) showed a transition toward reflection-dominated EMI shielding, with reflectivity increasing from 87% for pristine fibers to 94–95% for sulfurized samples at 10 GHz, accompanied by corresponding decreases in transmission and absorption. These results demonstrate a clear processing–structure–property relationship and highlight sulfur-functionalized VDCFs as efficient textile components for EMI shielding.