In this study, synthesis and characterization of new potential high-energy materials based on fullerene soot nanoparticles and nitroaryl diazonium ions were reported. Synthesis was carried out using reaction of fullerene soot with nitroaryl diazonium ions in acetonitrile or solvent free under thermal or microwave-assisted conditions. The nitroaryl diazonium ions were prepared insitu using reactions of 2-nitroaniline, 4-nitroaniline and 2,4-dinitroaniline with isoamyl nitrite. The spectroscopic and instrumental analytical methods such as Fourier transform infrared (FT-IR), Raman, ultraviolet–visible (UV–Vis), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray (EDX), elemental map and thermogravimetric analysis (TGA) were used to characterize the fullerene soot functionalized with nitroaryl groups. The differential thermal analysis (DTA) was applied to verify the energy releasing property of these compounds. The obtained results clearly confirmed the successful functionalization of fullerene soot nanoparticles by nitroaryl diazonium ions.