Carbon nanohybrid material (CNF/ -Fe 2 O 3 ) was obtained via a modified sol-gel technique consisting of two steps: functionalization of carbon nanofibers (CNF) in H 2 SO 4 /HNO 3 followed by synthesis using Fe(NO 3 ) 3 •9H 2 O. As a result, the iron content of the CNF/ -Fe 2 O 3 was increased by more than twice from about 40% to about 87% mass percent, compared to the pristine CNF and oxidized CNF specimens, as proved by energy dispersive X-ray fluorescence. Scanning electron microscopy images exhibited "cumulus" on the CNF/ -Fe 2 O 3 specimen surface, which showed the highest iron mass percentage, proved by energy dispersive X-ray spectroscopy. Transmission electron microscopy images confirmed attachment of -Fe 2 O 3 cumulus to the inner and outer surfaces of the CNF walls after synthesis. The characteristic peaks of Fe 2p 3/2 and Fe 2p 1/2 appeared in the XPS spectra obtained on CNF/ -Fe 2 O 3 . In addition, X-ray diffraction (XRD) results indicated formation of -Fe 2 O 3 during the synthesis process. The Raman spectrum of the CNF/ -Fe 2 O 3 sample displays peaks with positions close to characteristic peaks of highly crystalline and monodisperse maghemite nanocrystallites. The synthesis of CNF/ -Fe 2 O 3 leads to an increase in the hydrophilicity of CNF and magnetic properties at room temperature.