Nanocomposites of ferrite and ferroelectric phases are attractive functional ceramic materials. In this work, the nanocomposite Ni 1-x Co x Fe 2 O 4 -BaTiO 3 (x = 0.2, 0.3, 0.4, 0.5) fibers with fine diameters of 3 * 7 lm and high aspect ratios were synthesized by the organic gelthermal decomposition process from the raw materials of citric acid and metal salts. The structure, thermal decomposition process and morphologies of the gel precursors and the resultant fibers derived from thermal decomposition of the gel precursors were characterized by Fourier transform infrared spectroscopy, thermogravimetric differential thermal analysis, X-ray diffraction and scanning electron microscopy. The magnetic properties of the nanocomposite fibers were measured by vibrating sample magnetometer.