The present article reports the synthesis of copper, nickel and iron-based metal oxide nanocomposites by sol-gel method using disproportion of Cu(II) and Fe(III) in basic media. The synthesized nanocomposites were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Raman spectroscopy (RS), differential scanning calorimetery (DSC)/thermogravemetric analysis (TGA), field-emission scanning electron microscope (FE-SEM), high-resolution transmission electron microscope (HR-TEM) and vibrating sample magnetometer (VSM). The XRD patterns of nanocomposites confirm the presence of spinel, CuO and FeO phases. The particle size of the nanocomposite has been calculated using HR-TEM micrographs and found to be in the range of 10-120 nm. The magnetic properties of nanocomposites were measured at room temperature. The values of saturation magnetization (Ms) and remanent magnetization (Mr) were increasing with increase of iron concentration. (C) 2009 Elsevier B.V. All rights reserved.