Due to its magnetic, electrical, absorption, and emission properties, nanoscale gadolinium oxide is widely used in various fields. In this research, nanocrystalline Gd 2 O 3 powders and films on glass substrates have been produced by the extraction-pyrolytic method. X-ray diffraction analysis revealed the formation of single phase Gd 2 O 3 with cubic crystal structure and the mean crystallite size from 9 to 25 nm in all produced materials. The morphology of samples has been characterized by scanning electron microscopy and transmission electron microscopy.