Nanomaterials and nanostructures have received steadily growing interests as a result of their peculiar and fascinating properties and applications. Neodymia-silica nanocomposites were prepared by sol-gel route followed by calcination. The samples were prepared with different concentration of dopant (Nd2O3) and calcined in a programmable furnace at 1000 °C for 5 h. The structural evolution of samples was investigated by employing techniques such as XRD, FTIR and TEM. X-ray diffraction patterns showed that the samples were nanocrystalline and the size of crystallites has been determined using Debye-Scherrer relation. The FTIR spectra confirmed the presence of functional groups of prepared material. The particle size of samples was also estimated through TEM analysis. It has been observed that crystallinity as well as particle size of the samples increases with increase in dopant concentration.