The present work is aimed to compare the physical properties of (x = 0, and 0.05) nanopowders obtained by sol–gel method, mechanochemical alloying, and mechanochemical alloying followed by thermal treatment. The X-ray diffraction of samples prepared by sol–gel showed peaks due to the cassiterite phase of SnO2 and thier Mössbauer spectra showed ferromagnetic and paramagnetic signals. The samples obtained by the milling process of SnO2 mixed with -Fe showed Bragg peaks due to SnO2 (rutile) with a line broadening caused by the reduction of grain sizes and the presence of microstrains. Mössbauer spectra for these samples revealed the presence of Fe3 + as well as unreacted -Fe. In the case of mechanochemical alloying with thermal treatment, the incorporation of Fe3 + in the SnO2 structure with the presence of impurities was observed.