Iron-doped SnO 2 nanoparticles with chemical formula Sn 1−x Fe x O 2−y (x = 0.02, 0.05 and 0.10 at%) were successfully produced by a proteic sol-gel method. Thermogravimetric analysis and differential scanning calorimetry were performed to investigate the thermal behavior of the precursor powders as well as to select the appropriate calcination temperatures for oxide formation. X-ray absorption near-edge spectroscopy studies were carried out to determine the valence state of the transition metal used as dopant. Structural, morphological, and optical properties of the synthesized materials were studied by X-ray diffraction, Mössbauer spectroscopy, transmission electron microscopy, Fourier-transform infrared spectroscopy, and ultraviolet-visible spectroscopy. The results confirmed the formation of M. S. Pereira ( ) • C.