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Antimony-doped tin oxide powders were prepared using different routes and annealing conditions. The influence of preparation on the distribution of antimony in the powders was studied and correlated with the electrical properties of the powders. A model of doped SnO 2 powder that allows the bulk concentration of the doping element to be calculated from the XPS results is proposed. The doping after crystallization of SnO 2 leads to a very strong surface segregation that is proved by x-ray photoelectron spectroscopy. Antimony is incorporated at the largest concentration in the tin oxide lattice when it is added during the formation of stannic acid. The annealing temperature plays an important role in the antimony distribution. The lower the temperature, the smaller the crystallite size and the lower the incorporation of antimony in the lattice of SnO 2 . A strong correlation between bulk concentration and electrical and morphological properties was found.