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A series of nanocrystalline SnO2 powders, doped with different Sb contents, were synthesized by route of alkoxides hydrolysis using SnCl4·5H2O and SbCl3 as starting materials and calcined at different temperatures. The microstructure and morphology of samples are investigated by XRD and TEM, the valence state changes of Sb in SnO2 crystal lattice is detected by M(O)ssbauer spectroscopy and XPS.The resistivity of powders is examined with a mould of inside diameter d=10mm at a constant pressure. The results show that lightly-doping Sb is effective means of semiconducting of nanocrystalline SnO2. The ratio of Sb5+ to Sb3+ decreases with increasing Sb content in SnO2 crystal lattices and calcination temperature. The XPS diffraction confirms the same result as Mssbauer spectroscopy.