A series of Ge4+‐doped TiO2 is synthesized by a sol–gel method and annealed at different temperatures. The doping mechanism of Ge was studied via XRD, Raman spectroscopy, XPS, and HRTEM techniques. The doping behavior of introduced Ge4+ ions is related to the doping concentration and annealing temperature. It is revealed that the Ge4+ ions would exist as doped Ge ions in substitutional mode and GeO2 on surface. At certain concentration, the substitutional‐doped Ge ions are transferred to GeO2 on surface with the increase of annealing temperature. The introduction of Ge4+ ions inhibited the formation of the rutile phase of TiO2 and delayed the phase transition.
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