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Tm3+ ions doped β-PbF2 nanocrystals in oxyfluoride glass ceramics with different doping concentrations and thermal temperatures are prepared by a traditional melt-quenching and thermal treatment method to investigate the structure and the phase transition of Tm3+ doped nanocrystals. The structures are characterized by X-ray diffraction Rietveld analysis and confirmed with numerical simulation. The phase transitions are proved further by the emission spectra. Both of the doping concentration and thermal temperature can induce an Oh to D4h site symmetry distortion and a cubic to tetragonal phase transition. The luminescence of Tm3+ doped nanocrystals at 800 nm was modulated by the phase transition of the surrounding crystal field.