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Pr3+/Yb3+ co-doped different morphology hexagonal NaLuF4(β-NaLuF4)microcrystals(MCs)were synthesized via a hydrothermal method by tuning PH values.The samples were used to characterize by XRD,SEM and PL spectra.Pr3+ ions have very good luminescence properties and a wide range of applications.However,there is little research of Pr3+/Yb3+doped β-NaLuF4.