Abstract Sugar gourd shaped CeF 3 :Tb 3+ has been successfully synthesized by polyol method. The phase, morphology and fluorescent properties of CeF 3 :Tb 3+ were characterized by X‐ray diffraction (XRD), transmission electron microscopy (TEM), infrared spectroscopy (IR) and photoluminescence (PL) spectra, respectively. It can be seen that the volume changes of giethylene glycol (DEG) and H 2 O content did not affect the phase structure of CeF 3 :Tb 3+ . The emission spectrum of CeF 3 :Tb 3+ shows the characteristic emissions of Tb 3+ ion, indicating that an energy transfer from Ce 3+ to Tb 3+ occurs in CeF 3 :Tb 3+ , and the decay time of CeF 3 :Tb 3+ was not affected by the change of DEG content.