Abstract: GdB3O6 is a very good host luminescentmaterial; its advantages of excellent luminescent, stable physiochemical andthe non-toxic and non-radioactive properties have attracted more and morepeople’s attention, and so the simple and fast synthesizing of GdB3O6 is ofimportant significance. This topic makes use of Gd2O3 and H3BO3 as rawmaterials, keeps them hydro-thermal activated for three to five days byapplying the water thermal activation process, and GdB3O6 is synthesized afterhigh temperature annealing. The synthesis of chemical composition and crystal structure information is obtained by characterizing the syntheticcompounds with X-ray powder diffraction and analysis of its spectrogram.