Yttrium-aluminum-garnet (YAG, Y3Al5O12) hollow microspheres were synthesized by reverse-emulsion (w/o) technique starting with aqua-based precursors of oxides. The non-ionic surfactant was used as the emulsifying agent. The gel powders were calcined at 700 degrees-1200 degrees C. The synthesized powders were characterized by differential thermal analysis (DTA), thermogravimetry, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The appearance of an exothermic peak at 932 degrees C in the DTA curve revealed the crystallization of YAG, which was further confirmed by XRD and FTIR studies. SEM confirmed the formation of hollow microspheres.