Yttrium oxide nano-powder has been successfully synthesized by a novel approach. In the first step, a foamy structure was produced by combustion synthesis using yttrium nitrate and glycine. This was followed by the addition of sulfate ions and calcination at 1100 °C for 4 h. The sulfated and unsulfated powders were characterized by X-ray powder diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM) and the Brunauer-Emmett-Teller method (BET). The sinterability of the resulting powders was also studied by dilatometry. The studies indicated that this method not only allows for producing weakly-agglomerated nano-particles, but is also a very time-efficient process in comparison to precipitation techniques. Moreover, the possibility of performing all processing steps in a fully automated batch reactor was also considered.