Gadolinium scandate (GdScO3) has been synthesized at 300 degrees C through the decomposition of a mixed cation hydroxide hydrogel in a humid environment. Increasing the reaction temperature produced larger particles that better adopted the Wulff shape. A lack of water vapor during the synthesis caused the solid network of the hydrogel to collapse upon heating so an amorphous xerogel was produced. Water vapor in the system imbibed the hydrogel and allowed for greater diffusion of the atomic species to allow for crystallization into the perovskite phase at temperatures lower than typical sol-gel processes. Temperatures less than 300 degrees C, or an excess of water vapor, promoted the formation of Gd(OH)(3) and ScOOH in addition to or in lieu of GdScO3.