A novel microwave-assisted synthesis technique was used for the rapid preparation of nanocrystalline ZnGa2O4 at two different temperatures. The crystalline spinel oxide is formed at temperatures as low as 100 oC within few minutes, at a high yield of 96%, requiring no post-synthesis annealing. The as-prepared samples are polycrystalline and phase-pure as verified by XRD, with a crystallite size of ∼5 nm. Polycrystalline ZnGa2O4 substituted with Mn2+, Cr3+, Cu2+, and Co2+ was also similarly prepared. All samples are highly monodispersed, as measured by TEM. The ZnGa2O4 nanocrystals without further surface modification can be readily dispersed in chloroform to form a fully transparent colloidal solution, using which the bandgap of ZnGa2O4 was determined to be ~4.5 eV. The entire synthesis procedure, including solution preparation, microwave irradiation, and centrifugation takes about 30 minutes, which is faster than any procedure reported for a complex oxide like ZnGa2O4, as well as one with a small thermal budget. Photoluminescence shows a broad emission extending from 330 nm to 800 nm, which is surmised to be due to the defect structure in the oxide produced.