A general microwave-assisted two-phase strategy (MTS) has been developed for the synthesis of monodisperse inorganic nanocrystals (NCs). A series of metal oxides, ferrite, hydroxides, and metal sulfide NCs were synthesized by using water-soluble metal salts. The obtained NCs were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The composition, size, and shape of the NCs can be tuned by the types of precursors, the concentrations of metal ions, and the species of ligands. This protocol creates a new synthetic route, which may also be further extended to synthesize other nanomaterials, including alloy, noble metal, rare-earth fluorescent, etc.