Thin films of Y–Ba–Cu–O and Yb–Ba–Cu–O, 0.5–1.5 μm in thickness, were deposited onto (211) and (100) SrTiO3 single crystal substrates by metalorganic deposition (MOD). After deposition the samples were annealed either by conventional furnace annealing or rapid thermal annealing (RTA). The microstructures of these films were then characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive x-ray spectrometry (EDS). Grain size of the annealed films varied from 0.25 to 1.0 μm. Improved superconducting properties were found for the RTA samples, compared to furnace annealing, and were attributed to larger grain size, little strontium diffusion into the thin films from the substrate, and highly preferred orientation of the 1:2:3 phase.