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Thin films of Y‐Ba‐Cu‐O were produced by RF sputtering of YBa2Cu3O7‐x ceramic targets, using a variety of plasma compositions, RF power levels, and substrate temperatures. Post annealing of these films in oxygen produced superconducting films with Tc values between 40‐60 K, broad transition widths and semiconductor‐like electrical behavior above Tc. Subsequent annealing at 850°C in an inert gas with a residual oxygen partial pressure of ≤10 ppm followed by an oxygen anneal produced high quality thin films: Tc> 85 K with narrow transition widths. The structure and morphology of these films during reduction‐oxidation processing were monitored using X‐ray diffraction and electron microscopy.