The aim of this project is to investigate the photocatalytic activity of ZnO/TiO2 composite films for the gas-phase oxidation of ethanol. Pure TiO2, pure ZnO, and their composites were formulated using a sol-gel synthesis method, and the resulting powders were cast and dried as thin films in a flat-plate ultraviolet light-emitting diode (UV LED) reactor. P25 TiO2 and commercially available ZnO were also used for comparison. The structural, morphological, and optical characteristics of the materials were characterized. The photocatalytic oxidation of ethanol vapors in air after 24 h of reactor operation was used to assess the relative photocatalytic activity of the ZnO/TiO2 composite films. Our results show that as ZnO content increased in the coupled semiconductor materials, the apparent photocatalytic activity decreased. In this study, pure ZnO (both sol-gel and purchased) had the least photocatalytic activity for vapor-phase ethanol oxidation in our test apparatus. For gas-phase photocatalysis, surface area was shown to be a critical feature for photocatalytic activity. However, the inherent photocatalytic activity of the materials was not decoupled from the effects of surface area in this study.