This paper focuses on the use of QCM for the study of semiconductor film deposition processes. Specifically the electrosynthesis of metal chalcogenides (In2S3, CdS, and CdTe) is considered. A brief background is first given for electrodeposition as a process candidate for semiconductor film preparation. Previous studies are reviewed on the use of QCM (and specifically EQCM) in this area. New combined voltammetry-EQCM data are presented for the oxidative deposition of sulfur on polycrystalline Au surfaces from alkaline sulfide baths. The anodic growth of CdS films and the cathodic electrosynthesis of In2S3 are studied by the combined approach. Finally, data are presented on the cathodic electrosynthesis of CdTe films using EQCM in a rotating disc electrode (RDE) configuration. From an instrumental perspective, the presented data illustrate the virtues of combining the QCM technique with cyclic voltammetry, coulometry, and hydrodynamic (RDE) voltammetry for studies of semiconductor film deposition.