A zinc sulfate film is deposited from aqueous solutions of zinc sulfate onto the gold surface with the aim of preparation of a sensor for electrochemical quartz crystal microbalance (EQCM). The kinetics of this process, the particles formed in solution, and the film itself are studied by the methods of electrochemical quartz crystal microbalance, X-ray photoelectron spectroscopy, transmission electron microscopy, atomic force microscopy, optical and Raman spectroscopies, and dynamic light scattering. The effect of the procedure of gold surface preparation, the reagent concentration, and the temperature on the film adhesion, the length of induction period, the kinetics of film growth, and its structure and thickness are studied. It is shown that the film formation proceeds as a result of deposition of sufficiently coarse 200–700 nm colloid particles of sphalerite. It is demonstrated that this sensor can be used in studying the electrochemical reactions of ZnS and the interface phenomena by the methods of EQCM and cyclic voltammetry.