Due to their small size and thickness, metallic thin films exhibit novel properties which largely differ from the bulk materials. Due to their significant properties it can be used as different applications. Generally the shape, size, and size distribution of particulates and grains can be controlled by adjusting the reaction condition such as external and internal parameters like temperature, electrolyte concentration, current density, PH of the solution. Sonoelectrochemistry is the study of the effects of the combination of ultrasonic vibration with electrode processes occurring at surfaces of electrodes immersed in a solution in an electrochemical cell. This book provides a new method for the synthesis of metallic thin film i.e., sonoelectrosynthesis. The grain size, microstructure and mechanical properties of the electrodeposited metal thin film depends upon various parameters like temperature, PH, current density, and concentration of electrolyte and also ultrasound has many numerous effects on the grain size, hardness, porosity and brightness of the deposits. The analysis should help to synthesis of metallic thin film by sonoelectrosynthesis with better properties.