This book provides an electrochemical production of semi-conductor thin films of rhenium chalcogenide alloys. In the work mechanism and kinetics of rhenium-selenium alloy deposition process from acidic and alkaline Re-Te solutions and Re-S from thiocarbamide solutions were studied. Main regularities of co-deposition process, nature and character of rhenium chalcogenides polarization from solutions were researched. Some physical and electro-physical properties of rhenium alloys were studied. Photo-electrochemical activity of thin films on the basis of Re-Se alloys was studied and these thin films can be used as a photo-electrode material for conversion of solar energy into chemical. This book is a useful guide for students and scientists working on electrochemistry