The content of this book is devoted to the synthesis of advanced nano-materials and layers by application of electrochemical methods. Examples for their applications in fuel cells, batteries, photovoltaics, magnetic materials, environmentally friendly anticorrosion coatings and surface pretreatments, especially anodization are provided. Cu-metallization of non-conductive substrates is proposed, as well. In addition, electrochemical coating of copper surfaces by Ni-Co, Ni-P, Co-P and Ni-Co-P alloys with catalytic and magnetic properties is described in detail. The application of such layers is proposed PEMFC bipolar plates, after additional coating by polytetrafluoroethylene. The topic of the surface phosphatation is further extended by brief study of the properties of cesium dihydrogen phosphate for potential application in the fuel cell technology. Meanwhile, the Zn and Al anodization, as metal surface treatment approach is also proposed. Among the electrochemical analytical methods, special attention is turned to Electrochemical Noise analysis, Electrochemical Impedance Spectroscopy, and to classical potentiodynamic scanning techniques.