The synthesis of various nanoscale materials, such as nanoparticles, nanowires of Au, Pt, Ni Co, Fe, Ag etc., by electrodeposition techniques have been demonstrated in this article. Both potentiostatic and galvanostatic methods were employed to carry out the electrodeposition process under different potential ranges, time durations, and current densities. The electrochemical behavior of the deposited nanoparticles on various substrates was investigated by cyclic voltammetric and chronoamperometric techniques. The synthesis of mono-dispersed gold (Au) nanoparticles on indium tin oxide (ITO) coated glass, preparation of Au nanorods on nanoporous anodic alumina oxide (AAO), formation of Au nanoclusters on polypyrrole-modified glassy carbon electrode and one-step electrodeposition of nickel nanoparticle chains embedded in TiO 2 etc. have been highlighted in this article. The potential applications of synthesized nanoparticles such as the role of maghemite (Fe 2 O 3 ) in arsenic remediation, higher electrocatalytic activity of Ag nanoclusters for the reduction of benzyl chloride, and the role of C 60 nanoparticle-doped carbon film in fabrication processes are also presented in this article.