A home made microelectrodes constructed using platinum disc, gold disc and gold array were successfully fabricated and the microelectrodes were characterized using voltammetry techniques. Characterization and practical applications of the home made microeletrodes were determined through cyclic voltammetric experiments on sulfuric acid, potassium ferrocyanide trihydrate and ruthenium hexaamine (III) trichloride. Micro electrochemical technical using micro capillary as a micro cell are remarkable methods to study local phenomena on metals surface. A homemade electrochemical device drop let cell with capillary tip approximately diameter 100 μm positioned on sample surface characterise with cyclic voltammetry at microdisc electrode and plate electrode; experiments were carried out copper deposition on microdisc electrode followed with copper liner voltammetry and ruthenium hexaamine cyclic voltammetry by cyclic voltammetry on microdisc electrode. This research also includes a study on sulfuric acid voltammetry at gold plate and platinum plate electrode.