The electrochemical behavior of nickel (Ni) in different concentrations of sulfuric acid (H2SO4) was studied via cyclic voltammetry (CV) over a range of potentials (0.0 V– 3.0 V) at room temperature. The presented work displays novel experiments where external forcing by a platinum (Pt) electrode changed the proton concentration at a Ni electrode surface in order to control the frequency and magnitude of periodic oscillations produced. When studying unique phenomena such as the Ni phenomena in this thesis, efficient, durable, and inexpensive technology is always beneficial. A coupled microelectrode array sensor or CMAS which has been used for over four decades to study pitting corrosion, crevice corrosion, intergranular corrosion, galvanic corrosion, and other heterogeneous electrochemical processes were fabricated in a novel, systematic, inexpensive, and time efficient process. The presented work shows how to make the CMAS and proved that they functioned properly.