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.

This dissertation describes the electrochemical behavior of nickel and iron that was studied in different acid solutions via linear sweep voltammetry, cyclic voltammetry, and potentiostatic measurements over a range of temperatures at specific potential ranges. The presented work displays novel experiments where a nickel electrode was heated locally with an inductive heating system, and a platinum (Pt) electrode was used to change the proton concentration at iron and nickel electrode surfaces to control the periodic oscillations (frequency and amplitude) produced and to gain a greater understanding of the systems (kinetics), oscillatory processes, and corrosion processes. Temperature pulse voltammetry, linear sweep voltammetry, and cyclic voltammetry were used for temperature calibration at different heating conditions. Several other metal systems (bismuth, lead, zinc, and silver) also produce periodic oscillations as corrosion occurs; however, creating these with pure metal electrodes is very expensive. In this work, metal systems were created via electrodeposition by using inexpensive, efficient, coupled microelectrode array sensors (CMASs) as a substrate. CMASs are integrated devices with multiple electrodes that are connected externally in a circuit in which all of the electrodes have the same amount of potential applied or current passing through them. CMASs have been used for many years to study different forms of corrosion (crevice corrosion, pitting corrosion, intergranular corrosion, and galvanic corrosion), and they are beneficial because they can simulate single electrodes of the same size. The presented work also demonstrates how to construct CMASs and shows that the unique phenomena of periodic oscillations that can be created and studied by using coated and bare copper CMASs. Furthermore, these systems can be controlled by implementing external forcing with a Pt electrode at the CMAS surface. The data from the single Ni electrode experiments and CMAS experiments were analyzed by using the Nonlinear Time-Series Analysis approach.