Electrochemical Technique to Characterize the High Temperature Oxidation Behavior of Materials

This work demonstrates an approach using solid state electrochemical cells to study the long-term oxidation of materials at 800 °C. The capability of zirconia-based cells to control the oxygen partial pressure was first evaluated using an empty chamber. For most voltages applied to the pump cell, the steady state sensor voltage matches the pump voltage, leakage rates are low, and response times are short, allowing precise and prompt control over the chamber atmosphere. The technique was validated by measuring the oxidation of niobium and nickel. Niobium was oxidized at pump voltages ranging from 0 mV to +500 mV; decreasing the oxygen partial pressure around the specimen reduces the oxidation rate. Comparing the integrated oxidation rate with the weighed mass gain showed good agreement. Measured oxidation rates for nickel were of order 1 μ g h −1 , illustrating the sensitivity of this technique. For higher oxidation rates, a depression in oxygen partial pressure was observed around the specimen. Improved control over the oxidation potential was achieved by using a sensor cell to dynamically tune the pump voltage. Rates for both metals are compared to literature reports using other techniques.