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Evaluating Carrier Longevity Including Chemical/Microstructural Integrity for Extended Cycling: Effects of Atmosphere and Temperature on Particle Integrity

As part of a series of studies to determine the effects of extended cycling (50 – 1000 cycles), at different atmospheres and temperatures, has on the chemical structure, microstructure, and pellet morphology of existing manufactured oxygen carriers (OC), a progression of experiments utilizing Thermal Gravimetric Analysis (TGA) and Scanning Electron Microscopy/X-ray Microanalysis (SEM/XM) are in the process of being carried out. One of the experiments presently underway incorporates a unique wafer design which provides the ability to track specific particles imbedded in and/or on (Type-II and Type-I, respectively) the wafer for pre and post imaging and analysis, Figure 1. The primary particle properties under investigation are grain size distribution changes, void distribution changes, and phase segregation, with the goal of determining if particle steady state ever reached, what this comprises in terms of chemical and microstructural changes, and how this is impacted by phase controlling the reactive atmospheres such as fuel/soft oxidant ratios that limit reduction and coking effects. These particular series of experiments are being carried out utilizing a TA Instruments Q-50 TGA and a JEOL-840A SEM interfaced to a Noran NS6 XM system; image analysis is being carried utilizing ImageJ.