Post-test corrosion analysis of high-temperature thermal energy storage capsules

Thermal energy storage capsules have been freeze-thaw cycled in vacuum at 1000 ± 100 K. The capsules were fabricated from Inconel 617^® (Inco Alloys International, Inc.) and contained eutectic fluoride mixtures of sodium, magnesium, lithium, and potassium. Samples that were thermal cycled for 20,000 and 30,000 hr were analyzed for corrosion effects. Radiography indicated neither flaws nor inhomogeneities, and there were no significant microstructural changes in the container alloy. The microstructural damage penetrating the inside surface was as deep as 120 m and that penetrating the outside surface was approximately 150 m. Microprobe results on the containers revealed a concentration gradient of alloying elements. The aluminum concentration was reduced from 1.34% in the original matrix to 0.4% at 10 m from the inside surface, and chromium was reduced from a nominal value of 23% to 10% at the outer surface. The depletion of aluminum and chromium from the outer surface was due to vacuum vaporization at elevated temperature. X-ray diffraction revealed the formation of possible protective films consisting of MgNaF₃ and MgF₂. The measured and theoretically predicted concentrations of aluminum and chromium were in good agreement. It was concluded that the corrosion process is a solid-state diffusion-dominated process and an expected lifetime of 5 to 7 years is a reasonable estimate.