Microstructure of Oxide Layers Formed During Autoclave Testing of Zirconium Alloys

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Abstract
The microstructure of oxide layers formed in steam in a 400°C, 10.3-MPa autoclave on different zirconium alloys was studied by transmission electron microscopy. Pre-and post-transition oxide layers on Zircaloy-4 with different heat treatments, and post-transition oxide layers on Zr-0.5Sn-0.53Nb were compared. Special attention was paid to the oxide-metal interface. In Zircaloy-4 with short annealing times and high post-transition corrosion rates, the interface had a disordered structure, and pores were found in the oxide very close to the interface. In Zircaloy-4 with low uniform corrosion rates, the interface consisted of highly ordered, columnar grains. The interface in Zr-0.5Sn-0.53Nb had a different appearance, with an intermediate phase of equiaxed grains between the columnar oxide and the metal. The hydrogen absorption of the zirconium alloys during oxidation was measured by the melt extraction technique on samples oxidized for 63, 147, and 343 days. The Zr-0.5Sn0.53Nb alloy had considerably lower hydrogen absorption than Zircaloy-4.