Solute Concentrations in the Matrix of Zirconium Alloys Studied by Atom Probe Tomography

Paper in proceeding, 2023

This work indicates that the matrix content of the alloying elements iron, chromium, and nickel in as-produced commercial Zircaloy-2-type materials is lower than what has been indicated by many previous studies. Atom probe tomography in voltage pulse mode was used to study the matrix content of solutes in Zircaloy-2 of type LK3/L and a similar model alloy, called Alloy 2, of the same heat treatment. Both alloys were analyzed in the as-produced state and after reactor exposure. In the as-produced materials, the concentrations of iron, chromium, and nickel were all below the detection limits of around 10 wt. ppm. After reactor exposure, these alloying elements were observed to reside in clusters at loops, and the matrix content (including clusters) of iron had increased to about 1,200 wt. ppm in the fueled region of the rod and to about half that value in the plenum region. The chromium content in the fueled region was approximately 100 wt. ppm, and the nickel content was approximately 200 wt. ppm. In the plenum region, the content of these elements was lower. However, due to an uneven distribution of clusters, there was a wide scatter in the measured concentrations in the irradiated materials. Additionally, the matrix concentrations of solute elements in (nonirradiated) Zircaloy-2 were investigated for a series of samples subjected to a annealing at 770◦C followed by cooling at different rates. From these measurements, the solubilities at 770◦C were estimated to be around 65 wt. ppm for chromium, at least 37 wt. ppm for iron, and below 9 wt. ppm for nickel. Slow cooling resulted in virtually no iron, chromium, or nickel in the matrix. The concentration of aluminum in the matrix was observed to be between 10 and 20 wt. ppm for all a-annealed samples and for the as-produced materials of commercial heat treatment.