Studies of second phase particles in different zirconium alloys using extractive carbon replica and an electrolytic anodic dissolution procedure

Zirconium alloys are widely studied for applications as cladding tubes and structural components of PWR fuel assemblies. Due to their influence on some of the alloys properties (corrosion resistance, irradiation growth, …), the crystallographic structure and the chemical stoichiometry of the second phase particles (SPP) precipitated in these alloys have to be well established. The aim of this paper is to present the results obtained using two methods of SPP extractions. The first one, the extractive carbon replica method, allowed us to determine the chemical composition of SPP in different zirconium alloys: Zr–Sn–Fe–Cr (Zircaloy-4®), Zr–Sn–Fe–Cr–(V,Mo), Zr–Nb and Zr–Nb–Fe alloys. The second one, an anodic dissolution procedure of the matrix, is an interesting way of isolating SPP from the surrounding α-Zr matrix, giving access to a precise determination of the crystallographic structure and lattice parameters of the SPP by X-ray diffraction. This procedure was validated for Zy-4 by comparing the SPP size distribution obtained by extraction with that directly measured on a massive Zy-4 alloy (i.e. the SPP size distributions were the same for both measurements).