The use of a laser-assisted Local Electrode Atom Probe and TEM to examine the microstructure of Zircaloy and precipitate structure following low dose neutron irradiation at nominally 358 °C

Previous research has shown that the irradiation of Zircaloy at very low fluences (⩽7 × 1022 n/m2 (E > 1 MeV)) results in measurable irradiation hardening, but the defects or solute clusters responsible for such hardening are generally below the resolution limit of electron microscopy. Efforts to analyze Zr-based alloys using conventional atom probe have been largely unsuccessful due to the poor electrical conductivity of Zirconium at cryogenic temperatures. Laser-assisted atom probe methods were introduced in the 1980s as a means for enabling low electrical conductivity specimens to be analyzed. Some recent examples have been reported in the literature where a Local Electrode Atom Probe (LEAP)® was used to successfully analyze non-irradiated Zirconium based alloys, such as Zircaloy-4 and ZIRLO. In this work, the use of a LEAP to examine the microstructure of non-irradiated Zircaloy alloys is evaluated. Optimum conditions for applying the LEAP to non-irradiated Zircaloy-2 and Zircaloy-4 are investigated. Changes in the local composition of precipitates and grain boundaries following neutron irradiation at nominally 358 °C to a fluence of 2.9 × 1025 n/m2 in the High Flux Isotope Reactor (HFIR) are determined using Transmission Electron Microscopy. These results are provided as an example of the local changes in microstructure that can influence the evolution of the defect structure.