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Transmission electron microscopy (TEM) studies provide mechanistic understanding of nanoscale processes, whereas advanced synchrotron XRD (SXRD) enables precise measurements on volumes that are more representative of bulk materials. Therefore, the combined strengths of these techniques can provide new insight into irradiation-induced mechanistic processes. In the present study, their application to Zircaloy-2, proton-irradiated to 2.3, 4.7, and 7.0 dpa at 2 MeV and 350 °C and neutron-irradiated to 9.5 and 13.1 × 1025 n m−2 are exemplified. The application of correlative spectral imaging and structural TEM investigations to the phase transformation of Zr(Fe,Nb)2 precipitates in Low-Sn ZIRLO™, neutron-irradiated to 8.9–9 × 1025 n m−2, demonstrates the possibility of a Cr core nucleation site. Anomalous broadening is observed in SXRD profiles, which is believed to be caused by defect clusters and …