X-ray diffraction (XRD) and transmission electron microscopy (TEM) have been used to characterize microstructural and microchemical changes produced by neutron irradiation in zirconium and zirconium alloys. Zircaloy-2, Zircaloy-4, and Zr-2.5Nb alloys with differing metallurgical states have been analyzed after irradiation for neutron fluences up to 25 × 1025 n.m-2 (E > 1 MeV) for a range of temperatures between 330 and 580 K.
Irradiation modifies the dislocation structure through nucleation and growth of dislocation loops and, for cold-worked materials in particular, climb of existing network dislocations. In general, the a-type dislocation structure tends to saturate at low fluences (< 1 × 1025 n.m-2). The c-component dislocation structure, however, may evolve over long periods of irradiation (for fluences >10 × 1025 n.m-2 in some cases).
The phase structure is also modified by irradiation. The common alloying/impurity elements, Fe, Cr, and Ni, are relatively insoluble in the α-phase but are dispersed into the α-phase during irradiation irrespective of the state of the phase initially containing these elements, i.e., metastable β-phase or stable intermetallic precipitate. The stable intermetallic particles may undergo structural changes dependent on their composition and the temperature. For the metastable dual-phase α/β-alloys (Zr-2.5Nb alloy), the β-phase structure is modified during irradiation, but the change is complex, being a combination of thermal decomposition and radiation-induced mixing.
X-ray diffraction (XRD) line-broadening analysis has been used to determine dislocation densities in zirconium alloys with hexagonal closepacked (hep) crystal structures and a complex distribution of dislocations reflecting the plastic, anisotropy of the material. The validity of the technique has been assessed by comparison with direct measurements of dislocation densities in deformed polycrystalline and neutron-irradiated single crystal material using transmission electron microscopy (TEM). The results show that-there is good agreement between the XRD and TEM for measurements on the deformed material whereas there is a large discrepancy for measurements on the irradiated single crystal; the XRD measurements significantly underestimating the TEM observations.
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