Isothermal Annealing of Shocked Zirconium: Stability of the Two-phase $\alpha/\omega$ Microstructure

TL;DR

This study investigates the stability and transformation behavior of the $eta$-phase zirconium microstructure after shock loading and annealing, revealing partial reverse transformation and dislocation effects using in-situ synchrotron X-ray diffraction.

Contribution

It provides new insights into the metastable $eta$-phase microstructure stability and transformation mechanisms in zirconium under high-pressure shock and annealing conditions.

Findings

Reverse transformation to $eta$-phase is incomplete and reaches a metastable state.

Higher initial shock pressures increase transformation rates.

Dislocation densities decrease with annealing, affecting transformation dynamics.

Abstract

Under high pressure conditions, Zr undergoes a phase transformation from its ambient equilibrium hexagonal close packed $\alpha$ phase to hexagonal $\omega$ phase. Upon returning to ambient conditions, the material displays hysteretic behavior, retaining a significant amount of metastable $\omega$ phase. This study presents an in-situ synchrotron X-ray diffraction analysis of Zr samples shock-loaded to compressive peak stresses of 8 and 10.5 GPa and then annealed at temperatures of 443, 463, 483, and 503K. The evolution of the $\alpha$ phase volume fraction was tracked quantitatively, and the dislocation densities in both phases were tracked qualitatively during annealing. Upon heating, the reverse transformation of $\omega\to\alpha$ does not go to completion, but instead reaches a new metastable state. The initial rate of transformation is faster at higher temperatures. Samples shock-loaded to higher peak pressures experienced higher initial transformation rates and more extensive transformation. Dislocation content in both phases was observed to be high in the as-shocked samples. Annealing the samples reduces the dislocation content in both phases, with the reduction being lesser in the $\omega$ phase, leading to the postulation that transformation from $\omega\to\alpha$ is restricted by the pinning effect of dislocation structures within the $\omega$ phase. Electron backscatter diffraction analysis affirmed that the expected $(0\;0\;0\;1)_\alpha\parallel(1\;0\;\overline{1}\;1)_\omega$ and $[1\;0\;\overline{1}\;0]_\alpha\parallel[1\;1\;\overline{2}\;\overline{3}]_\omega$ orientation relationship is maintained during nucleation and growth of the $\alpha$ phase during the annealing. \end{abstract}