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The superconducting and magnetic properties of phase-separated A x Fe 2−y Se 2 compounds are known to depend on postgrowth heat treatments and cooling profiles. This paper focuses on the evolution of microstructure on annealing and how this influences the superconducting properties of Rb x Fe 2−y Se 2 single crystals. We find that the minority phase in the as-grown crystal has increased unit cell anisotropy (c/a ratio), reduced Rb content, and increased Fe content compared to the main phase. The microstructure is rather complex, with two-phase mesoscopic plate-shaped features aligned along {113} habit planes. The minority phases are strongly faceted on the {113} planes, which we have shown to be driven by minimizing the volume strain energy introduced as a result of the phase transformation. Annealing at 488 K results in coarsening of the mesoscopic plate-shaped features and the formation of a third distinct phase. The subtle differences in structure and chemistry of the minority phase(s) in the crystals are thought to be responsible for changes in the superconducting transition temperature. In addition, scanning photoemission microscopy has clearly shown that the electronic structure of the minority phase has a higher occupied density of states of the low binding energy Fe3d orbitals, which is characteristic of crystals that exhibit superconductivity. This demonstrates a clear correlation between the Fe-vacancy-free phase with high c/a ratio and the electronic structure characteristics of the superconducting phase.

High-resolution characterizations of intergranular attack in alloy 600 (Ni-17Cr-9Fe) exposed to 325°C simulated pressurized water reactor primary water have been conducted using a combination of scanning electron microscopy, NanoSIMS, analytical transmission electron microscopy, and atom probe tomography. The intergranular attack exhibited a two-stage microstructure that consisted of continuous corrosion/oxidation to a depth of ~200 nm from the surface followed by discrete Cr-rich sulfides to a further depth of ~500 nm. The continuous oxidation region contained primarily nanocrystalline MO-structure oxide particles and ended at Ni-rich, Cr-depleted grain boundaries with spaced CrS precipitates. Three-dimensional characterization of the sulfidized region using site-specific atom probe tomography revealed extraordinary grain boundary composition changes, including total depletion of Cr across a several nm wide dealloyed zone as a result of grain boundary migration.

Analysis of the detected Fe ion charge states from laser-assisted field evaporation of magnetite (Fe3O4) reveals unexpected trends as a function of laser pulse energy that break from conventional post-ionization theory for metals. For Fe ions evaporated from magnetite, the effects of post-ionization are partially offset by the increased prevalence of direct evaporation into higher charge states with increasing laser pulse energy. Therefore, the final charge state is related to both the field strength and the laser pulse energy, despite those variables themselves being intertwined when analyzing at a constant detection rate. Comparison of data collected at different base temperatures also shows that the increased prevalence of Fe2+ at higher laser energies is possibly not a direct thermal effect. Conversely, the ratio of 16O+:(16O2+ + 16O+) is well correlated with field strength and unaffected by laser pulse energy on its own, making it a better overall indicator of the field evaporation conditions. Plotting the normalized field strength versus laser pulse energy also elucidates a non-linear dependence, in agreement with the previous observations on semiconductors, which suggests field-dependent laser absorption efficiency. Together these observations demonstrate that the field evaporation process for laser-pulsed oxides exhibits fundamental differences from metallic specimens that cannot be completely explained by post-ionization theory. Further theoretical studies, combined with detailed analytical observations, are required to understand fully the field evaporation process of non-metallic samples.