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Derby, Benjamin

Publications and source records attributed to Derby, Benjamin.

Irradiation-Induced Grain Growth of gamma-Fe2O3 and Fe3O4 at Cryogenic Temperatures

This work reports the first observations of grain growth under irradiation of Fe oxides, specifically maghemite gamma-Fe2O3 and magnetite Fe3O4. The Fe oxide thin films were grown by Pulsed Laser Deposition and irradiated in-situ in a Transmission Electron Microscope at - 223°C using 1 MeV Kr2+ ions up to 8.75 x 10^19 ions/m^2 to study grain growth kinetics under irradiation. Grain growth at such low temperatures appears to follow kinetics that can be accounted for by the thermal spike model developed for metals in the literature. The corresponding activation energies were calculated and compared with other oxides. The results demonstrate that gamma-Fe2O3, despite its larger initial grain size, exhibits surprisingly fast grain growth in comparison with Fe3O4, likely due to the presence of iron vacancies in the crystal structure that facilitate faster atomic diffusion under irradiation.

Kretov, Dmitrii↗

The mechanism behind the high radiation tolerance of Fe-Cr alloys

With the great demand for high radiation tolerant materials for advanced nuclear energy technologies, Fe-Cr alloys are at the forefront with long standing validated performance. Yet, the real mechanism behind their high radiation resistance is in question and understanding the effect of varying Cr percentage is a grand challenge limiting further improvements. Here we applied depth resolved atomic scale probe of defects to uncover the real mechanism on how Cr improves radiation resistance and explain the controversial impact of increasing Cr percentage. By combining depth-resolved positron annihilation lifetime spectroscopy and Doppler broadening spectroscopy we investigated the effect of Cr alloying on the formation and evolution of atomic size clusters induced by ion irradiation in Fe. We also used atom probe tomography to investigate the possible presence of Cr clusters or a’ phase with high Cr composition. The study reveals that the well-known resistance to radiation in Fe-Cr alloys arises from the stabilization of vacancy clusters around Cr atoms which act as sinks for radiation-induced defects. Thus, Cr atoms do not provide a direct sink for interstitials; rather defect complexes for that consist of Cr atoms and vacancies in turn act as sinks for irradiation-induced vacancies and interstitials. Most importantly, we find that lower amounts of Cr create smaller, uniformly distributed defect clusters that act as efficient sinks for radiation damage, but larger quantities of Cr form a defect structure that is less homogenous in size and spatial distribution, resulting in less efficient damage recombination. No evidence of phase a’ was found before or after irradiation, which indicates that it does not contribute to the observed radiation tolerance.

36 MATERIALS SCIENCE↗

Hierarchical morphologies in co-sputter deposited thin films

Co-depositions of immiscible alloy films at specific processing conditions have yielded hierarchical microstructures which consist of distinct features at multiple length scales, often agglomerates and concentration modulations on the sub-micrometer-scale and fine nanoprecipitates in a matrix on the nanoscale. The present work examined a series of immiscible alloy systems: Cu-Mo, Cu-Ag, Cu-Fe, Cu-Ta, Mo-Ag, Cu-Mo-Ag, to determine the kinetic conditions favorable for hierarchical organization and the formation mechanism of such structures. Thin films of six immiscible systems were sputter co-deposited over a range of deposition rates from 0.12 to 2 nm/s and various temperatures from 400 to 800°C. The resulting microstructures indicate that hierarchical structures form with sufficient disparity in kinetic energy between the constituent atoms, one species being highly mobile (A) and the other relatively immobile (B). This condition arises typically at elevated deposition temperatures and reduced deposition rates but is also alloy dependent. The hierarchical structures form during deposition via phase separation and self-organization processes across the multiple length scales. The adatoms diffuse on the film surface with the highly mobile species swiftly agglomerating into A-rich domains within which B-rich nanoprecipitates form, often self-organizing into periodic arrays. The smallest B-rich nanoprecipitates in the A-rich domains are found to be coherent and in a metastable crystal structure (B taking the structure of A), but coarser precipitates that exhibit the equilibrium structure of B element. The A-rich domains are surrounded by a B-rich matrix that phase-separates into a concentration modulated structure. In conclusion, the observations are interpreted via a model incorporating material properties and process parameters.

36 MATERIALS SCIENCE↗

A pathway to synthesizing single-crystal Fe and FeCr films

Nuclear reactor environments provide a unique scientific and engineering challenge wherein materials must tolerate prolonged exposure to concurrent irradiation, elevated temperatures, and corrosive media. However, uncontrolled variability in material composition and structure often prohibits truly single-variable experiments that can reveal basic aspects of environmental damage. Here, Magnetron sputtering is used to provide a more controlled model system for these fundamental studies, yielding reproducible single-crystal Fe and FeCr thin films containing 8 and 18 at.% Cr. Electron microscopy is used to determine the systematic correlations between growth conditions and the resulting film microstructure and surface morphology. It is found that the substrate temperature and applied radio frequency (RF) bias can be tuned to obtain consistent homogeneous and single crystal films with a minimal amount of Ar impurities from the RF bias process. Epitaxial, single-crystal Fe films are obtained on MgO substrates at 500 °C with 10 Watt (W) RF bias deposition. However, when Cr is alloyed with Fe, higher substrate temperatures (600 °C) and applied RF biases (15 W) are required to achieve a similar epitaxial single-crystal FeCr film. Accelerated molecular dynamics simulations reveal that Cr impedes surface transport, explaining the need for higher temperature and bias during the growth of the Cr-bearing films.

36 MATERIALS SCIENCE↗

Fracture resistance of hierarchical Cu–Mo nanocomposite thin films

We report the fracture behavior of high-temperature co-sputtered Cu/Mo nanocomposite thin films was investigated through in situ 3-point bend testing of pre-notched microbeams in SEM. The as-synthesized nanocomposites present hierarchical nano/microstructures composed of a matrix of phase-separated Cu–Mo with nanoscale ligaments dispersed with sub-micron scale Cu-rich islands containing Mo nano-precipitates. Results show a significant crack growth resistance in the hierarchical nanocomposite, several times higher than that measured in Cu/Mo nanoscale multilayers. Based on electron microscopy characterization, three mechanisms of crack growth resistance in the hierarchical structures are proposed: crack bridging by the Cu-rich layer, crack deflection via shear along the Cu/Mo interface, and multiple cracking. This work demonstrates an approach to increase toughness in high strength nanocomposites through interface micro-structure design.

36 MATERIALS SCIENCE↗

Microstructural characterization of phase-separated co-deposited Cu–Ta immiscible alloy thin films

Elevated temperature co-sputtering of immiscible elements ends in a variety of self-organized morphologies due to phase separation. Cu–Ta is used as a model system to understand the evolution of phase-separated microstructural morphologies by co-sputtering thin films with nominal 50–50 at.% composition at four temperatures: 25, 400, 600, and 800 °C. Scanning/transmission electron microscopy of the film cross sections showed the microstructure morphology varied from nanocrystalline Cu–Ta at 25 °C to a wavy ribbon-like structure at 400 °C, to Cu-rich agglomerates surrounded by Ta-rich veins at 600 and 800 °C. In the agglomerate-vein morphology, microstructural features were present on two length scales, from a few nanometers to a few tens of nanometers, thus making the structures hierarchical. On the nanoscale, the Cu-rich agglomerates contained Ta precipitates, whereas the Ta-rich veins had embedded Cu nanocrystals. The various microstructures can be attributed to the highly disparate constituent element interdiffusion at the deposition temperatures with the Cu having orders of magnitude higher mobility than Ta at the deposition temperatures. This research of processing–microstructure relationship will be useful in guiding the design of hierarchical multiphase microstructures in binary or multicomponent thin films with tailored mechanical properties.

36 MATERIALS SCIENCE↗