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  1. Shielded magnetic small-angle neutron scattering for characterization of radioactive samples

    The development of a Pb-shielded fixture for the execution of a small-angle neutron scattering (SANS)-based workflow for interrogation of highly irradiated nuclear materials has been explored. The Pb shielding was specially designed to reduce the detected radioactivity from the specimen during SANS experiments, and the overall configuration is termed shielded magnetic SANS (SM-SANS). Two FeCrAl-based alloys, C35M and 125YF, were examined with the SM-SANS technique using a free-form size distribution locally monodisperse model in both the as-received and irradiated states. Quantitative values derived from the free-form size distribution were compared with atom probe tomography experiments. Microstructural and compositional parameters determinedmore » using the two characterization techniques were complements of each other. The results demonstrate that the SM-SANS technique is an effective means of characterizing nanoscale clustering in irradiated material systems and provides new avenues for investigating radioactive material microstructures.« less
  2. Effect of corrosion behavior of cast and extruded ZK60 magnesium alloys processed via friction extrusion

    The increasing demand for high-strength, corrosion-resistant magnesium alloys in transportation has led to the development of new processing techniques. In this work, cast and extruded ZK60 magnesium alloys were processed using the innovative solid-phase process, Friction Extrusion (FE). The microstructure was analyzed using Scanning Electron Microscopy (SEM), and Energy Dispersive Spectroscopy (EDS), showing a marked reduction in grain size, uniform solute distribution (Zn and Zr), and second phases after FE processing. Moreover, optical micrographs and Electron Backscatter Diffraction (EBSD) were employed to further evaluate the alloy microstructure. The corrosion resistance and electrochemical behavior were analyzed using potentiodynamic polarization, Scanning Electrochemicalmore » Cell Impedance Microscopy (SECCIM), and atomic emission spectroelectrochemistry analysis (AESEC). Time evolution surface imaging and post-corrosion microstructures were also analyzed to support the understanding of underlying corrosion mechanisms. Corrosion initiation and propagation in FE-processed samples followed grain boundary patterns, differing from cast and extruded ZK60 behaviors. Electrochemical measurements and in-situ time-dependent optical imaging demonstrated that FE processing enhanced corrosion potential, reduced corrosion current, and increased cathodic activity. Additionally, FE processing reduced the disparity in pitting potential between cast and extruded samples, resulting in intermediate pitting potentials. Higher Mg and lower Zn dissolution was observed in the lower anodic currents for FE-processed samples. During aggravated anodic current cycles, Mg dissolution equalized, but the Zn/Mg dissolution ratio increased for FE-processed extruded samples, suggesting less cathodic activation and better resistance to further pitting.« less
  3. Manufacturing ODS Steels from GARS Powders by Friction Consolidation and Extrusion

    Previous research suggested that friction-based processing is a promising method for fabricating oxide dispersion-strengthened (ODS) steel. In this study, we combined friction consolidation and friction extrusion to successfully manufacture ODS steel rods using precursor powder made with gas atomization reaction synthesis. We examined the microstructure evolution from the initial powder to the final extruded rod, which revealed the dispersion process of Y. Additionally, by comparing the microstructures of three rods extruded at different temperatures, we showed that low-temperature friction extrusion effectively enhanced microstructure uniformity and prevented grain coarsening, leading to improved mechanical properties. Furthermore, our findings provide practical guidelines formore » adjusting processing parameters in the production of ODS steel using friction-based processing.« less
  4. Manufacturing Oxide Dispersion Strengthened (ODS) steel plate via cold spray and friction stir processing

    Oxide dispersion strengthened (ODS) steels, traditionally fabricated by ball milling and conventional powder metallurgy techniques to achieve bulk form, followed by intricate rolling and thermal treatment steps to achieve plate or sheet form. Here, we present a novel processing route that combines cold spray (CS) with friction stir processing (FSP) to manufacture ODS steel plate directly from gas atomization reaction synthesis (GARS)-prepared powder, thus no rolling steps involved. Microstructural and mechanical characterizations were performed to assess the quality and properties of the resulting ODS steel plate. Our findings demonstrate that the slightly porous CS deposited layer was fully consolidated aftermore » FSP, yielding a fully dense ODS steel plate that exhibited a favorable tradeoff between strength and ductility upon extraction from the substrate. Furthermore, through microstructural analysis, we revealed the presence of an appreciable density (∼1022/m3) of nano-sized oxide particles, with the majority being smaller than 5 nm via the combined CS + FSP fabrication route. This work serves as a first proof-of-concept demonstration of the manufacturing approach described herein, offering a possible alternative route for producing ODS steel plates.« less
  5. Friction extrusion of ODS copper rod made from powder

    Meters-long oxide dispersion strengthened copper rods were manufactured directly from powder by a single-step process, called friction extrusion. The average grain size was 880 nm, which was refined 40 times from powder precursor due to extensive shear deformation. Meanwhile, the average size of alumina particles was 60 nm which retains a decent oxide dispersion strengthening. Here, mechanical properties, including hardness, tensile strength, and ductility, were tested and found to have better or similar values than conventional sintered-then-extruded oxide dispersion strengthened copper materials. The presented technique promises a convenient avenue for the fabrication of oxide dispersion strengthened copper from powder.
  6. Multi-scale characterization of supersolidus liquid phase sintered H13 tool steel manufactured via binder jet additive manufacturing

    Additive manufacturing (AM) of H13 tool steel by binder jet 3D printing (BJ3DP) followed by pressureless supersolidus liquid phase sintering (SLPS) provides a low-cost alternative manufacturing method for components with intricate geometric features. However, the microstructure-mechanical property relationships for BJ3DP-SLPS produced H13 tool steel are not well understood, which makes it challenging to develop printing and post-processing methods that maximize part performance. In this work, we leverage atom probe tomography and transmission electron microscopy along with thermodynamic calculations to rationalize the microstructure-mechanical property relationships in as-sintered BJ3DP H13 tool steel. Here, we report for the first time, the presence ofmore » a continuous eutectic film-like carbide in H13 along with the more commonly observed cuboidal MX carbides in the prior liquid channels of the microstructure. Further, atom probe tomography revealed the interconnected nature of the MX carbides that appear to be discrete in two-dimensional micrographs. These continuous eutectic carbides and interconnected MX carbides result in brittle failure of the material. Characterization of these microstructural features will be critical in developing appropriate post-processing heat treatments for the improved mechanical performance of BJ3DP H13.« less
  7. No ball milling needed: Alternative ODS steel manufacturing with gas atomization reaction synthesis (GARS) and friction-based processing

    Oxide dispersion strengthened (ODS) steels are promising structural materials for future fusion reactors. The high-density (~1023/m3) of highly stable Y-(Ti)-O nano-oxides provide high sink strength for radiation resistance and high-temperature (> 650 °C) creep strength. Concomitantly, helium management is enabled by trapping high density (~1023/m3) of small (< 3 nm) helium bubbles in the vicinity of nano-oxides. However, conventional route of making ODS steels involves prolonged ball milling, canning, degassing, and laborious thermo-mechanical processing (TMP). Such route, especially the batch-by-batch ball milling step, faces persistent challenge with scalability and high costs. Gas atomization reaction synthesis (GARS) method has demonstrated themore » potential of making precursor ODS steel powders without ball milling, but the nano-oxide density was around 1021/m3 in the final consolidated form by conventional TMP. Taking advantage of GARS precursor powder, we use friction-based processing, including friction consolidation and extrusion, to manufacture ODS steel with further improved nano-oxide characteristics. Here, preliminary results showed that Y/Ti/O species were intimately mixed and rapidly reacted to form nano-oxides with a number density of ~1022/m3.« less
  8. Improved irradiation resistance of accident-tolerant high-strength FeCrAl alloys with heterogeneous structures

    In this work, post–neutron irradiation examination is performed on advanced accident-tolerant fuel (ATF) cladding iron-chromium-aluminum (FeCrAl) alloys with ~10–13at. % Cr, ~10–12 at. % Al, ~1 at. % Mo, and minor alloying elements including Y irradiated to a damage level of 7 displacements per atom (dpa) at irradiation temperatures of 267–282 °C. A compositional dependency of the Cr and Al content is observed on the ratio of sessile and glissile dislocation loops, where the density of a$$\langle$$100$$\rangle$$ type loops is somewhat higher than the a/2$$\langle$$111$$\rangle$$ type loops. The α' precipitate number density is inversely correlated to the starting Cr concentrationmore » of the alloys of interest. The irradiation to a higher dose of 7 dpa results in a higher density of dislocation loops and α' precipitates for the same alloys at a lower irradiation dose, such as 1.8 dpa. In this work, the effect of α' precipitates on the dislocation loop density is discussed, and the presence of α' appears to inhibit the nucleation of loops. Compared with first-generation FeCrAl alloys, these advanced alloys with heterogeneous structure exhibit a lower Cr concentration in α' precipitation at the same dose level; they act as weaker obstacles deviating from the primary hardening contribution from the mature α'. Hence, the overall irradiation-induced hardening decreases; our alloys show improved radiation resistance because of their stronger sink strengths. The results presented in this paper could provide insights for the design and optimization of ATF cladding materials for future fission and space applications.« less
  9. Microstructure evolution, enhanced aging kinetics, and mechanical properties of AA7075 alloy after friction extrusion

    In the present study we utilized Friction Extrusion (FE) a solid phase processing technique to produce fully consolidated dense 5 mm rods of AA7075 alloy. The combination of large shear stresses and temperatures at the tool-billet interface during the FE process resulted in the formation of dynamically recrystallized ~2.0 μm equiaxed grains and fine uniformly distributed stable η (MgZn2) precipitates ~25–100 nm in size. Formation of such a microstructure resulted in lower solutionizing temperature and times (flash annealing) as compared to the conventionally extruded counterparts. Here we demonstrate for the first time that the solutionizing times for the T6 heatmore » treatment of AA7075 can be reduced by three times using this FE process. In addition to being an energy efficient process, FE also serves to improve the performance of AA7075 alloys by retaining their strength while enhancing the ductility of the material. The tensile data for samples that were flash annealed and artificially aged after FE processing showed exceptional increase in ultimate tensile strength by over 19% and yield strength by over 59%, compared with an as-FE-processed sample.« less
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"Zhang, Dalong"

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